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_7108552
_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         'C60 H102.00 Co2 K2 N6 O4 Si4'
_chemical_formula_sum            'C60 H102 Co2 K2 N6 O4 Si4'
_chemical_formula_weight         1279.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-01-06
_audit_creation_method           CRYSTALS_ver_14.30
_cell_angle_alpha                90
_cell_angle_beta                 105.108(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3587(14)
_cell_length_b                   12.8112(14)
_cell_length_c                   20.986(2)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     3467.4(6)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_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      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            73885
_diffrn_reflns_theta_full        30.059
_diffrn_reflns_theta_max         30.059
_diffrn_reflns_theta_min         1.636
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368.001
_exptl_crystal_size_max          0.541
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.73
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         10123
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.0016818
_refine_ls_shift/su_mean         0.0000501
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 1.95P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0860
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0860
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                7366
_reflns_number_total             10151
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0527
_oxford_refine_ls_scale          0.105429(19)
_oxford_reflns_number_all        10123
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_12003_0m in P2(1)/n'
_cod_data_source_file            c2cc34560a.txt
_cod_data_source_block           12003_Complex_3
_cod_original_cell_volume        3467.3(6)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C60 H102.00 Co2 K2 N6 O4 Si4'
_cod_database_code               7108552
_iucr_refine_instruction_details_constraints
;
BLOCK
CONT SCALE
CONT CO ( 1 ,X'S,U'S) UNTIL C ( 28 )
CONT C ( 29 ,X'S,U[ISO]) UNTIL C ( 301 )
SUMFIX PART(1001,OCC) AND PART(1002,OCC)
RIDE C ( 4,X'S) H ( 41,X'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 ( 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)
RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) H ( 233,X'S)
RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S)
RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S)
RIDE C ( 26,X'S) H ( 261,X'S) H ( 262,X'S) H ( 263,X'S)
RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S) H ( 273,X'S)
RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S)
RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S)
RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S)
RIDE C ( 291,X'S) H (2911,X'S) H (2912,X'S)
RIDE C ( 301,X'S) H (3011,X'S) H (3012,X'S) H (3013,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
;