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_4325115
_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_sum            'C138 H198 Cl2 Co2 Hf2 N10 Na2 O12 P6'
_chemical_formula_weight         2966.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-07-24
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                99.384(3)
_cell_angle_beta                 102.512(3)
_cell_angle_gamma                100.827(3)
_cell_formula_units_Z            1
_cell_length_a                   12.7902(8)
_cell_length_b                   13.8837(8)
_cell_length_c                   22.7745(14)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     3789.3(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_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  0.033
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22129
_diffrn_reflns_theta_full        29.480
_diffrn_reflns_theta_max         30.082
_diffrn_reflns_theta_min         1.528
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.865
_exptl_crystal_size_mid          0.424
_exptl_crystal_size_min          0.236
_platon_squeeze_details
;
;
_refine_diff_density_max         1.83
_refine_diff_density_min         -1.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9981
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         22129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.0164176
_refine_ls_shift/su_mean         1.9137303
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 7.13P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0800
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0800
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                19495
_reflns_number_total             22129
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.25
_oxford_diffrn_Wilson_scale      221.11
_oxford_refine_ls_r_factor_ref   0.0343
_oxford_refine_ls_scale          0.069500(6)
_oxford_reflns_number_all        22129
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMT_22_0m in P1'
_cod_data_source_file            ic200445x_si_002_4.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C69 H99 Cl1 Co1 Hf1 N5 Na1 O6 P3'
_cod_database_code               4325115