Isolation and Assessment of the Molecular and Electronic Structures of Azo-Anion-Radical Complexes of Chromium and Molybdenum. Experimental and Theoretical Characterization of Complete Electron-Transfer Series
Sucheta Joy; Tobias Krämer; Nanda D. Paul; Priyabrata Banerjee; John E. McGrady; Sreebrata Goswami; Inorganic Chemistry 50 (2011) 9993–10004; doi:10.1021/ic200708c

data_4326451
_publ_section_title
;
 Isolation and Assessment of the Molecular and Electronic Structures of
 Azo-Anion-Radical Complexes of Chromium and Molybdenum. Experimental and
 Theoretical Characterization of Complete Electron-Transfer Series
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9993
_journal_page_last               10004
_journal_paper_doi               10.1021/ic200708c
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C33 H24 Cl3 Cr N9, C H2 Cl2'
_chemical_formula_sum            'C34 H26 Cl5 Cr N9'
_chemical_formula_weight         789.89
_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                79.0880(10)
_cell_angle_beta                 78.4510(10)
_cell_angle_gamma                64.2980(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9804(6)
_cell_length_b                   10.1877(7)
_cell_length_c                   18.9810(12)
_cell_measurement_reflns_used    5954
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.1
_cell_volume                     1692.27(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi 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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16029
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.8732
_exptl_absorpt_correction_T_min  0.8009
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       Plate
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+1.3719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                4858
_reflns_number_total             5954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200708c_si_002_1.cif
_cod_data_source_block           1a.CH2Cl2_0m
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrn' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4326451