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_4325116
_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         'C65 H115 Cl0.76 Co1 Hf1 I0.24 N5 Na1 O5 P3'
_chemical_formula_sum            'C65 H115 Cl0.76 Co Hf I0.24 N5 Na O5 P3'
_chemical_formula_weight         1457.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-08-23
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 90.2243(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6354(4)
_cell_length_b                   24.6754(7)
_cell_length_c                   19.2156(6)
_cell_measurement_reflns_used    8189
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     6939.4(3)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.073
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67184
_diffrn_reflns_theta_full        29.037
_diffrn_reflns_theta_max         29.037
_diffrn_reflns_theta_min         1.343
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.997
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       prism
_exptl_crystal_F_000             3043.183
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.117
_refine_diff_density_max         1.64
_refine_diff_density_min         -1.92
_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     749
_refine_ls_number_reflns         18434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.0006430
_refine_ls_shift/su_mean         0.0000790
_refine_ls_structure_factor_coef Fsqd
_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: 
 2.83 3.37 1.64 0.517 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0797
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0797
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                12903
_reflns_number_total             18434
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.95
_oxford_diffrn_Wilson_scale      273.96
_oxford_refine_ls_r_factor_ref   0.0739
_oxford_refine_ls_scale          0.047173(3)
_oxford_reflns_number_all        18434
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic200445x_si_002_5.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C65 H115 Cl0.76 Co1 Hf1 I0.24 N5 Na1 O5 P3'
_cod_database_code               4325116