Probing the redox non-innocence of dinuclear, three-coordinate Co(II) nindigo complexes: not simply beta-diketiminate variants
Skye Fortier; Octavio Gonzalez-del Moral; Chun-Hsing Chen; Maren Pink; Daniel J. Mindiola; Kenneth G. Caulton; Chem.Commun. 48 (2012) 11082–; doi:10.1039/c2cc34560a

data_7108554
_publ_section_title
;
 Probing the redox non-innocence of dinuclear, three-coordinate Co(II)
 nindigo complexes: not simply beta-diketiminate variants
;
_journal_name_full               Chem.Commun.
_journal_page_first              11082
_journal_paper_doi               10.1039/c2cc34560a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C22 H31 Co1 N3 Si2'
_chemical_formula_sum            'C22 H31 Co N3 Si2'
_chemical_formula_weight         452.61
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-06-18
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.5775(4)
_cell_length_b                   17.1584(5)
_cell_length_c                   19.2207(6)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    100
_cell_measurement_theta_max      21
_cell_measurement_theta_min      2
_cell_volume                     4807.6(2)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
'0.5 degree frames measured for 0.3 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Si 1 1 1 and 3 1 1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            124878
_diffrn_reflns_theta_full        20.685
_diffrn_reflns_theta_max         22.984
_diffrn_reflns_theta_min         1.380
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.96
_refine_diff_density_min         -1.25
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9547
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         16557
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.0015920
_refine_ls_shift/su_mean         0.0000936
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.63P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1103
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.1102
_reflns_limit_h_max              26
_reflns_limit_h_min              0
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                9653
_reflns_number_total             16577
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.29
_oxford_diffrn_Wilson_scale      73.21
_oxford_refine_ls_r_factor_ref   0.0869
_oxford_refine_ls_scale          0.11800(2)
_oxford_reflns_number_all        16560
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'CMC0904_0m in Pbca'
_cod_data_source_file            c2cc34560a.txt
_cod_data_source_block           12501_Complex_1
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C22 H31 Co1 N3 Si2'
_cod_database_code               7108554
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S)
RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S)
RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S)
RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S)
RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) H ( 193,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) H ( 203,X'S)
RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) H ( 213,X'S)
RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) H ( 223,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;