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_7119845
_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_absolute_configuration ad
_chemical_formula_moiety         'C96 H120 Cu16 N12 O6 S25, Cl O4, 4(O)'
_chemical_formula_sum            'C96 H120 Cl Cu16 N12 O14 S25'
_chemical_formula_weight         3519.62
_chemical_name_common
'[(L2)~12~Cu^I^~5~Cu^II^~11~(\m~4~-S)(\m~4~-O)~6~][ClO~4~]^.^4H~2~O'
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   mixed
_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
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   18.1253(7)
_cell_length_b                   18.1253(7)
_cell_length_c                   29.8697(14)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      3.0
_cell_volume                     8498.3(6)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'Apex2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_publication_material  'SHELXL-2014 (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 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 CMOS detector'
_diffrn_measurement_method       '\w/\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.0332
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            65370
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        38.298
_diffrn_reflns_theta_max         38.298
_diffrn_reflns_theta_min         2.131
_diffrn_source                   'beamline 11.3.1 Advanced Light Source'
_exptl_absorpt_coefficient_mu    6.410
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             3546
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.809
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.214
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.16(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.427
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         10246
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.431
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.1258
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3432
_refine_ls_wR_factor_ref         0.3727
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7295
_reflns_number_total             10246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08301c2.cif
_cod_data_source_block           kbg227
_cod_original_cell_volume        8498.3(8)
_cod_database_code               7119845
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.467
_shelx_estimated_absorpt_t_max   0.628
_shelx_res_checksum              87015
_shelx_hkl_checksum              27446