Mixed valence copper-sulfur clusters of highest nuclearity: a Cu8 wheel and a Cu16 nanoball.
Maji, Ram Chandra; Das, Partha Pratim; Bhandari, Anirban; Mishra, Saikat; Maji, Milan; Ghiassi, Kamran B.; Olmstead, Marilyn M.; Patra, Apurba K.; Chemical communications (Cambridge, England) 53 (2017) 3334–3337; doi:10.1039/c6cc08301c

data_7119846
_publ_section_title
;
 Mixed valence copper-sulfur clusters of highest nuclearity: a Cu8 wheel
 and a Cu16 nanoball.
;
_journal_issue                   23
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3334
_journal_page_last               3337
_journal_paper_doi               10.1039/c6cc08301c
_journal_volume                  53
_journal_year                    2017
_chemical_formula_sum            'C99.5 H87 Cl2 Cu8 N9 O9.5 S16'
_chemical_formula_weight         2652.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-19 deposited with the CCDC.
2016-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 92.805(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   18.757(5)
_cell_length_b                   30.586(5)
_cell_length_c                   20.498(5)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      2.27
_cell_volume                     11746(5)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'Apex2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_unetI/netI     0.1188
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            94954
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.098
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.805
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             5380
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.469
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1295
_refine_ls_number_reflns         21817
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1530
_refine_ls_R_factor_gt           0.0842
_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^)+(0.1139P)^2^+86.0966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2136
_refine_ls_wR_factor_ref         0.2496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12667
_reflns_number_total             21817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08301c2.cif
_cod_data_source_block           cu8_sq
_cod_original_formula_sum        'C99.50 H87 Cl2 Cu8 N9 O9.50 S16'
_cod_database_code               7119846
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.614
_shelx_estimated_absorpt_t_max   0.714
_shelx_res_checksum              78192
_shelx_hkl_checksum              91745
_shelx_fab_checksum              77543