Tertiary Hierarchical Complexity in Assemblies of Sulfur-Bridged Metal Chiral Clusters
Han, Haixiang; Yao, Yuan; Bhargava, Anuj; Wei, Zheng; Tang, Zhichu; Suntivich, Jin; Voznyy, Oleksandr; Robinson, Richard D.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c04764

data_4135155
_publ_section_title
;
 Tertiary Hierarchical Complexity in Assemblies of Sulfur-Bridged Metal
 Chiral Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c04764
_journal_year                    2020
_chemical_formula_moiety         '(C84 H48 Cu13 N12 O12 S12), 1(C2 H3 N)'
_chemical_formula_sum            'C86 H51 Cu13 N13 O12 S12'
_chemical_formula_weight         2669.14
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.8513(2)
_cell_length_b                   18.8513(2)
_cell_length_c                   49.4010(6)
_cell_measurement_reflns_used    17456
_cell_measurement_temperature    253(1)
_cell_measurement_theta_max      63.5240
_cell_measurement_theta_min      3.2260
_cell_volume                     15203.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      253(1)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  HyPix
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1262
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            68399
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        63.572
_diffrn_reflns_theta_max         63.572
_diffrn_reflns_theta_min         3.245
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.699
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9466
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       block
_exptl_crystal_F_000             7938
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.1021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1692P)^2^+230.9269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2905
_refine_ls_wR_factor_ref         0.2953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2501
_reflns_number_total             2764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04764_si_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        15203.7(4)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4135155
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.486
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13)
2.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C2), C14(C9,C10,C11,C12,C13)
;
_shelx_res_checksum              92556
_shelx_hkl_checksum              34420
_shelx_fab_checksum              64503
_olex2_submission_special_instructions 'No special instructions were received'