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_4302567
_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         'C45 H54 Co1 I1 N3 P3'
_chemical_formula_sum            'C45 H54 Co I N3 P3'
_chemical_formula_weight         915.70
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-02-16
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   14.8343(4)
_cell_length_b                   14.8343(4)
_cell_length_c                   74.260(2)
_cell_measurement_reflns_used    9191
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     14152.1(7)
_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       '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  0.031
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       104
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4666
_diffrn_reflns_theta_full        30.193
_diffrn_reflns_theta_max         30.193
_diffrn_reflns_theta_min         1.645
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             5640
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         4666
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.000916
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +29.02P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0662
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0662
_reflns_limit_h_max              0
_reflns_limit_h_min              -18
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              104
_reflns_limit_l_min              0
_reflns_number_gt                4290
_reflns_number_total             4666
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.88
_oxford_diffrn_Wilson_scale      1531.93
_oxford_refine_ls_r_factor_ref   0.0266
_oxford_refine_ls_scale          0.0263492(13)
_oxford_reflns_number_all        4666
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'SF_21_2_0m in R-3c'
_cod_data_source_file            ic900552b_si_002_5.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        14152.0(7)
_cod_original_sg_symbol_Hall     '-R 3 2"c '
_cod_original_sg_symbol_H-M      'R -3 c '
_cod_original_formula_sum        'C45 H54 Co1 I1 N3 P3'
_cod_database_code               4302567