Copper Chalcogenide Clusters Stabilized with Ferrocene-Based Diphosphine Ligands
Chhatra B. Khadka; Bahareh Khalili Najafabadi; Mahdi Hesari; Mark S. Workentin; John F. Corrigan; Inorganic Chemistry 52 (2013) 6798–6805; doi:10.1021/ic3021854

data_4335151
_publ_contact_author_address
;Dept of Chemistry
The University of Western Ontario
London ON 
N6A 5B7 Canada
;
_publ_contact_author_email       corrigan@uwo.ca
_publ_contact_author_name        'John F Corrigan'
_publ_section_title
;
 Copper Chalcogenide Clusters Stabilized with Ferrocene-Based Diphosphine
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6798
_journal_page_last               6805
_journal_paper_doi               10.1021/ic3021854
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C136 H112 Cu12 Fe4 P8 S6,  10 (C H Cl3) '
_chemical_formula_sum            'C146 H120 Cl30 Cu12 Fe4 P8 S6'
_chemical_formula_weight         4364.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.4243(2)
_cell_length_b                   21.4243(2)
_cell_length_c                   17.8779(3)
_cell_measurement_reflns_used    8662
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.04
_cell_volume                     8205.97(18)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonium Kappa CCD'
_diffrn_measurement_method       'phi scans + omega to complete'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16417
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    2.551
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       plates
_exptl_crystal_F_000             4348
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.244
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8374
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1491P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.2110
_reflns_number_gt                6512
_reflns_number_total             8374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3021854_si_002_1.cif
_cod_data_source_block           n12011
_cod_database_code               4335151