Exploring Trends in Metal-Metal Bonding, Spectroscopic Properties, and Conformational Flexibility in a Series of Heterobimetallic Ti/M and V/M Complexes (M = Fe, Co, Ni, and Cu).
Wu, Bing; Wilding, Matthew J. T.; Kuppuswamy, Subramaniam; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Inorganic chemistry 55 (2016) 12137–12148; doi:10.1021/acs.inorgchem.6b01543

data_4348734
_publ_section_title
;
 Exploring Trends in Metal-Metal Bonding, Spectroscopic Properties, and
 Conformational Flexibility in a Series of Heterobimetallic Ti/M and V/M
 Complexes (M = Fe, Co, Ni, and Cu).
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12137
_journal_page_last               12148
_journal_paper_doi               10.1021/acs.inorgchem.6b01543
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C46 H79 Cu1 I1 N3 O1 P3 V1'
_chemical_formula_sum            'C46 H79 Cu I N3 O P3 V'
_chemical_formula_weight         1024.46
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2013-09-18
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.7987(3)
_cell_length_b                   42.8341(12)
_cell_length_c                   20.1806(5)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     10199.0(5)
_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      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.056
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15247
_diffrn_reflns_theta_full        29.994
_diffrn_reflns_theta_max         29.994
_diffrn_reflns_theta_min         1.726
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4272
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.26
_refine_diff_density_min         -1.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         15247
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.0185032
_refine_ls_shift/su_mean         0.0004548
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +19.50P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1188
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1188
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              60
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                11893
_reflns_number_total             15247
_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   0.0608
_oxford_refine_ls_scale          0.0294117(17)
_oxford_reflns_number_all        15247
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'sk_1013_0ma in Pbcm'
_cod_data_source_file            ic6b01543_si_002.cif
_cod_data_source_block           10
_cod_original_sg_symbol_Hall     '-P 2c 2b '
_cod_original_sg_symbol_H-M      'P b c m '
_cod_original_formula_sum        'C46 H79 Cu1 I1 N3 O1 P3 V1'
_cod_database_code               4348734
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT CU   (    1 ,X'S,U'S)  UNTIL P    (  202 ) 
CONT O    (    1 ,X'S,U[ISO])  UNTIL O    (  101 ) 
CONT N    (    1 ,X'S,U'S)  UNTIL C    (   22 ) 
CONT C    (   23 ,X'S,U[ISO])  UNTIL C    (  129 ) 
CONT C    (  201 ,X'S,U'S)  UNTIL C    (  222 ) 
CONT C    (  223 ,X'S,U[ISO])  UNTIL C    (  342 ) 
EQUIVALENCE PART(3001, OCC) 
CONTINUE    PART(3002, OCC) 
WEIGHT -1   PART(3002, OCC) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) H   (  43,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 183,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  21,X'S) H   ( 213,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,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) 
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) H   ( 293,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) H   (1242,X'S) H   (1243,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) H   (1252,X'S) H   (1253,X'S) 
RIDE C   ( 126,X'S) H   (1261,X'S) H   (1262,X'S) H   (1263,X'S) 
RIDE C   ( 127,X'S) H   (1271,X'S) H   (1272,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) H   (1282,X'S) 
RIDE C   ( 129,X'S) H   (1291,X'S) H   (1292,X'S) H   (1293,X'S) 
RIDE C   ( 202,X'S) H   (2021,X'S) 
RIDE C   ( 204,X'S) H   (2041,X'S) H   (2042,X'S) H   (2043,X'S) 
RIDE C   ( 205,X'S) H   (2051,X'S) 
RIDE C   ( 207,X'S) H   (2071,X'S) H   (2072,X'S) H   (2073,X'S) 
RIDE C   ( 208,X'S) H   (2081,X'S) 
RIDE C   ( 209,X'S) H   (2091,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) H   (2102,X'S) H   (2103,X'S) 
RIDE C   ( 211,X'S) H   (2111,X'S) H   (2112,X'S) H   (2113,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) 
RIDE C   ( 213,X'S) H   (2131,X'S) H   (2132,X'S) H   (2133,X'S) 
RIDE C   ( 214,X'S) H   (2141,X'S) H   (2142,X'S) H   (2143,X'S) 
RIDE C   ( 216,X'S) H   (2161,X'S) 
RIDE C   ( 218,X'S) H   (2182,X'S) H   (2181,X'S) 
RIDE C   ( 219,X'S) H   (2191,X'S) 
RIDE C   ( 221,X'S) H   (2213,X'S) H   (2211,X'S) 
RIDE C   ( 222,X'S) H   (2221,X'S) 
RIDE C   ( 223,X'S) H   (2231,X'S) 
RIDE C   ( 224,X'S) H   (2241,X'S) H   (2242,X'S) H   (2243,X'S) 
RIDE C   ( 225,X'S) H   (2251,X'S) H   (2252,X'S) H   (2253,X'S) 
RIDE C   ( 323,X'S) H   (3231,X'S) 
RIDE C   ( 325,X'S) H   (3251,X'S) H   (3252,X'S) H   (3253,X'S) 
RIDE C   ( 342,X'S) H   (3421,X'S) H   (3422,X'S) H   (3423,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
A-U(IJ)'S  0.0, 0.005000 = C(20) TO C(21) 
END                                                                             
;