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_4323409
_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            'C35 H38 F12 Fe N6 O3 P2 V'
_chemical_formula_weight         987.44
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.791(3)
_cell_length_b                   20.350(7)
_cell_length_c                   27.058(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     8144(3)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens 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       'Siemens 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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.1709
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            10383
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.763
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.00109(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   1.460
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_restrained_S_obs      1.460
_refine_ls_R_factor_all          0.1531
_refine_ls_R_factor_obs          0.0556
_refine_ls_shift/esd_max         0.197
_refine_ls_shift/esd_mean        0.009
_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         0.1245
_refine_ls_wR_factor_obs         0.1106
_reflns_number_observed          3157
_reflns_number_total             8951
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9609923_1.cif
_cod_data_source_block           bos20
_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_database_code               4323409