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_4302568
_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         'C65 H115 Cl0.27 Co1 I0.73 N5 Na1 O5 P3 Zr1'
_chemical_formula_sum            'C65 H115 Cl0.27 Co I0.73 N5 Na O5 P3 Zr'
_chemical_formula_weight         1415.34
_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             09-02-02
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90.284(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7610(9)
_cell_length_b                   24.6060(15)
_cell_length_c                   19.1884(11)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     6969.3(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 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.043
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            128032
_diffrn_reflns_theta_full        29.556
_diffrn_reflns_theta_max         30.159
_diffrn_reflns_theta_min         1.346
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             2985.757
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         20441
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.012332
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 8.17P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0799
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0799
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                15456
_reflns_number_total             20441
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.34
_oxford_diffrn_Wilson_scale      460.41
_oxford_refine_ls_r_factor_ref   0.0499
_oxford_refine_ls_scale          0.055370(4)
_oxford_reflns_number_all        20441
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'CMT13_0m in P2(1)/n'
_cod_data_source_file            ic900552b_si_002_6.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      'P 1 21/n 1 '
_cod_original_formula_sum        'C65 H115 Cl0.27 Co1 I0.73 N5 Na1 O5 P3 Zr1'
_cod_database_code               4302568