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_4303167
_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            'C54 H40 Br2 O3 P2 S2'
_chemical_formula_weight         1022.74
_chemical_name_systematic
;
 ?
;
_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                97.3930(10)
_cell_angle_beta                 103.5190(10)
_cell_angle_gamma                95.8200(10)
_cell_formula_units_Z            1
_cell_length_a                   10.0956(7)
_cell_length_b                   10.1702(7)
_cell_length_c                   11.9686(8)
_cell_measurement_temperature    85(2)
_cell_volume                     1173.82(14)
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23757
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.928
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.346
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0589P)^2^+1.2132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                4525
_reflns_number_total             4798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901002y_si_001_2.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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_database_code               4303167