Chemistry of Thiocarboxylates: Synthesis and Structures of Neutral Copper(I) Thiocarboxylates with Triphenylphosphine
Theivanayagam C. Deivaraj; Ghee Xiong Lai; Jagadese J. Vittal; Inorganic Chemistry 39 (2000) 1028–1034; doi:10.1021/ic9907314

data_4300076
_publ_contact_author_address
; Department of Chemistry
  National University of Singapore
  Kent Ridge
  Singapore 119 260
;
_publ_contact_author_email       chmjjv@nus.edu.sg
_publ_contact_author_fax         '(65) 874 2975'
_publ_contact_author_name        'Jagadese J. Vittal'
_publ_contact_author_phone       '(65) 779 1691'
_publ_section_title
;
Chemistry of Thiocarboxylates: Synthesis and Structures of Neutral
Copper(I) Thiocarboxylates with Triphenylphosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1028
_journal_page_last               1034
_journal_paper_doi               10.1021/ic9907314
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C82.5 H67 Cl Cu4 O5 P3 S4'
_chemical_formula_weight         1649.12
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                94.974(1)
_cell_angle_beta                 95.976(1)
_cell_angle_gamma                100.450(1)
_cell_formula_units_Z            2
_cell_length_a                   12.4413(1)
_cell_length_b                   15.5443(1)
_cell_length_c                   20.4637(3)
_cell_measurement_reflns_used    6764
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.76
_cell_volume                     3848.09(7)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXTL (Siemens, 1996)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker AXS 3-circle CCD system'
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19210
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.346
_exptl_absorpt_correction_T_max  0.8204
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long thin rods, cut'
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00032(16)
_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   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         12777
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0521P)^2^+1.4155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                7868
_reflns_number_total             12777
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C82.50 H67 Cl Cu4 O5 P3 S4'
_cod_database_code               4300076