Synthesis, structures and 31P NMR studies of bis(diphenylphosphino)methane adducts of copper and silver thiocarboxylates †
Deivaraj, Theivanayagam C.; Vittal, Jagadese J.; Journal of the Chemical Society, Dalton Transactions  (2001) 322–; doi:10.1039/b007867k

data_7010298
_publ_section_title
;
 Synthesis, structures and 31P NMR studies of
 bis(diphenylphosphino)methane adducts of copper and silver
 thiocarboxylates&#x200A;&#x2020;
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              322
_journal_paper_doi               10.1039/b007867k
_journal_year                    2001
_chemical_formula_sum            'C81.25 H76.5 Cl6.75 Cu3 F6 O3 P7 S2'
_chemical_formula_weight         1925.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 95.806(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.8440(3)
_cell_length_b                   14.3432(3)
_cell_length_c                   33.9877(7)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.74
_cell_volume                     17384.0(5)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_method       '\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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            41839
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.8312
_exptl_absorpt_correction_T_min  0.6250
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'hexagonal shape, cut'
_exptl_crystal_F_000             7846
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.206
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00004(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         15016
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+159.1934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2269
_reflns_number_gt                10697
_reflns_number_total             15016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007867k.txt
_cod_data_source_block           Compound1
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C81.25 H76.50 Cl6.75 Cu3 F6 O3 P7 S2'
_cod_database_code               7010298