Electronic Structure Description of a Doubly Oxidized Bimetallic Cobalt Complex with Proradical Ligands.
Clarke, Ryan M.; Hazin, Khatera; Thompson, John R.; Savard, Didier; Prosser, Kathleen E.; Storr, Tim; Inorganic chemistry 55 (2016) 762–774; doi:10.1021/acs.inorgchem.5b02231

data_4344549
_publ_section_title
;
 Electronic Structure Description of a Doubly Oxidized Bimetallic Cobalt
 Complex with Proradical Ligands.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              762
_journal_page_last               774
_journal_paper_doi               10.1021/acs.inorgchem.5b02231
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C38 H52 Cl2 Co F6 N2 O3 Sb'
_chemical_formula_sum            'C38 H52 Cl2 Co F6 N2 O3 Sb'
_chemical_formula_weight         950.42
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.132(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5959(9)
_cell_length_b                   9.1176(7)
_cell_length_c                   32.637(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4332.0(5)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            36570
_diffrn_reflns_theta_full        67.202
_diffrn_reflns_theta_max         68.574
_diffrn_reflns_theta_min         2.715
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.610
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick , 1996)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         5241
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.0011601
_refine_ls_shift/su_mean         0.0000243
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.344 0.392 0.183 0.647E-01 0.189E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1116
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0569
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                5810
_reflns_number_total             7916
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.93
_oxford_diffrn_Wilson_scale      354.76
_oxford_refine_ls_r_factor_ref   0.0487
_oxford_refine_ls_scale          0.07119(12)
_oxford_reflns_number_all        7916
_oxford_reflns_threshold_expression_ref I>2.5\s(I)
_cod_data_source_file            ic5b02231_si_002.cif
_cod_data_source_block           '[CoL-H2O]+'
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4344549
_iucr_refine_instruction_details_constraints
;
BLOC SCALE X'S U'S 
EQUIV CL(1,OCC) UNTIL CL(4) C(41,OCC) C(42,OCC) 
WEIGHT -1 CL(1,OCC) CL(2,OCC) C(42,OCC) 
RIDE C ( 1,X'S) H( 11,X'S) 
RIDE C ( 2,X'S) H( 21,X'S) 
RIDE C ( 3,X'S) H( 31,X'S) 
RIDE C ( 4,X'S) H( 41,X'S) 
RIDE C ( 5,X'S) H( 51,X'S) 
RIDE C ( 8,X'S) H( 81,X'S) 
RIDE C ( 12,X'S) H( 121,X'S) 
RIDE C ( 14,X'S) H( 141,X'S) H( 142,X'S) H( 143,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) 
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) 
RIDE C ( 23,X'S) H( 231,X'S) H( 232,X'S) H( 233,X'S) 
RIDE C ( 27,X'S) H( 271,X'S) 
RIDE C ( 29,X'S) H( 291,X'S) 
RIDE C ( 31,X'S) H( 311,X'S) H( 312,X'S) H( 313,X'S) 
RIDE C ( 32,X'S) H( 321,X'S) H( 322,X'S) H( 323,X'S) 
RIDE C ( 33,X'S) H( 331,X'S) H( 332,X'S) H( 333,X'S) 
RIDE C ( 35,X'S) H( 351,X'S) H( 352,X'S) H( 353,X'S) 
RIDE C ( 36,X'S) H( 361,X'S) H( 362,X'S) H( 363,X'S) 
RIDE C ( 37,X'S) H( 371,X'S) H( 372,X'S) H( 373,X'S) 
RIDE C ( 41,X'S) H( 411,X'S) H( 412,X'S) 
RIDE C ( 42,X'S) H( 421,X'S) H( 422,X'S) 
RIDE O ( 3,X'S) H( 32,X'S) H( 33,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
VIB 0,0.01 = CL(3) TO C(41), CL(4) TO C(41) 
CONT CL(1) TO C(42), CL(2) TO C(42) 
U(IJ)'S 0,0.01 = CL(3) TO C(41), CL(4) TO C(41) 
CONT CL(1) TO C(42), CL(2) TO C(42) 
DIST 1.77 0.01 = CL(3) TO C(41), CL(4) TO C(41) 
CONT CL(1) TO C(42), CL(2) TO C(42) 
ANGLE 111 0.01 = CL(3) TO C(41) TO CL(4) 
CONT CL(1) TO C(42) TO CL(2) 
END                                                                             
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