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_4335152
_publ_contact_author_address
;Dept of Chemistry
The University of Western Ontario
London ON
N6A 5B7
;
_publ_contact_author_email       corrigan@uwo.ca
_publ_contact_author_name        'John Corrigan'
_publ_contact_author_phone       '519 661 2111'
_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         'C102 H84 Cu8 Fe3 P6 Se4, 6(C H2 Cl2)'
_chemical_formula_sum            'C108 H96 Cl12 Cu8 Fe3 P6 Se4'
_chemical_formula_weight         2996.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.220(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7936(11)
_cell_length_b                   22.2859(15)
_cell_length_c                   30.1023(19)
_cell_measurement_reflns_used    345118
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.96
_cell_measurement_theta_min      2.20
_cell_volume                     11150.4(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  '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  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0954
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            339794
_diffrn_reflns_theta_full        25.84
_diffrn_reflns_theta_max         25.84
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    3.596
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       Plates
_exptl_crystal_F_000             5936
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.046
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1270
_refine_ls_number_reflns         21522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0387P)^2^+75.9369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                15758
_reflns_number_total             21522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3021854_si_002_2.cif
_cod_data_source_block           b12027
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4335152