data_cu_0315_n3_nh3_br_0m
_audit_creation_date               2023-11-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number       '2018/3'
_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. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety          
 '2(C21 H12 N O6), 2(C21 H15 N O6), 6(H4 N), 1.5(H2 O2), 2(C H Br3)'
_chemical_formula_sum              'C86 H83 Br6 N10 O27'
_chemical_formula_weight           2168.08
_chemical_absolute_configuration   ?
_chemical_melting_point            ?
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'
 'Br' 'Br' -0.6763 1.2805
 '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        'cubic'
_space_group_IT_number             197
_space_group_name_H-M_alt          'I 2 3'
_space_group_name_Hall             'I 2 2 3'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-x, y, -z'
 'x, -y, -z'
 'z, x, y'
 'z, -x, -y'
 '-z, -x, y'
 '-z, x, -y'
 'y, z, x'
 '-y, z, -x'
 'y, -z, -x'
 '-y, -z, x'
 'x+1/2, y+1/2, z+1/2'
 '-x+1/2, -y+1/2, z+1/2'
 '-x+1/2, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z+1/2'
 'z+1/2, x+1/2, y+1/2'
 'z+1/2, -x+1/2, -y+1/2'
 '-z+1/2, -x+1/2, y+1/2'
 '-z+1/2, x+1/2, -y+1/2'
 'y+1/2, z+1/2, x+1/2'
 '-y+1/2, z+1/2, -x+1/2'
 'y+1/2, -z+1/2, -x+1/2'
 '-y+1/2, -z+1/2, x+1/2'

_cell_length_a                     20.9596(12)
_cell_length_b                     20.9596(12)
_cell_length_c                     20.9596(12)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       9207.7(16)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      9705
_cell_measurement_temperature      300.00
_cell_measurement_theta_max        68.29
_cell_measurement_theta_min        5.17
_shelx_estimated_absorpt_T_max     0.596
_shelx_estimated_absorpt_T_min     0.513
_exptl_absorpt_coefficient_mu      3.846
_exptl_absorpt_correction_T_max    0.7531
_exptl_absorpt_correction_T_min    0.6678
_exptl_absorpt_correction_type     none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1020 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.8867.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              gold
_exptl_crystal_density_diffrn      1.564
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               4380
_exptl_crystal_size_max            0.2
_exptl_crystal_size_mid            0.16
_exptl_crystal_size_min            0.15
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0557
_diffrn_reflns_av_unetI/netI       0.0237
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.999
_diffrn_reflns_limit_h_max         23
_diffrn_reflns_limit_h_min         -24
_diffrn_reflns_limit_k_max         24
_diffrn_reflns_limit_k_min         -20
_diffrn_reflns_limit_l_max         25
_diffrn_reflns_limit_l_min         -22
_diffrn_reflns_number              21116
_diffrn_reflns_point_group_measured_fraction_full  0.999
_diffrn_reflns_point_group_measured_fraction_max  0.999
_diffrn_reflns_theta_full          67.679
_diffrn_reflns_theta_max           68.281
_diffrn_reflns_theta_min           5.169
_diffrn_ambient_temperature        300.00
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.999
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54178
_diffrn_source                     ?
_diffrn_source_current             1.2
_diffrn_source_power               0.06
_diffrn_source_voltage             50.0
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.840
_reflns_Friedel_fraction_full      1.000
_reflns_Friedel_fraction_max       1.000
_reflns_number_gt                  2624
_reflns_number_total               2828
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'SAINT V8.40B (?, 2016)'
_computing_data_collection         ?
_computing_data_reduction          'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics      'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution      'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max           0.473
_refine_diff_density_min           -0.516
_refine_diff_density_rms           0.104
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack     0.5
_refine_ls_extinction_coef         0.0006(2)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.157
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       194
_refine_ls_number_reflns           2828
_refine_ls_number_restraints       1
_refine_ls_R_factor_all            0.0705
_refine_ls_R_factor_gt             0.0677
_refine_ls_restrained_S_all        1.157
_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)+(0.1378P)²+1.1114P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1894
_refine_ls_wR_factor_ref           0.1932
_refine_special_details
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All N(H) groups, All O(H) groups
2. Restrained distances
 N006-H00H
 0.9 with sigma of 0.02
3. Others
 Fixed Sof: H00M(0.5)
4.a Riding coordinates:
 N006(H00A,H00C,H00D), O00M(H00M), C5(H5)
4.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00E(H00E), C00F(H00F), C00G(H00G), C00I(H00I), C00J(H00J),
 C00K(H00K), C00L(H00L)
4.c Idealised tetrahedral OH refined as rotating group:
 O003(H003)
;
_atom_sites_solution_hydrogens     mixed
_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
 O001 O 0.60596(15) 0.72940(15) 1.02008(14) 0.0630(8) Uani 1 1 d . . . . .
 O002 O 0.58546(16) 0.83287(17) 1.01323(16) 0.0720(10) Uani 1 1 d . . . . .
 O003 O 0.76973(16) 0.60164(15) 0.98017(16) 0.0696(10) Uani 1 1 d . . . . .
 H003 H 0.771150 0.566697 0.962622 0.104 Uiso 1 1 calc R U . . .
 O004 O 0.87484(17) 0.5878(2) 0.9883(2) 0.0866(13) Uani 1 1 d . . . . .
 N005 N 0.8282(3) 0.8282(3) 1.1718(3) 0.081(3) Uani 1 3 d S T P . .
 N006 N 0.5041(2) 0.88635(19) 0.90837(18) 0.0678(10) Uani 1 1 d D . . . .
 H00A H 0.493448 0.885950 0.867274 0.081 Uiso 1 1 d R U . . .
 H00C H 0.489608 0.851110 0.927114 0.081 Uiso 1 1 d R U . . .
 H00D H 0.487008 0.920400 0.927114 0.081 Uiso 1 1 d R U . . .
 H00H H 0.543(2) 0.874(3) 0.923(3) 0.102 Uiso 1 1 d D U . . .
 C007 C 0.61621(17) 0.78458(19) 0.99801(18) 0.0527(8) Uani 1 1 d . . . . .
 C008 C 0.8257(2) 0.61612(18) 1.0018(2) 0.0571(9) Uani 1 1 d . . . . .
 C009 C 0.66822(18) 0.7918(2) 0.94975(17) 0.0518(9) Uani 1 1 d . . . . .
 C00A C 0.8271(2) 0.7754(2) 1.1289(2) 0.0691(14) Uani 1 1 d . . . . .
 C00B C 0.6953(2) 0.7385(2) 0.92104(19) 0.0596(10) Uani 1 1 d . . . . .
 H00B H 0.681324 0.697999 0.932458 0.072 Uiso 1 1 calc R U . . .
 C00C C 0.8259(2) 0.6713(2) 1.04669(17) 0.0559(9) Uani 1 1 d . . . . .
 N00D N 0.8126(3) 0.8126(3) 0.8126(3) 0.090(3) Uani 1 3 d S T P . .
 C00E C 0.7691(2) 0.6969(2) 1.0690(2) 0.0622(11) Uani 1 1 d . . . . .
 H00E H 0.730442 0.679263 1.056168 0.075 Uiso 1 1 calc R U . . .
 C00F C 0.7424(2) 0.7451(2) 0.8759(2) 0.0684(13) Uani 1 1 d . . . . .
 H00F H 0.759380 0.709236 0.856103 0.082 Uiso 1 1 calc R U . . .
 C00G C 0.7698(2) 0.7481(3) 1.1099(2) 0.0709(14) Uani 1 1 d . . . . .
 H00G H 0.731479 0.764642 1.125002 0.085 Uiso 1 1 calc R U . . .
 C00H C 0.7647(2) 0.8059(2) 0.8600(2) 0.0698(14) Uani 1 1 d . . . . .
 C00I C 0.6900(2) 0.8514(2) 0.9334(2) 0.0664(12) Uani 1 1 d . . . . .
 H00I H 0.672001 0.887223 0.952371 0.080 Uiso 1 1 calc R U . . .
 C00J C 0.8838(2) 0.7506(3) 1.1064(3) 0.0850(18) Uani 1 1 d . . . . .
 H00J H 0.922439 0.768803 1.118243 0.102 Uiso 1 1 calc R U . . .
 C00K C 0.8827(2) 0.6984(3) 1.0660(3) 0.0799(16) Uani 1 1 d . . . . .
 H00K H 0.921030 0.681331 1.051521 0.096 Uiso 1 1 calc R U . . .
 C00L C 0.7384(3) 0.8587(2) 0.8890(3) 0.0815(17) Uani 1 1 d . . . . .
 H00L H 0.753088 0.899342 0.878812 0.098 Uiso 1 1 calc R U . . .
 O00M O 0.5489(6) 1.000000 1.000000 0.183(5) Uani 1 2 d S T P . .
 H00M H 0.549001 0.967190 0.976170 0.274 Uiso 0.5 1 d R U P . .
 Br1 Br 0.8834(18) 0.8641(14) 0.994(3) 1.55(3) Uiso 1 1 d . . . . .
 C5 C 0.9220(13) 0.9220(13) 0.9220(13) 0.33(3) Uiso 1 3 d S . P . .
 H5 H 0.895438 0.895440 0.895440 0.396 Uiso 1 3 d R U P . .


_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
 O001 C007 1.264(5) . ?
 O002 C007 1.242(5) . ?
 O003 H003 0.8200 . ?
 O003 C008 1.294(5) . ?
 O004 C008 1.220(5) . ?
 N005 C00A 1.426(4) 8_757 ?
 N005 C00A 1.426(4) 11_577 ?
 N005 C00A 1.426(4) . ?
 N006 H00A 0.8899 . ?
 N006 H00C 0.8900 . ?
 N006 H00D 0.8899 . ?
 N006 H00H 0.91(3) . ?
 C007 C009 1.495(4) . ?
 C008 C00C 1.492(5) . ?
 C009 C00B 1.388(6) . ?
 C009 C00I 1.374(6) . ?
 C00A C00G 1.389(7) . ?
 C00A C00J 1.381(6) . ?
 C00B H00B 0.9300 . ?
 C00B C00F 1.374(5) . ?
 C00C C00E 1.386(6) . ?
 C00C C00K 1.380(6) . ?
 N00D C00H 1.418(3) 9 ?
 N00D C00H 1.418(3) . ?
 N00D C00H 1.418(3) 5 ?
 C00E H00E 0.9300 . ?
 C00E C00G 1.375(5) . ?
 C00F H00F 0.9300 . ?
 C00F C00H 1.399(7) . ?
 C00G H00G 0.9300 . ?
 C00H C00L 1.379(6) . ?
 C00I H00I 0.9300 . ?
 C00I C00L 1.385(6) . ?
 C00J H00J 0.9300 . ?
 C00J C00K 1.382(6) . ?
 C00K H00K 0.9300 . ?
 C00L H00L 0.9300 . ?
 O00M H00M 0.8499 . ?
 O00M H00M 0.8498 4_577 ?
 Br1 C5 2.09(4) . ?
 C5 H5 0.9660 . ?

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
 C008 O003 H003 109.5 . . ?
 C00A N005 C00A 119.12(16) 11_577 . ?
 C00A N005 C00A 119.12(16) 8_757 11_577 ?
 C00A N005 C00A 119.12(16) 8_757 . ?
 H00A N006 H00C 109.5 . . ?
 H00A N006 H00D 109.5 . . ?
 H00A N006 H00H 122.8 . . ?
 H00C N006 H00D 109.5 . . ?
 H00C N006 H00H 86.1 . . ?
 H00D N006 H00H 116.2 . . ?
 O001 C007 C009 117.6(3) . . ?
 O002 C007 O001 124.3(3) . . ?
 O002 C007 C009 118.1(4) . . ?
 O003 C008 C00C 113.9(3) . . ?
 O004 C008 O003 124.8(3) . . ?
 O004 C008 C00C 121.3(4) . . ?
 C00B C009 C007 120.7(4) . . ?
 C00I C009 C007 120.2(3) . . ?
 C00I C009 C00B 119.1(3) . . ?
 C00G C00A N005 121.0(4) . . ?
 C00J C00A N005 119.6(5) . . ?
 C00J C00A C00G 119.4(3) . . ?
 C009 C00B H00B 119.6 . . ?
 C00F C00B C009 120.8(4) . . ?
 C00F C00B H00B 119.6 . . ?
 C00E C00C C008 120.7(4) . . ?
 C00K C00C C008 120.4(4) . . ?
 C00K C00C C00E 118.9(3) . . ?
 C00H N00D C00H 119.62(11) 9 . ?
 C00H N00D C00H 119.62(11) 9 5 ?
 C00H N00D C00H 119.62(11) 5 . ?
 C00C C00E H00E 119.9 . . ?
 C00G C00E C00C 120.2(4) . . ?
 C00G C00E H00E 119.9 . . ?
 C00B C00F H00F 120.1 . . ?
 C00B C00F C00H 119.8(4) . . ?
 C00H C00F H00F 120.1 . . ?
 C00A C00G H00G 119.7 . . ?
 C00E C00G C00A 120.6(4) . . ?
 C00E C00G H00G 119.7 . . ?
 C00F C00H N00D 119.6(4) . . ?
 C00L C00H N00D 120.9(5) . . ?
 C00L C00H C00F 119.5(3) . . ?
 C009 C00I H00I 119.6 . . ?
 C009 C00I C00L 120.8(4) . . ?
 C00L C00I H00I 119.6 . . ?
 C00A C00J H00J 120.2 . . ?
 C00A C00J C00K 119.6(4) . . ?
 C00K C00J H00J 120.2 . . ?
 C00C C00K C00J 121.2(4) . . ?
 C00C C00K H00K 119.4 . . ?
 C00J C00K H00K 119.4 . . ?
 C00H C00L C00I 120.0(4) . . ?
 C00H C00L H00L 120.0 . . ?
 C00I C00L H00L 120.0 . . ?
 H00M O00M H00M 179.6 . 4_577 ?
 Br1 C5 Br1 117.9(9) 9 . ?
 Br1 C5 Br1 117.9(9) 9 5 ?
 Br1 C5 Br1 117.9(9) 5 . ?
 Br1 C5 H5 81.7 9 . ?
 Br1 C5 H5 81.7 . . ?
 Br1 C5 H5 81.7 5 . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O001 C007 C009 C00B 12.6(6) . . . . ?
 O001 C007 C009 C00I -167.2(4) . . . . ?
 O002 C007 C009 C00B -166.6(4) . . . . ?
 O002 C007 C009 C00I 13.6(6) . . . . ?
 O003 C008 C00C C00E 8.9(7) . . . . ?
 O003 C008 C00C C00K -170.1(5) . . . . ?
 O004 C008 C00C C00E -170.2(5) . . . . ?
 O004 C008 C00C C00K 10.8(8) . . . . ?
 N005 C00A C00G C00E -179.5(6) . . . . ?
 N005 C00A C00J C00K 178.5(7) . . . . ?
 C007 C009 C00B C00F 179.0(4) . . . . ?
 C007 C009 C00I C00L 179.6(5) . . . . ?
 C008 C00C C00E C00G -179.4(5) . . . . ?
 C008 C00C C00K C00J 178.4(6) . . . . ?
 C009 C00B C00F C00H 1.8(8) . . . . ?
 C009 C00I C00L C00H 0.9(10) . . . . ?
 C00A N005 C00A C00G 133.0(6) 8_757 . . . ?
 C00A N005 C00A C00G -28.5(12) 11_577 . . . ?
 C00A N005 C00A C00J -46.5(12) 8_757 . . . ?
 C00A N005 C00A C00J 152.0(6) 11_577 . . . ?
 C00A C00J C00K C00C 1.3(10) . . . . ?
 C00B C009 C00I C00L -0.2(8) . . . . ?
 C00B C00F C00H N00D -179.0(6) . . . . ?
 C00B C00F C00H C00L -1.1(8) . . . . ?
 C00C C00E C00G C00A 0.7(8) . . . . ?
 N00D C00H C00L C00I 177.6(6) . . . . ?
 C00E C00C C00K C00J -0.6(9) . . . . ?
 C00F C00H C00L C00I -0.3(9) . . . . ?
 C00G C00A C00J C00K -0.9(10) . . . . ?
 C00H N00D C00H C00F -33.3(13) 5 . . . ?
 C00H N00D C00H C00F 134.5(7) 9 . . . ?
 C00H N00D C00H C00L 148.9(7) 5 . . . ?
 C00H N00D C00H C00L -43.4(13) 9 . . . ?
 C00I C009 C00B C00F -1.2(7) . . . . ?
 C00J C00A C00G C00E 0.0(9) . . . . ?
 C00K C00C C00E C00G -0.4(8) . . . . ?

_olex2_submission_special_instructions  'No special instructions were received'
