Reaction of Elemental Sulfur with a Copper(I) Complex Forming a trans-μ-1,2 End-On Disulfide Complex: New Directions in Copper-Sulfur Chemistry
Matthew E. Helton; Peng Chen; Partha P. Paul; Zoltán Tyeklár; Roger D. Sommer; Lev N. Zakharov; Arnold L. Rheingold; Edward I. Solomon; Kenneth D. Karlin; Journal of the American Chemical Society 125 (2003) 1160–1161; doi:10.1021/ja027574j

data_4113423
_publ_section_title
;
 Reaction of Elemental Sulfur with a Copper(I) Complex Forming a
 trans-\m-1,2 End-On Disulfide Complex: New Directions in Copper-Sulfur
 Chemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1160
_journal_page_last               1161
_journal_paper_doi               10.1021/ja027574j
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C24 H33 Cl Cu N4 O5.5 S'
_chemical_formula_weight         596.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.9730(16)
_cell_length_b                   16.9730(16)
_cell_length_c                   18.229(2)
_cell_measurement_temperature    173(2)
_cell_volume                     5251.5(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0913
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21179
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    1.07
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0809P)^2^+14.8368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                3783
_reflns_number_total             4605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027574j.cif
_cod_data_source_block           kdk48
_cod_original_cell_volume        5251.6(10)
_cod_original_formula_sum        'C24 H33 Cl1 Cu1 N4 O5.50 S1'
_cod_database_code               4113423