Bimetallic Reactivity. Oxo Transfer Reactions with a Heterobimetallic Complex of Iron(II) and Vanadium(III)
David G. McCollum; Glenn P. A. Yap; Louise Liable-Sands; Arnold L. Rheingold; B. Bosnich; Inorganic Chemistry 36 (1997) 2230–2235; doi:10.1021/ic9609923

data_4323410
_publ_contact_author
;
        Prof. B. Bosnich
        University of Chicago
        Department of Chemistry
        5735 South Ellis Avenue
        Chicago, Illinois 60637
;
_publ_contact_author_fax         '312 702 0805'
_publ_contact_author_phone       '312 702 7250'
_publ_section_title
;
 Bimetallic Reactivity. Oxo Transfer Reactions with a Heterobimetallic
 Complex of Iron(II) and Vanadium(III)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2230
_journal_page_last               2235
_journal_paper_doi               10.1021/ic9609923
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C36.2 H41 Cl2 F6 Fe N6 O2.3 P V'
_chemical_formula_weight         919.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 122.73(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.881(4)
_cell_length_b                   10.265(1)
_cell_length_c                   17.184(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     4285.6(11)
_computing_cell_refinement       P4
_computing_data_collection       P4
_computing_data_reduction        XSCANS
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       P4
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3403
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.784
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1882
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.504
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_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2996
_refine_ls_number_restraints     2
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_refine_ls_restrained_S_obs      1.690
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_obs          0.0633
_refine_ls_shift/esd_max         2.128
_refine_ls_shift/esd_mean        0.072
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1482
_refine_ls_wR_factor_obs         0.1356
_reflns_number_observed          2353
_reflns_number_total             3002
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9609923_2.cif
_cod_data_source_block           bos21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4286(1)
_cod_original_formula_sum        'C36.20 H41 Cl2 F6 Fe N6 O2.30 P V'
_cod_database_code               4323410