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_4302564
_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_absolute_configuration ad
_chemical_formula_moiety         'C45 H75 Cl1 Co1 I1 N3 P3 Zr1'
_chemical_formula_sum            'C45 H75 Cl Co I N3 P3 Zr'
_chemical_formula_weight         1063.54
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-10-30
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.8496(8)
_cell_length_b                   53.0394(14)
_cell_length_c                   15.0536(4)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    120
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     22236.1(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       74
_diffrn_reflns_limit_k_min       -74
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16289
_diffrn_reflns_theta_full        30.070
_diffrn_reflns_theta_max         30.070
_diffrn_reflns_theta_min         1.536
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             8768
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.35
_refine_diff_density_min         -1.45
_refine_ls_abs_structure_details 'Flack (1983), 7843 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.002(10)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         16289
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.021782
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +56.32P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0902
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0902
_reflns_limit_h_max              39
_reflns_limit_h_min              0
_reflns_limit_k_max              74
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                14737
_reflns_number_total             16289
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.23
_oxford_diffrn_Wilson_scale      2489.08
_oxford_refine_ls_r_factor_ref   0.0380
_oxford_refine_ls_scale          0.21847(7)
_oxford_reflns_number_all        16289
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMT_04_0ma in Fdd2'
_cod_data_source_file            ic900552b_si_002_2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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_sg_symbol_H-M      'F d d 2 '
_cod_original_formula_sum        'C45 H75 Cl1 Co1 I1 N3 P3 Zr1'
_cod_database_code               4302564