Anion Encapsulation and Geometric Changes in Hepta- and Hexanuclear Copper(I) Dichalcogeno Clusters: A Theoretical and Experimental Investigation
Camille Latouche; Samia Kahlal; Yan-Ru Lin; Jian-Hong Liao; Eric Furet; C. W. Liu; Jean-Yves Saillard; Inorganic Chemistry 52 (2013) 13253–13262; doi:10.1021/ic402207u

data_4336768
_publ_section_title
;
 Anion Encapsulation and Geometric Changes in Hepta- and Hexanuclear
 Copper(I) Dichalcogeno Clusters: A Theoretical and Experimental
 Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13253
_journal_page_last               13262
_journal_paper_doi               10.1021/ic402207u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C36 H84 Br Cu7 O12 P6 Se12'
_chemical_formula_weight         2367.06
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   22.467(5)
_cell_length_b                   22.467(5)
_cell_length_c                   12.533(3)
_cell_measurement_reflns_used    3390
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.84
_cell_measurement_theta_min      2.65
_cell_volume                     5479(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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10644
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    8.700
_exptl_absorpt_correction_T_max  0.1834
_exptl_absorpt_correction_T_min  0.1285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_description       block
_exptl_crystal_F_000             3396
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.066
_refine_diff_density_min         -2.042
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+76.6566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1533
_reflns_number_gt                1535
_reflns_number_total             2159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402207u_si_002_2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4336768