Assembly of Supertetrahedral Cluster into Cu-In-S Superlattice via Unprecedented Vertex-Edge Connection Mode
Wang, Hongxiang; Yang, Huajun; Wang, Wei; Xue, Chaozhuang; Zhang, Yingying; Luo, Min; Hu, Dandan; Lin, Jian; Li, Dong-Sheng; Wu, Tao; CrystEngComm  (2017) –; doi:10.1039/C7CE00849J

data_7228735
_publ_section_title
;
 Assembly of Supertetrahedral Cluster into Cu-In-S Superlattice via
 Unprecedented Vertex-Edge Connection Mode
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00849J
_journal_year                    2017
_chemical_formula_sum            'C77 H190.2 Cu5 Ge0 In30 N11 O7.1 S53'
_chemical_formula_weight         6845.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-16 deposited with the CCDC.
2017-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.1467(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.4954(18)
_cell_length_b                   19.3412(11)
_cell_length_c                   35.425(2)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.43
_cell_volume                     20775(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.1092
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            171721
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.271
_diffrn_reflns_theta_min         1.974
_exptl_absorpt_coefficient_mu    4.322
_exptl_absorpt_correction_T_max  0.709
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Higashi, T.(1995).'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.189
_exptl_crystal_description       pyramidal
_exptl_crystal_F_000             12996
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;                          
 Disordered solvents including 11 protonated 3,5-DMP (C7NH16) molecules and 7.1 water molecules (H2O) have been removed from each formula unit by the SQUEEZE process.
;
_refine_diff_density_max         1.750
_refine_diff_density_min         -2.853
_refine_diff_density_rms         0.231
_refine_ls_abs_structure_details
;
 Flack x determined using 8135 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.056(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         47051
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0200P)^2^+200.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                23545
_reflns_number_total             47051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00849j2.cif
_cod_data_source_block           CIS27
_cod_original_formula_sum        'C77 H190.20 Cu5 Ge0 In30 N11 O7.10 S53'
_cod_database_code               7228735
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              25538