Synthesis of Copper(I) Thiolate Complexes in the Thioetherification of Aryl Halides.
Chen, Chaohuang; Weng, Zhiqiang; Hartwig, John F.; Organometallics 31 (2012) 8031–8037; doi:10.1021/om300711c

data_4079397
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Synthesis of Copper(I) Thiolate Complexes in the Thioetherification of
 Aryl Halides.
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              8031
_journal_page_last               8037
_journal_paper_doi               10.1021/om300711c
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C42 H42 Cu4 S6, 2(C42 H36 K N6), C4 H8 O'
_chemical_formula_sum            'C130 H122 Cu4 K2 N12 O S6'
_chemical_formula_weight         2393.12
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2007-10-10   text and data added, srw 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.072(3)
_cell_length_b                   19.072(3)
_cell_length_c                   54.419(16)
_cell_measurement_reflns_used    935
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.66
_cell_measurement_theta_min      2.58
_cell_volume                     17142(6)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4 (Bruker, 2005 & 2007) 
;
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  g05was
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            58004
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_time  364
_diffrn_standards_number         265
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  0.9015
_exptl_absorpt_correction_T_min  0.8121
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             7464
_exptl_crystal_id                g05was
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 0 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         6987
_refine_ls_number_restraints     502
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                4698
_reflns_number_total             6987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300711c_si_002.cif
_cod_data_source_block           g05was
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        17143(6)
_cod_original_sg_symbol_Hall     '-R 3 '
_cod_original_sg_symbol_H-M      'R -3   '
_cod_database_code               4079397