Crystal structure of (?-oxalato)bis[chlorotris(triphenylphosphine oxide-O)iron(III)] tetrachloroferrate(III), [FeCl(C18H15PO)3][C2O4][FeCl4]
Zhi-Fang Zhang; Zeitschrift für Kristallographie - New Crystal Structures 226 (2011) 486–; doi:

data_8103231
_publ_contact_author
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     Z.F. Zhang
School of Chemistry and Chemical Engineering, Yulin University,
      Yulin 719000, P. R. China
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_publ_section_title
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 Crystal structure of (?-oxalato)bis[chlorotris(triphenylphosphine
 oxide-O)iron(III)] tetrachloroferrate(III),
 [FeCl(C18H15PO)3][C2O4][FeCl4]
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              486
_journal_volume                  226
_journal_year                    2011
_chemical_formula_moiety         'C110 H90 Cl2 Fe2 O10 P6, 2(Cl4 Fe)'
_chemical_formula_sum            'C110 H90 Cl10 Fe4 O10 P6'
_chemical_formula_weight         2335.54
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
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2011-09-02 # Formatted by publCIF
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_cell_angle_alpha                78.803(8)
_cell_angle_beta                 85.771(9)
_cell_angle_gamma                81.857(9)
_cell_formula_units_Z            1
_cell_length_a                   10.672(7)
_cell_length_b                   15.740(10)
_cell_length_c                   16.709(10)
_cell_measurement_reflns_used    3007
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.77
_cell_measurement_theta_min      2.48
_cell_volume                     2722(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16701
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1194
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         10468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+1.3083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                6711
_reflns_number_total             10468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3560.cff
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8103231
_publ_section_exptl_
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All H atoms on C atoms were generated geometrically and refined as riding 
atoms with d(C-H) = 0.95\%A, and U~iso~(H)=1.2 U~eq~(O).Three Cl atoms of 
the FeCl~4~ are disorderedover two equivalent positions.
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