data_exp_1242
_audit_creation_date               2020-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2016/6'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety           'C H Cl3, C49 H43 N3 O'
_chemical_formula_sum              'C50 H44 Cl3 N3 O'
_chemical_formula_weight           809.23
_chemical_absolute_configuration   ?
_chemical_melting_point            ?
_chemical_oxdiff_formula           'C50 H50 O N4 Si'
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             9
_space_group_name_H-M_alt          'C 1 c 1'
_space_group_name_Hall             'C -2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 'x, -y, z+1/2'
 'x+1/2, y+1/2, z'
 'x+1/2, -y+1/2, z+1/2'

_cell_length_a                     19.2386(5)
_cell_length_b                     14.0313(3)
_cell_length_c                     15.2313(4)
_cell_angle_alpha                  90
_cell_angle_beta                   95.628(2)
_cell_angle_gamma                  90
_cell_volume                       4091.76(18)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      4381
_cell_measurement_temperature      100.01(10)
_cell_measurement_theta_max        71.4750
_cell_measurement_theta_min        3.8890
_shelx_estimated_absorpt_T_max     0.891
_shelx_estimated_absorpt_T_min     0.799
_exptl_absorpt_coefficient_mu      2.353
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.75763
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              blue
_exptl_crystal_colour_primary      blue
_exptl_crystal_density_diffrn      1.314
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1696
_exptl_crystal_size_max            0.1
_exptl_crystal_size_mid            0.1
_exptl_crystal_size_min            0.05
_exptl_special_details
;
 ?
;
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0351
_diffrn_reflns_av_unetI/netI       0.0550
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  1.000
_diffrn_reflns_limit_h_max         22
_diffrn_reflns_limit_h_min         -21
_diffrn_reflns_limit_k_max         16
_diffrn_reflns_limit_k_min         -16
_diffrn_reflns_limit_l_max         18
_diffrn_reflns_limit_l_min         -16
_diffrn_reflns_number              7244
_diffrn_reflns_point_group_measured_fraction_full  0.606
_diffrn_reflns_point_group_measured_fraction_max  0.606
_diffrn_reflns_theta_full          66.595
_diffrn_reflns_theta_max           66.595
_diffrn_reflns_theta_min           3.906
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        100.01(10)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   8.0697
_diffrn_detector_type              EosS2
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     17.00  61.00   1.00    2.50    --   34.73 -19.00 -30.00   44
  2  ω      3.00  74.00   1.00    2.50    --   34.73 -99.00  30.00   71
  3  ω     38.00 101.00   1.00    9.00    --  105.88 -94.00  60.00   63
  4  ω     38.00 109.00   1.00    9.00    --  105.88 -94.00 150.00   71
  5  ω    121.00 147.00   1.00    9.00    --  105.88  45.00 120.00   26
  6  ω     89.00 118.00   1.00    9.00    --  105.88  45.00 120.00   29
  7  ω     92.00 173.00   1.00    9.00    --  105.88  45.00   0.00   81
  8  ω    115.00 173.00   1.00    9.00    --  105.88  61.00-150.00   58
  9  ω     88.00 142.00   1.00    9.00    --  105.88 160.00 -11.00   54
 10  ω     18.00 102.00   1.00    2.50    --   34.73  57.00 -60.00   84
 11  ω     50.00 115.00   1.00    9.00    --  105.88 -45.00 -90.00   65
 12  ω     59.00 120.00   1.00    9.00    --  105.88 -61.00-150.00   61
 13  ω     39.00  86.00   1.00    2.50    --   34.73-125.00-120.00   47
 14  ω      3.00  40.00   1.00    2.50    --   34.73 -57.00 -60.00   37
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0183366000
_diffrn_orient_matrix_UB_12        -0.0974931000
_diffrn_orient_matrix_UB_13        -0.0381870000
_diffrn_orient_matrix_UB_21        0.0553549000
_diffrn_orient_matrix_UB_22        0.0480907000
_diffrn_orient_matrix_UB_23        -0.0517040000
_diffrn_orient_matrix_UB_31        0.0554230000
_diffrn_orient_matrix_UB_32        -0.0157964000
_diffrn_orient_matrix_UB_33        0.0786793000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.211
_reflns_Friedel_fraction_full      0.211
_reflns_Friedel_fraction_max       0.211
_reflns_number_gt                  4142
_reflns_number_total               4376
_reflns_odcompleteness_completeness  99.97
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       66.49
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection         'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction          'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.813
_refine_diff_density_min           -0.879
_refine_diff_density_rms           0.089
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack     0.03(3)
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.021
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       520
_refine_ls_number_reflns           4376
_refine_ls_number_restraints       131
_refine_ls_R_factor_all            0.0759
_refine_ls_R_factor_gt             0.0734
_refine_ls_restrained_S_all        1.042
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.1467P)²+6.0835P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1932
_refine_ls_wR_factor_ref           0.1978
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C1, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2, C3, C4, C5, C6, C7, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C38) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C50(H50)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C3(H3A), C4(H4), C12(H12), C13(H13), C17(H17),
 C18(H18), C21(H21), C23(H23), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31),
  C32(H32), C33(H33), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
 C46(H46), C48(H48)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C41(H41A,H41B,H41C),
 C45(H45A,H45B,H45C), C49(H49A,H49B,H49C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Cl1 Cl 0.50841(12) 1.20342(14) 0.61306(14) 0.0477(5) Uani 1 1 d . . . . .
 Cl2 Cl 0.65771(15) 1.1718(2) 0.65455(14) 0.0665(8) Uani 1 1 d . . . . .
 Cl3 Cl 0.60660(12) 1.29054(16) 0.50697(13) 0.0512(5) Uani 1 1 d . . . . .
 C50 C 0.5900(5) 1.1891(6) 0.5703(6) 0.047(2) Uani 1 1 d . . . . .
 H50 H 0.587408 1.133090 0.531614 0.056 Uiso 1 1 calc R . . . .
 O1 O 0.4201(2) 0.6037(3) 0.4630(3) 0.0209(8) Uani 1 1 d . . . . .
 N1 N 0.5300(3) 0.6859(3) 0.4166(3) 0.0180(10) Uani 1 1 d . . . . .
 H1 H 0.493489 0.677644 0.444092 0.022 Uiso 1 1 calc R . . . .
 N2 N 0.4692(3) 0.7887(3) 0.5669(3) 0.0165(9) Uani 1 1 d . . . . .
 H2 H 0.471352 0.728871 0.555043 0.020 Uiso 1 1 calc R . . . .
 N3 N 0.3917(3) 0.6186(3) 0.6240(3) 0.0186(10) Uani 1 1 d . . . . .
 H3 H 0.414514 0.632749 0.579932 0.022 Uiso 1 1 calc R . . . .
 C1 C 0.2585(10) 1.0467(12) 0.9117(12) 0.116(5) Uani 1 1 d . U . . .
 H1A H 0.244863 1.102368 0.877693 0.173 Uiso 1 1 calc GR . . . .
 H1B H 0.292918 1.063743 0.959002 0.173 Uiso 1 1 calc GR . . . .
 H1C H 0.218335 1.020235 0.935700 0.173 Uiso 1 1 calc GR . . . .
 C2 C 0.2889(5) 0.9734(6) 0.8530(7) 0.0503(19) Uani 1 1 d . U . . .
 C3 C 0.2605(4) 0.9569(5) 0.7709(6) 0.0365(15) Uani 1 1 d . U . . .
 H3A H 0.220007 0.989220 0.750160 0.044 Uiso 1 1 calc R . . . .
 C4 C 0.3522(6) 0.9237(7) 0.8840(6) 0.054(2) Uani 1 1 d . U . . .
 H4 H 0.372750 0.934424 0.941014 0.065 Uiso 1 1 calc R . . . .
 C5 C 0.3825(4) 0.8603(5) 0.8296(4) 0.0264(13) Uani 1 1 d . U . . .
 C6 C 0.4503(4) 0.8111(6) 0.8632(5) 0.0401(17) Uani 1 1 d . U . . .
 H6A H 0.447304 0.744604 0.848362 0.060 Uiso 1 1 calc GR . . . .
 H6B H 0.457982 0.817979 0.926133 0.060 Uiso 1 1 calc GR . . . .
 H6C H 0.488367 0.839477 0.836396 0.060 Uiso 1 1 calc GR . . . .
 C7 C 0.3514(3) 0.8442(4) 0.7450(4) 0.0164(10) Uani 1 1 d . U . . .
 C8 C 0.2895(4) 0.8933(5) 0.7161(5) 0.0311(14) Uani 1 1 d . U . . .
 C9 C 0.2570(6) 0.8846(11) 0.6258(8) 0.078(3) Uani 1 1 d . U . . .
 H9A H 0.271295 0.936994 0.591212 0.117 Uiso 1 1 calc GR . . . .
 H9B H 0.207117 0.885247 0.625841 0.117 Uiso 1 1 calc GR . . . .
 H9C H 0.271266 0.825754 0.600807 0.117 Uiso 1 1 calc GR . . . .
 C10 C 0.3850(3) 0.7819(4) 0.6815(4) 0.0176(11) Uani 1 1 d . . . . .
 C11 C 0.4266(3) 0.8286(4) 0.6261(4) 0.0177(11) Uani 1 1 d . . . . .
 C12 C 0.4367(3) 0.9304(4) 0.6204(4) 0.0163(11) Uani 1 1 d . . . . .
 H12 H 0.413879 0.976300 0.650903 0.020 Uiso 1 1 calc R . . . .
 C13 C 0.4847(3) 0.9481(4) 0.5637(4) 0.0175(11) Uani 1 1 d . . . . .
 H13 H 0.500263 1.008254 0.549129 0.021 Uiso 1 1 calc R . . . .
 C14 C 0.5079(3) 0.8599(4) 0.5293(3) 0.0163(11) Uani 1 1 d . . . . .
 C15 C 0.5580(3) 0.8489(4) 0.4709(3) 0.0152(10) Uani 1 1 d . . . . .
 C16 C 0.5711(3) 0.7652(4) 0.4235(4) 0.0170(11) Uani 1 1 d . . . . .
 C17 C 0.6260(3) 0.7485(4) 0.3702(4) 0.0221(12) Uani 1 1 d . . . . .
 H17 H 0.663003 0.789667 0.363498 0.026 Uiso 1 1 calc R . . . .
 C18 C 0.6155(3) 0.6611(4) 0.3299(4) 0.0224(12) Uani 1 1 d . . . . .
 H18 H 0.643319 0.633584 0.290232 0.027 Uiso 1 1 calc R . . . .
 C19 C 0.5548(3) 0.6209(4) 0.3599(4) 0.0196(11) Uani 1 1 d . . . . .
 C20 C 0.5264(3) 0.5281(4) 0.3426(4) 0.0201(11) Uani 1 1 d . . . . .
 C21 C 0.4774(3) 0.4807(4) 0.3889(4) 0.0201(11) Uani 1 1 d . . . . .
 H21 H 0.470463 0.416892 0.373895 0.024 Uiso 1 1 calc R . . . .
 C22 C 0.4358(3) 0.5151(4) 0.4563(4) 0.0198(11) Uani 1 1 d . . . . .
 C23 C 0.4117(3) 0.4421(4) 0.5125(4) 0.0209(12) Uani 1 1 d . . . . .
 H23 H 0.416845 0.380591 0.491458 0.025 Uiso 1 1 calc R . . . .
 C24 C 0.3823(3) 0.4458(4) 0.5916(4) 0.0192(12) Uani 1 1 d . . . . .
 C25 C 0.3701(3) 0.5278(4) 0.6436(4) 0.0201(11) Uani 1 1 d . . . . .
 C26 C 0.3357(3) 0.5368(4) 0.7215(4) 0.0199(11) Uani 1 1 d . . . . .
 H26 H 0.316299 0.487145 0.751353 0.024 Uiso 1 1 calc R . . . .
 C27 C 0.3361(3) 0.6315(4) 0.7453(4) 0.0189(11) Uani 1 1 d . . . . .
 H27 H 0.316314 0.657415 0.793226 0.023 Uiso 1 1 calc R . . . .
 C28 C 0.3720(3) 0.6820(4) 0.6837(4) 0.0169(11) Uani 1 1 d . . . . .
 C29 C 0.3274(4) 0.2844(5) 0.5755(6) 0.0407(17) Uani 1 1 d . U . . .
 H29 H 0.312098 0.299363 0.517306 0.049 Uiso 1 1 calc R . . . .
 C30 C 0.3139(5) 0.1951(6) 0.6093(7) 0.056(2) Uani 1 1 d . U . . .
 H30 H 0.289588 0.150271 0.573325 0.067 Uiso 1 1 calc R . . . .
 C31 C 0.3363(6) 0.1716(6) 0.6963(7) 0.057(2) Uani 1 1 d . U . . .
 H31 H 0.326738 0.111634 0.718258 0.069 Uiso 1 1 calc R . . . .
 C32 C 0.3722(5) 0.2371(5) 0.7491(6) 0.0462(19) Uani 1 1 d . U . . .
 H32 H 0.387483 0.221158 0.807104 0.055 Uiso 1 1 calc R . . . .
 C33 C 0.3866(4) 0.3280(5) 0.7175(5) 0.0321(14) Uani 1 1 d . U . . .
 H33 H 0.410705 0.372160 0.754407 0.038 Uiso 1 1 calc R . . . .
 C34 C 0.3644(3) 0.3521(4) 0.6300(5) 0.0261(13) Uani 1 1 d . U . . .
 C35 C 0.5554(3) 0.5142(4) 0.1860(4) 0.0225(12) Uani 1 1 d . . . . .
 H35 H 0.538414 0.575710 0.176099 0.027 Uiso 1 1 calc R . . . .
 C36 C 0.5549(3) 0.4742(4) 0.2692(4) 0.0213(12) Uani 1 1 d . . . . .
 C37 C 0.5806(4) 0.3814(5) 0.2816(5) 0.0318(15) Uani 1 1 d . . . . .
 H37 H 0.580082 0.352428 0.336413 0.038 Uiso 1 1 calc R . . . .
 C38 C 0.6067(4) 0.3320(4) 0.2133(5) 0.0341(16) Uani 1 1 d . U . . .
 H38 H 0.624267 0.270737 0.223037 0.041 Uiso 1 1 calc R . . . .
 C39 C 0.6070(3) 0.3730(5) 0.1311(4) 0.0273(13) Uani 1 1 d . . . . .
 H39 H 0.624727 0.339843 0.085337 0.033 Uiso 1 1 calc R . . . .
 C40 C 0.5805(3) 0.4645(4) 0.1175(4) 0.0246(13) Uani 1 1 d . . . . .
 H40 H 0.579678 0.492400 0.062015 0.030 Uiso 1 1 calc R . . . .
 C41 C 0.6720(4) 0.9072(5) 0.6012(4) 0.0275(13) Uani 1 1 d . . . . .
 H41A H 0.635406 0.922341 0.637377 0.041 Uiso 1 1 calc GR . . . .
 H41B H 0.716071 0.927367 0.630316 0.041 Uiso 1 1 calc GR . . . .
 H41C H 0.672963 0.839631 0.591440 0.041 Uiso 1 1 calc GR . . . .
 C42 C 0.6589(3) 0.9578(4) 0.5140(4) 0.0216(12) Uani 1 1 d . . . . .
 C43 C 0.6026(3) 0.9333(4) 0.4534(4) 0.0151(10) Uani 1 1 d . . . . .
 C44 C 0.5903(3) 0.9837(4) 0.3738(4) 0.0195(11) Uani 1 1 d . . . . .
 C45 C 0.5281(4) 0.9603(5) 0.3096(5) 0.0330(15) Uani 1 1 d . . . . .
 H45A H 0.531358 0.895384 0.290463 0.050 Uiso 1 1 calc GR . . . .
 H45B H 0.527339 1.001960 0.259491 0.050 Uiso 1 1 calc GR . . . .
 H45C H 0.486079 0.968610 0.337804 0.050 Uiso 1 1 calc GR . . . .
 C46 C 0.6354(4) 1.0572(5) 0.3561(4) 0.0258(13) Uani 1 1 d . . . . .
 H46 H 0.626080 1.092360 0.304451 0.031 Uiso 1 1 calc R . . . .
 C47 C 0.6933(3) 1.0796(4) 0.4126(5) 0.0284(14) Uani 1 1 d . . . . .
 C48 C 0.7051(3) 1.0302(5) 0.4926(4) 0.0257(13) Uani 1 1 d . . . . .
 H48 H 0.743692 1.045200 0.531807 0.031 Uiso 1 1 calc R . . . .
 C49 C 0.7433(4) 1.1591(6) 0.3918(6) 0.0412(18) Uani 1 1 d . . . . .
 H49A H 0.733563 1.215253 0.424357 0.062 Uiso 1 1 calc GR . . . .
 H49B H 0.737338 1.172779 0.329747 0.062 Uiso 1 1 calc GR . . . .
 H49C H 0.790569 1.139136 0.408144 0.062 Uiso 1 1 calc GR . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Cl1 C50 1.768(10) . ?
 Cl2 C50 1.754(9) . ?
 Cl3 C50 1.767(9) . ?
 C50 H50 0.9800 . ?
 O1 C22 1.286(7) . ?
 N1 H1 0.8600 . ?
 N1 C16 1.362(7) . ?
 N1 C19 1.374(7) . ?
 N2 H2 0.8600 . ?
 N2 C11 1.394(7) . ?
 N2 C14 1.401(7) . ?
 N3 H3 0.8600 . ?
 N3 C25 1.381(8) . ?
 N3 C28 1.354(8) . ?
 C1 H1A 0.9600 . ?
 C1 H1B 0.9600 . ?
 C1 H1C 0.9600 . ?
 C1 C2 1.518(13) . ?
 C2 C3 1.334(13) . ?
 C2 C4 1.442(15) . ?
 C3 H3A 0.9300 . ?
 C3 C8 1.376(10) . ?
 C4 H4 0.9300 . ?
 C4 C5 1.383(11) . ?
 C5 C6 1.520(10) . ?
 C5 C7 1.385(9) . ?
 C6 H6A 0.9600 . ?
 C6 H6B 0.9600 . ?
 C6 H6C 0.9600 . ?
 C7 C8 1.409(9) . ?
 C7 C10 1.498(8) . ?
 C8 C9 1.459(13) . ?
 C9 H9A 0.9600 . ?
 C9 H9B 0.9600 . ?
 C9 H9C 0.9600 . ?
 C10 C11 1.383(8) . ?
 C10 C28 1.425(8) . ?
 C11 C12 1.445(7) . ?
 C12 H12 0.9300 . ?
 C12 C13 1.346(8) . ?
 C13 H13 0.9300 . ?
 C13 C14 1.433(8) . ?
 C14 C15 1.383(8) . ?
 C15 C16 1.414(8) . ?
 C15 C43 1.502(7) . ?
 C16 C17 1.414(8) . ?
 C17 H17 0.9300 . ?
 C17 C18 1.377(9) . ?
 C18 H18 0.9300 . ?
 C18 C19 1.412(8) . ?
 C19 C20 1.427(8) . ?
 C20 C21 1.400(8) . ?
 C20 C36 1.497(8) . ?
 C21 H21 0.9300 . ?
 C21 C22 1.445(8) . ?
 C22 C23 1.441(8) . ?
 C23 H23 0.9300 . ?
 C23 C24 1.381(9) . ?
 C24 C25 1.429(8) . ?
 C24 C34 1.493(8) . ?
 C25 C26 1.419(8) . ?
 C26 H26 0.9300 . ?
 C26 C27 1.378(8) . ?
 C27 H27 0.9300 . ?
 C27 C28 1.409(8) . ?
 C29 H29 0.9300 . ?
 C29 C30 1.389(12) . ?
 C29 C34 1.408(10) . ?
 C30 H30 0.9300 . ?
 C30 C31 1.391(16) . ?
 C31 H31 0.9300 . ?
 C31 C32 1.365(15) . ?
 C32 H32 0.9300 . ?
 C32 C33 1.400(10) . ?
 C33 H33 0.9300 . ?
 C33 C34 1.399(11) . ?
 C35 H35 0.9300 . ?
 C35 C36 1.387(9) . ?
 C35 C40 1.381(9) . ?
 C36 C37 1.400(9) . ?
 C37 H37 0.9300 . ?
 C37 C38 1.384(10) . ?
 C38 H38 0.9300 . ?
 C38 C39 1.379(10) . ?
 C39 H39 0.9300 . ?
 C39 C40 1.389(10) . ?
 C40 H40 0.9300 . ?
 C41 H41A 0.9600 . ?
 C41 H41B 0.9600 . ?
 C41 H41C 0.9600 . ?
 C41 C42 1.506(9) . ?
 C42 C43 1.395(8) . ?
 C42 C48 1.409(9) . ?
 C43 C44 1.403(8) . ?
 C44 C45 1.504(9) . ?
 C44 C46 1.392(9) . ?
 C45 H45A 0.9600 . ?
 C45 H45B 0.9600 . ?
 C45 H45C 0.9600 . ?
 C46 H46 0.9300 . ?
 C46 C47 1.376(10) . ?
 C47 C48 1.401(9) . ?
 C47 C49 1.526(8) . ?
 C48 H48 0.9300 . ?
 C49 H49A 0.9600 . ?
 C49 H49B 0.9600 . ?
 C49 H49C 0.9600 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 Cl1 C50 H50 108.6 . . ?
 Cl2 C50 Cl1 111.6(5) . . ?
 Cl2 C50 Cl3 110.5(6) . . ?
 Cl2 C50 H50 108.6 . . ?
 Cl3 C50 Cl1 108.9(5) . . ?
 Cl3 C50 H50 108.6 . . ?
 C16 N1 H1 124.6 . . ?
 C16 N1 C19 110.8(5) . . ?
 C19 N1 H1 124.6 . . ?
 C11 N2 H2 124.9 . . ?
 C11 N2 C14 110.3(4) . . ?
 C14 N2 H2 124.9 . . ?
 C25 N3 H3 124.7 . . ?
 C28 N3 H3 124.7 . . ?
 C28 N3 C25 110.5(5) . . ?
 H1A C1 H1B 109.5 . . ?
 H1A C1 H1C 109.5 . . ?
 H1B C1 H1C 109.5 . . ?
 C2 C1 H1A 109.5 . . ?
 C2 C1 H1B 109.5 . . ?
 C2 C1 H1C 109.5 . . ?
 C3 C2 C1 121.6(11) . . ?
 C3 C2 C4 118.6(7) . . ?
 C4 C2 C1 119.7(10) . . ?
 C2 C3 H3A 119.1 . . ?
 C2 C3 C8 121.9(8) . . ?
 C8 C3 H3A 119.1 . . ?
 C2 C4 H4 119.8 . . ?
 C5 C4 C2 120.4(8) . . ?
 C5 C4 H4 119.8 . . ?
 C4 C5 C6 119.3(7) . . ?
 C4 C5 C7 119.5(7) . . ?
 C7 C5 C6 121.1(6) . . ?
 C5 C6 H6A 109.5 . . ?
 C5 C6 H6B 109.5 . . ?
 C5 C6 H6C 109.5 . . ?
 H6A C6 H6B 109.5 . . ?
 H6A C6 H6C 109.5 . . ?
 H6B C6 H6C 109.5 . . ?
 C5 C7 C8 119.1(6) . . ?
 C5 C7 C10 121.5(5) . . ?
 C8 C7 C10 119.3(5) . . ?
 C3 C8 C7 120.5(7) . . ?
 C3 C8 C9 117.7(8) . . ?
 C7 C8 C9 121.6(7) . . ?
 C8 C9 H9A 109.5 . . ?
 C8 C9 H9B 109.5 . . ?
 C8 C9 H9C 109.5 . . ?
 H9A C9 H9B 109.5 . . ?
 H9A C9 H9C 109.5 . . ?
 H9B C9 H9C 109.5 . . ?
 C11 C10 C7 115.4(5) . . ?
 C11 C10 C28 126.5(5) . . ?
 C28 C10 C7 118.1(5) . . ?
 N2 C11 C12 105.5(5) . . ?
 C10 C11 N2 128.0(5) . . ?
 C10 C11 C12 126.5(5) . . ?
 C11 C12 H12 125.5 . . ?
 C13 C12 C11 109.0(5) . . ?
 C13 C12 H12 125.5 . . ?
 C12 C13 H13 125.3 . . ?
 C12 C13 C14 109.4(5) . . ?
 C14 C13 H13 125.3 . . ?
 N2 C14 C13 105.7(5) . . ?
 C15 C14 N2 128.0(5) . . ?
 C15 C14 C13 126.4(5) . . ?
 C14 C15 C16 126.2(5) . . ?
 C14 C15 C43 118.2(5) . . ?
 C16 C15 C43 115.6(5) . . ?
 N1 C16 C15 125.9(5) . . ?
 N1 C16 C17 106.3(5) . . ?
 C17 C16 C15 127.6(5) . . ?
 C16 C17 H17 125.7 . . ?
 C18 C17 C16 108.5(5) . . ?
 C18 C17 H17 125.7 . . ?
 C17 C18 H18 126.2 . . ?
 C17 C18 C19 107.6(5) . . ?
 C19 C18 H18 126.2 . . ?
 N1 C19 C18 106.7(5) . . ?
 N1 C19 C20 124.8(5) . . ?
 C18 C19 C20 128.2(5) . . ?
 C19 C20 C36 115.9(5) . . ?
 C21 C20 C19 127.3(5) . . ?
 C21 C20 C36 116.8(5) . . ?
 C20 C21 H21 114.9 . . ?
 C20 C21 C22 130.2(5) . . ?
 C22 C21 H21 114.9 . . ?
 O1 C22 C21 122.1(5) . . ?
 O1 C22 C23 123.2(5) . . ?
 C23 C22 C21 114.7(5) . . ?
 C22 C23 H23 113.8 . . ?
 C24 C23 C22 132.5(5) . . ?
 C24 C23 H23 113.8 . . ?
 C23 C24 C25 128.1(5) . . ?
 C23 C24 C34 116.0(5) . . ?
 C25 C24 C34 115.9(5) . . ?
 N3 C25 C24 123.6(5) . . ?
 N3 C25 C26 106.0(5) . . ?
 C26 C25 C24 130.5(5) . . ?
 C25 C26 H26 125.8 . . ?
 C27 C26 C25 108.3(5) . . ?
 C27 C26 H26 125.8 . . ?
 C26 C27 H27 126.3 . . ?
 C26 C27 C28 107.5(5) . . ?
 C28 C27 H27 126.3 . . ?
 N3 C28 C10 124.7(5) . . ?
 N3 C28 C27 107.7(5) . . ?
 C27 C28 C10 127.6(5) . . ?
 C30 C29 H29 120.3 . . ?
 C30 C29 C34 119.4(9) . . ?
 C34 C29 H29 120.3 . . ?
 C29 C30 H30 119.5 . . ?
 C29 C30 C31 121.0(9) . . ?
 C31 C30 H30 119.5 . . ?
 C30 C31 H31 120.2 . . ?
 C32 C31 C30 119.5(8) . . ?
 C32 C31 H31 120.2 . . ?
 C31 C32 H32 119.5 . . ?
 C31 C32 C33 121.1(9) . . ?
 C33 C32 H32 119.5 . . ?
 C32 C33 H33 120.1 . . ?
 C34 C33 C32 119.7(8) . . ?
 C34 C33 H33 120.1 . . ?
 C29 C34 C24 119.0(6) . . ?
 C33 C34 C24 121.7(6) . . ?
 C33 C34 C29 119.2(6) . . ?
 C36 C35 H35 119.3 . . ?
 C40 C35 H35 119.3 . . ?
 C40 C35 C36 121.4(5) . . ?
 C35 C36 C20 120.9(5) . . ?
 C35 C36 C37 117.7(6) . . ?
 C37 C36 C20 121.3(6) . . ?
 C36 C37 H37 119.5 . . ?
 C38 C37 C36 121.0(6) . . ?
 C38 C37 H37 119.5 . . ?
 C37 C38 H38 119.8 . . ?
 C39 C38 C37 120.5(6) . . ?
 C39 C38 H38 119.8 . . ?
 C38 C39 H39 120.4 . . ?
 C38 C39 C40 119.1(6) . . ?
 C40 C39 H39 120.4 . . ?
 C35 C40 C39 120.3(6) . . ?
 C35 C40 H40 119.9 . . ?
 C39 C40 H40 119.9 . . ?
 H41A C41 H41B 109.5 . . ?
 H41A C41 H41C 109.5 . . ?
 H41B C41 H41C 109.5 . . ?
 C42 C41 H41A 109.5 . . ?
 C42 C41 H41B 109.5 . . ?
 C42 C41 H41C 109.5 . . ?
 C43 C42 C41 121.3(5) . . ?
 C43 C42 C48 119.4(5) . . ?
 C48 C42 C41 119.2(5) . . ?
 C42 C43 C15 119.8(5) . . ?
 C42 C43 C44 120.1(5) . . ?
 C44 C43 C15 120.0(5) . . ?
 C43 C44 C45 120.5(5) . . ?
 C46 C44 C43 119.0(5) . . ?
 C46 C44 C45 120.4(5) . . ?
 C44 C45 H45A 109.5 . . ?
 C44 C45 H45B 109.5 . . ?
 C44 C45 H45C 109.5 . . ?
 H45A C45 H45B 109.5 . . ?
 H45A C45 H45C 109.5 . . ?
 H45B C45 H45C 109.5 . . ?
 C44 C46 H46 119.0 . . ?
 C47 C46 C44 122.0(6) . . ?
 C47 C46 H46 119.0 . . ?
 C46 C47 C48 118.9(6) . . ?
 C46 C47 C49 121.7(6) . . ?
 C48 C47 C49 119.4(6) . . ?
 C42 C48 H48 119.8 . . ?
 C47 C48 C42 120.4(6) . . ?
 C47 C48 H48 119.8 . . ?
 C47 C49 H49A 109.5 . . ?
 C47 C49 H49B 109.5 . . ?
 C47 C49 H49C 109.5 . . ?
 H49A C49 H49B 109.5 . . ?
 H49A C49 H49C 109.5 . . ?
 H49B C49 H49C 109.5 . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
 N1 H1 O1 0.86 1.80 2.568(6) 147.9 .
 N3 H3 O1 0.86 1.84 2.571(6) 141.8 .

_olex2_date_sample_data_collection  2020-10-22
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.864
_oxdiff_exptl_absorpt_empirical_full_min  0.396
