data_cu_tca_br_0m
_audit_creation_date               2023-11-09
_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. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety          
 '2(C H Cl3), 2(C21 H15 N O6), 2(C21 H12 N O6), 6(H4 N), 1.5(H2 O2)'
_chemical_formula_sum              'C86 H83 Cl6 N10 O27'
_chemical_formula_weight           1901.32
_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'
 '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        '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                     20.9699(4)
_cell_length_b                     20.9699(4)
_cell_length_c                     20.9699(4)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       9221.2(5)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      6514
_cell_measurement_temperature      298.00
_cell_measurement_theta_max        62.49
_cell_measurement_theta_min        4.22
_shelx_estimated_absorpt_T_max     0.554
_shelx_estimated_absorpt_T_min     0.515
_exptl_absorpt_coefficient_mu      2.393
_exptl_absorpt_correction_T_max    0.7522
_exptl_absorpt_correction_T_min    0.5802
_exptl_absorpt_correction_type     none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1579 before and 0.0884 after correction.
The Ratio of minimum to maximum transmission is 0.7713.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light colourless'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      1.370
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         prism
_exptl_crystal_F_000               3948
_exptl_crystal_size_max            0.32
_exptl_crystal_size_mid            0.31
_exptl_crystal_size_min            0.28
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.1188
_diffrn_reflns_av_unetI/netI       0.0554
_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         18
_diffrn_reflns_limit_l_min         -24
_diffrn_reflns_number              20212
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  1.000
_diffrn_reflns_theta_full          62.482
_diffrn_reflns_theta_max           62.482
_diffrn_reflns_theta_min           4.216
_diffrn_ambient_temperature        298.00
_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           0.830
_reflns_Friedel_fraction_full      1.000
_reflns_Friedel_fraction_max       1.000
_reflns_number_gt                  2171
_reflns_number_total               2462
_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           0.381
_refine_diff_density_min           -0.592
_refine_diff_density_rms           0.066
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack     0.5
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.103
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       203
_refine_ls_number_reflns           2462
_refine_ls_number_restraints       1
_refine_ls_R_factor_all            0.0599
_refine_ls_R_factor_gt             0.0522
_refine_ls_restrained_S_all        1.102
_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)+(0.1055P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1543
_refine_ls_wR_factor_ref           0.1579
_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 O(H) groups
2. Restrained distances
 Cl01-C1
 1.85 with sigma of 0.02
3. Others
 Fixed Sof: H00N(0.5)
4.a Riding coordinates:
 N006(H00A,H00B,H00C)
4.b Free rotating group:
 O00N(H00N)
4.c Ternary CH refined with riding coordinates:
 C1(H1)
4.d Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K),
 C00L(H00L), C00M(H00M)
4.e Idealised tetrahedral OH refined as rotating group:
 O002(H002)
;
_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
 Cl01 Cl 0.48280(10) 0.36233(13) 0.60175(15) 0.1234(9) Uani 1 1 d D . . . .
 O002 O 0.47987(18) 0.10231(18) 0.72746(18) 0.0654(10) Uani 1 1 d . . . . .
 H002 H 0.452583 0.074526 0.723963 0.098 Uiso 1 1 calc R U . . .
 O003 O 0.39402(17) 0.02079(17) 0.72687(17) 0.0606(9) Uani 1 1 d . . . . .
 O004 O 0.41487(19) 0.01338(18) 0.83028(18) 0.0690(11) Uani 1 1 d . . . . .
 O005 O 0.4874(3) 0.0888(2) 0.62367(19) 0.0853(15) Uani 1 1 d . . . . .
 N006 N 0.5044(3) 0.0897(2) 0.8855(2) 0.0636(12) Uani 1 1 d . . . . .
 H00A H 0.533875 0.104619 0.858804 0.076 Uiso 1 1 d R U . . .
 H00B H 0.490165 0.121349 0.909914 0.076 Uiso 1 1 d R U . . .
 H00C H 0.521435 0.059499 0.909914 0.076 Uiso 1 1 d R U . . .
 C007 C 0.3341(2) -0.0523(2) 0.7878(2) 0.0469(10) Uani 1 1 d . . . . .
 N008 N 0.6688(3) 0.3312(3) 0.6688(3) 0.061(2) Uani 1 3 d S T P . .
 C009 C 0.5010(2) 0.1172(2) 0.6720(2) 0.0521(10) Uani 1 1 d . . . . .
 C00A C 0.3843(2) -0.0024(2) 0.7818(2) 0.0496(10) Uani 1 1 d . . . . .
 N00B N 0.1931(3) -0.1931(3) 0.8069(3) 0.076(3) Uani 1 3 d S T P . .
 C00C C 0.6260(2) 0.2785(2) 0.6699(2) 0.0540(12) Uani 1 1 d . . . . .
 C00D C 0.3076(2) -0.0811(2) 0.7350(2) 0.0544(11) Uani 1 1 d . . . . .
 H00D H 0.321396 -0.069022 0.694559 0.065 Uiso 1 1 calc R U . . .
 C00E C 0.2617(3) -0.1267(3) 0.7404(2) 0.0600(13) Uani 1 1 d . . . . .
 H00E H 0.244503 -0.145260 0.704041 0.072 Uiso 1 1 calc R U . . .
 C00F C 0.54441(19) 0.1734(2) 0.6711(2) 0.0484(10) Uani 1 1 d . . . . .
 C00G C 0.2405(3) -0.1456(3) 0.8006(3) 0.0641(15) Uani 1 1 d . . . . .
 C00H C 0.5663(2) 0.1995(2) 0.7285(2) 0.0554(12) Uani 1 1 d . . . . .
 H00H H 0.553470 0.182118 0.767256 0.067 Uiso 1 1 calc R U . . .
 C00I C 0.3131(2) -0.0704(3) 0.8478(2) 0.0592(13) Uani 1 1 d . . . . .
 H00I H 0.330621 -0.051371 0.883779 0.071 Uiso 1 1 calc R U . . .
 C00J C 0.6038(3) 0.2529(3) 0.6136(2) 0.0659(14) Uani 1 1 d . . . . .
 H00J H 0.615041 0.271507 0.574958 0.079 Uiso 1 1 calc R U . . .
 C00K C 0.5649(3) 0.1998(3) 0.6145(2) 0.0650(14) Uani 1 1 d . . . . .
 H00K H 0.552303 0.181519 0.576117 0.078 Uiso 1 1 calc R U . . .
 C00L C 0.6071(2) 0.2514(3) 0.7274(2) 0.0567(13) Uani 1 1 d . . . . .
 H00L H 0.622034 0.268369 0.765595 0.068 Uiso 1 1 calc R U . . .
 C00M C 0.2665(3) -0.1162(3) 0.8546(2) 0.0683(16) Uani 1 1 d . . . . .
 H00M H 0.252389 -0.127652 0.895085 0.082 Uiso 1 1 calc R U . . .
 O00N O 0.500000 0.0482(10) 0.500000 0.177(5) Uani 1 2 d GS T P . .
 H00N H 0.531524 0.057317 0.476201 0.265 Uiso 0.5 1 d G U P . .
 C1 C 0.4111(16) 0.4111(16) 0.5889(16) 0.25(2) Uani 1 3 d DS T P . .
 H1 H 0.384133 0.384133 0.615867 0.302 Uiso 1 3 calc R U P . .
 H00F H 0.472(3) 0.077(3) 0.859(3) 0.073(18) Uiso 1 1 d . . . . .


_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
 Cl01 C1 1.838(4) . ?
 O002 H002 0.8200 . ?
 O002 C009 1.282(6) . ?
 O003 C00A 1.266(6) . ?
 O004 C00A 1.247(6) . ?
 O005 C009 1.211(6) . ?
 N006 H00A 0.8900 . ?
 N006 H00B 0.8899 . ?
 N006 H00C 0.8899 . ?
 N006 H00F 0.91(7) . ?
 C007 C00A 1.490(6) . ?
 C007 C00D 1.378(7) . ?
 C007 C00I 1.386(7) . ?
 N008 C00C 1.425(4) . ?
 N008 C00C 1.425(4) 12_665 ?
 N008 C00C 1.425(4) 6_566 ?
 C009 C00F 1.490(6) . ?
 N00B C00G 1.413(4) . ?
 N00B C00G 1.413(4) 10_546 ?
 N00B C00G 1.413(4) 7_656 ?
 C00C C00J 1.377(7) . ?
 C00C C00L 1.391(7) . ?
 C00D H00D 0.9300 . ?
 C00D C00E 1.362(6) . ?
 C00E H00E 0.9300 . ?
 C00E C00G 1.395(7) . ?
 C00F C00H 1.401(7) . ?
 C00F C00K 1.379(7) . ?
 C00G C00M 1.401(7) . ?
 C00H H00H 0.9300 . ?
 C00H C00L 1.384(6) . ?
 C00I H00I 0.9300 . ?
 C00I C00M 1.378(7) . ?
 C00J H00J 0.9300 . ?
 C00J C00K 1.380(7) . ?
 C00K H00K 0.9300 . ?
 C00L H00L 0.9300 . ?
 C00M H00M 0.9300 . ?
 O00N H00N 0.85(19) 3_656 ?
 O00N H00N 0.8502 . ?
 C1 H1 0.9800 . ?

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
 C009 O002 H002 109.5 . . ?
 H00A N006 H00B 109.5 . . ?
 H00A N006 H00C 109.5 . . ?
 H00A N006 H00F 103.9 . . ?
 H00B N006 H00C 109.5 . . ?
 H00B N006 H00F 109.0 . . ?
 H00C N006 H00F 115.3 . . ?
 C00D C007 C00A 121.6(4) . . ?
 C00D C007 C00I 118.8(4) . . ?
 C00I C007 C00A 119.6(4) . . ?
 C00C N008 C00C 119.13(14) 6_566 12_665 ?
 C00C N008 C00C 119.13(14) . 6_566 ?
 C00C N008 C00C 119.13(14) . 12_665 ?
 O002 C009 C00F 114.6(4) . . ?
 O005 C009 O002 123.9(4) . . ?
 O005 C009 C00F 121.5(4) . . ?
 O003 C00A C007 117.4(4) . . ?
 O004 C00A O003 123.8(4) . . ?
 O004 C00A C007 118.7(4) . . ?
 C00G N00B C00G 119.71(10) 7_656 10_546 ?
 C00G N00B C00G 119.70(10) . 10_546 ?
 C00G N00B C00G 119.71(10) 7_656 . ?
 C00J C00C N008 120.1(5) . . ?
 C00J C00C C00L 119.2(4) . . ?
 C00L C00C N008 120.7(4) . . ?
 C007 C00D H00D 119.2 . . ?
 C00E C00D C007 121.6(5) . . ?
 C00E C00D H00D 119.2 . . ?
 C00D C00E H00E 119.9 . . ?
 C00D C00E C00G 120.1(5) . . ?
 C00G C00E H00E 119.9 . . ?
 C00H C00F C009 119.9(4) . . ?
 C00K C00F C009 121.4(4) . . ?
 C00K C00F C00H 118.8(4) . . ?
 C00E C00G N00B 120.7(5) . . ?
 C00E C00G C00M 118.8(4) . . ?
 C00M C00G N00B 120.5(5) . . ?
 C00F C00H H00H 120.2 . . ?
 C00L C00H C00F 119.7(4) . . ?
 C00L C00H H00H 120.2 . . ?
 C007 C00I H00I 119.6 . . ?
 C00M C00I C007 120.7(5) . . ?
 C00M C00I H00I 119.6 . . ?
 C00C C00J H00J 119.9 . . ?
 C00C C00J C00K 120.1(5) . . ?
 C00K C00J H00J 119.9 . . ?
 C00F C00K C00J 121.3(4) . . ?
 C00F C00K H00K 119.3 . . ?
 C00J C00K H00K 119.3 . . ?
 C00C C00L H00L 119.6 . . ?
 C00H C00L C00C 120.7(4) . . ?
 C00H C00L H00L 119.6 . . ?
 C00G C00M H00M 120.0 . . ?
 C00I C00M C00G 119.9(5) . . ?
 C00I C00M H00M 120.0 . . ?
 H00N O00N H00N 153.9 . 3_656 ?
 Cl01 C1 Cl01 119.6(4) 11_566 8_656 ?
 Cl01 C1 Cl01 119.6(4) . 11_566 ?
 Cl01 C1 Cl01 119.6(4) . 8_656 ?
 Cl01 C1 H1 93.8 . . ?
 Cl01 C1 H1 93.8 8_656 . ?
 Cl01 C1 H1 93.8 11_566 . ?

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
 O002 C009 C00F C00H 9.3(7) . . . . ?
 O002 C009 C00F C00K -172.2(5) . . . . ?
 O005 C009 C00F C00H -171.0(6) . . . . ?
 O005 C009 C00F C00K 7.5(9) . . . . ?
 C007 C00D C00E C00G -0.2(9) . . . . ?
 C007 C00I C00M C00G 0.7(10) . . . . ?
 N008 C00C C00J C00K 176.7(6) . . . . ?
 N008 C00C C00L C00H -179.0(6) . . . . ?
 C009 C00F C00H C00L 179.4(5) . . . . ?
 C009 C00F C00K C00J 178.3(6) . . . . ?
 C00A C007 C00D C00E -179.9(5) . . . . ?
 C00A C007 C00I C00M 179.7(5) . . . . ?
 N00B C00G C00M C00I 179.5(7) . . . . ?
 C00C N008 C00C C00J -45.7(12) 12_665 . . . ?
 C00C N008 C00C C00J 152.7(6) 6_566 . . . ?
 C00C N008 C00C C00L -28.5(12) 6_566 . . . ?
 C00C N008 C00C C00L 133.1(5) 12_665 . . . ?
 C00C C00J C00K C00F 3.8(10) . . . . ?
 C00D C007 C00A O003 12.0(7) . . . . ?
 C00D C007 C00A O004 -166.8(5) . . . . ?
 C00D C007 C00I C00M 0.0(8) . . . . ?
 C00D C00E C00G N00B -179.8(6) . . . . ?
 C00D C00E C00G C00M 0.9(9) . . . . ?
 C00E C00G C00M C00I -1.2(10) . . . . ?
 C00F C00H C00L C00C 0.8(8) . . . . ?
 C00G N00B C00G C00E -31.4(14) 10_546 . . . ?
 C00G N00B C00G C00E 137.8(7) 7_656 . . . ?
 C00G N00B C00G C00M -42.9(14) 7_656 . . . ?
 C00G N00B C00G C00M 147.9(7) 10_546 . . . ?
 C00H C00F C00K C00J -3.1(9) . . . . ?
 C00I C007 C00A O003 -167.7(5) . . . . ?
 C00I C007 C00A O004 13.5(7) . . . . ?
 C00I C007 C00D C00E -0.3(8) . . . . ?
 C00J C00C C00L C00H -0.2(9) . . . . ?
 C00K C00F C00H C00L 0.8(8) . . . . ?
 C00L C00C C00J C00K -2.1(9) . . . . ?

_olex2_submission_special_instructions  'No special instructions were received'
