Multielectron Redox Activity Facilitated by Metal-Metal Interactions in Early/Late Heterobimetallics: Co/Zr Complexes Supported by Phosphinoamide Ligands
Bennett P. Greenwood; Scott I. Forman; Gerard T. Rowe; Chun-Hsing Chen; Bruce M. Foxman; Christine M. Thomas; Inorganic Chemistry 48 (2009) 6251–6260; doi:10.1021/ic900552b

data_4302565
_publ_section_title
;
Multielectron Redox Activity Facilitated by Metal-Metal Interactions in
Early/Late Heterobimetallics: Co/Zr Complexes Supported by Phosphinoamide
Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6251
_journal_page_last               6260
_journal_paper_doi               10.1021/ic900552b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C27 H63 Cl1 Co1 I1 N3 P3 Zr1'
_chemical_formula_sum            'C27 H63 Cl Co I N3 P3 Zr'
_chemical_formula_weight         835.25
_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             09-02-03
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1913(8)
_cell_length_b                   18.1727(10)
_cell_length_c                   13.4668(7)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     3717.7(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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.000
_diffrn_reflns_limit_h_max       21
_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       -19
_diffrn_reflns_number            136211
_diffrn_reflns_theta_full        30.111
_diffrn_reflns_theta_max         30.111
_diffrn_reflns_theta_min         1.882
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.80
_refine_ls_extinction_coef       41(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5630
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.006555
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 6.57P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0648
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0648
_reflns_limit_h_max              21
_reflns_limit_h_min              0
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5479
_reflns_number_total             5630
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.97
_oxford_diffrn_Wilson_scale      286.05
_oxford_refine_ls_r_factor_ref   0.0310
_oxford_refine_ls_scale          0.066777(8)
_oxford_reflns_number_all        5630
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'BG_1_28_0ma in Pnma'
_cod_data_source_file            ic900552b_si_002_3.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C27 H63 Cl1 Co1 I1 N3 P3 Zr1'
_cod_database_code               4302565