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_4303168
_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 Ni O4 P3 S4'
_chemical_formula_weight         1581.06
_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                 93.1770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3511(14)
_cell_length_b                   14.3261(11)
_cell_length_c                   27.677(2)
_cell_measurement_temperature    85(2)
_cell_volume                     7265.1(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0234
_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            85309
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3244
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         7609
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+8.7231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                6756
_reflns_number_total             7609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901002y_si_001_3.cif
_cod_data_source_block           V
_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        7265.1(10)
_cod_database_code               4303168