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_7010299
_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            'C91 H78 Cl7 Cu3 O6 P6 S2'
_chemical_formula_weight         1956.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.647(1)
_cell_angle_beta                 85.295(1)
_cell_angle_gamma                83.440(1)
_cell_formula_units_Z            2
_cell_length_a                   13.9558(1)
_cell_length_b                   15.9713(2)
_cell_length_c                   20.6451(3)
_cell_measurement_reflns_used    8085
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.06
_cell_volume                     4523.29(9)
_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 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22244
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.110
_exptl_absorpt_correction_T_max  0.8085
_exptl_absorpt_correction_T_min  0.6574
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'blocks, cut'
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.921
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00046(19)
_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   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         14871
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+15.3962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.2023
_reflns_number_gt                10252
_reflns_number_total             14871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007867k.txt
_cod_data_source_block           compound2
_cod_original_cell_volume        4523.33(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010299