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_4325114
_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         'C27 H63 Cl1 Co1 Hf1 I1 N3 P3'
_chemical_formula_sum            'C27 H63 Cl Co Hf I N3 P3'
_chemical_formula_weight         922.52
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-01-17
_audit_creation_method           CRYSTALS_ver_14.01
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1818(4)
_cell_length_b                   18.1649(5)
_cell_length_c                   13.5297(4)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     3731.16(18)
_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  0.062
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49011
_diffrn_reflns_theta_full        30.052
_diffrn_reflns_theta_max         30.052
_diffrn_reflns_theta_min         1.877
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.273
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.103
_refine_diff_density_max         4.16
_refine_diff_density_min         -2.77
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         5615
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.0023138
_refine_ls_shift/su_mean         0.4210044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.01P)^2^ +16.75P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0691
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0691
_reflns_limit_h_max              21
_reflns_limit_h_min              0
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                3963
_reflns_number_total             5615
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.19
_oxford_diffrn_Wilson_scale      478.80
_oxford_refine_ls_r_factor_ref   0.0550
_oxford_refine_ls_scale          0.048365(4)
_oxford_reflns_number_all        5615
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMT27_0ma in Pnma'
_cod_data_source_file            ic200445x_si_002_3.cif
_cod_data_source_block           6
_cod_original_cell_volume        3731.17(18)
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C27 H63 Cl1 Co1 Hf1 I1 N3 P3'
_cod_database_code               4325114