Subtle Differences Between Zr and Hf in Early/Late Heterobimetallic Complexes with Cobalt
Vinay N. Setty; Wen Zhou; Bruce M. Foxman; Christine M. Thomas; Inorganic Chemistry 50 (2011) 4647–4655; doi:10.1021/ic200445x

data_4325113
_publ_section_title
;
 Subtle Differences Between Zr and Hf in Early/Late Heterobimetallic
 Complexes with Cobalt
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4647
_journal_page_last               4655
_journal_paper_doi               10.1021/ic200445x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C45 H75 Cl1 Co1 Hf1 I1 N3 P3'
_chemical_formula_sum            'C45 H75 Cl Co Hf I N3 P3'
_chemical_formula_weight         1150.81
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-09-23
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.0541(3)
_cell_length_b                   12.0541(3)
_cell_length_c                   19.7252(7)
_cell_measurement_reflns_used    8186
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2482.11(12)
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120
_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  0.034
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38543
_diffrn_reflns_theta_full        30.060
_diffrn_reflns_theta_max         30.060
_diffrn_reflns_theta_min         1.951
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.229
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.28
_refine_diff_density_min         -1.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9670
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4850
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.0032887
_refine_ls_shift/su_mean         0.0000756
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 3.38P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0446
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0446
_reflns_limit_h_max              8
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                4136
_reflns_number_total             4850
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.04
_oxford_diffrn_Wilson_scale      93.56
_oxford_refine_ls_r_factor_ref   0.0282
_oxford_refine_ls_scale          0.104819(14)
_oxford_reflns_number_all        4850
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMT45_0m in P-3'
_cod_data_source_file            ic200445x_si_002_2.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P -3 '
_cod_original_formula_sum        'C45 H75 Cl1 Co1 Hf1 I1 N3 P3'
_cod_database_code               4325113
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'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                                                                             
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