Synthesis, Electronic Structure, and Structural Characterization of the New, "Non-Innocent" 4,5-Dithio-Catecholate Ligand, Its Metal Complexes, and Their Oxidized 4,5-Dithio-o-quinone Derivatives
Dimitri Coucouvanis; Alok R. Paital; Qinwei Zhang; Nicolai Lehnert; Reinhart Ahlrichs; Karin Fink; Dieter Fenske; Annie K. Powell; Yanhua Lan; Inorganic Chemistry 48 (2009) 8830–8844; doi:10.1021/ic901002y

data_4303169
_publ_contact_author_address
;Department of Chemistry
University of Michigan
Ann Arbor-48109
USA
;
_publ_contact_author_email       dcouc@umich.edu
_publ_contact_author_name        'Dimitri Coucouvanis'
_publ_contact_author_phone       734-764-7339
_publ_section_title
;
Synthesis, Electronic Structure, and Structural Characterization of the
New, "Non-Innocent" 4,5-Dithio-Catecholate Ligand, Its Metal Complexes,
and Their Oxidized 4,5-Dithio-o-quinone Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8830
_journal_page_last               8844
_journal_paper_doi               10.1021/ic901002y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C84 H68 Br2 Cu O4 P3 S4'
_chemical_formula_weight         1585.89
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.9890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4277(14)
_cell_length_b                   14.2991(11)
_cell_length_c                   27.646(2)
_cell_measurement_temperature    85(2)
_cell_volume                     7274.8(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89419
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  0.676
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.535
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         7620
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0311P)^2^+45.8515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                7183
_reflns_number_total             7620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901002y_si_001_4.cif
_cod_data_source_block           VI
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        7274.7(9)
_cod_database_code               4303169