Crystal structures of two new six-coordinate iron(III) complexes with 1,2-bis(diphenylphosphane) ligands
McNeil, Jr, Derek L.; Beckford, Daihlia J.; Kneebone, Jared L.; Carpenter, Stephanie H.; Brennessel, William W.; Neidig, Michael L.; Acta Crystallographica Section E 74 (2018) 803–807; doi:10.1107/S2056989018006898

data_2242496
_publ_section_title
;
 Crystal structures of two new six-coordinate iron(III) complexes with
 1,2-bis(diphenylphosphane) ligands
;
_journal_coeditor_code           PJ2052
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              803
_journal_page_last               807
_journal_paper_doi               10.1107/S2056989018006898
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Fe Cl2 (C30 H24 P2)2] [Fe Cl4], C H2 Cl2'
_chemical_formula_moiety         'C60 H48 Cl2 Fe P4 +, Cl4 Fe -, C H2 Cl2'
_chemical_formula_sum            'C61 H50 Cl8 Fe2 P4'
_chemical_formula_weight         1302.19
_chemical_name_systematic
;<i>trans</i>-Bis[1,2-bis(diphenylphosphane)benzene]dichloridoiron(III)
tetrachloridoferrate(III) dichloromethane monosolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                81.0580(10)
_cell_angle_beta                 83.0500(10)
_cell_angle_gamma                68.3350(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8771(7)
_cell_length_b                   12.6516(8)
_cell_length_c                   12.8258(8)
_cell_measurement_reflns_used    4051
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      30.68
_cell_measurement_theta_min      2.28
_cell_volume                     1467.87(17)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL-2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT-2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27211
_diffrn_reflns_theta_full        34.972
_diffrn_reflns_theta_max         34.976
_diffrn_reflns_theta_min         2.224
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al</i>., 2015)
;
_exptl_crystal_colour            'dichroic red-green'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.229
_refine_diff_density_min         -1.394
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.24(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         22268
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1465
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0641P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1823
_reflns_number_gt                11890
_reflns_number_total             22268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pj2052sup1.cif
_cod_data_source_block           2
_cod_database_code               2242496
_shelx_estimated_absorpt_t_min   0.794
_shelx_estimated_absorpt_t_max   0.924
_shelx_hkl_checksum              19212
_shelx_res_checksum              2547
_cod_database_fobs_code 2242496