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_2242495
_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 (C26 H22 P2)2] [Fe Cl4], 0.59C H2 Cl2'
_chemical_formula_moiety
'C52 H44 Cl2 Fe P4 +, Cl4 Fe -, 0.59(C H2 Cl2)'
_chemical_formula_sum            'C52.59 H45.18 Cl7.18 Fe2 P4'
_chemical_formula_weight         1167.47
_chemical_name_systematic
;<i>trans</i>-Bis[1,2-bis(diphenylphosphane)ethylene]dichloridoiron(III)
tetrachloridoferrate(III) dichloromethane 0.59-solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 100.541(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7528(7)
_cell_length_b                   23.6871(17)
_cell_length_c                   23.6871(17)
_cell_measurement_reflns_used    4040
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      2.31
_cell_volume                     5379.7(7)
_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-2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT-2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0913
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            71735
_diffrn_reflns_theta_full        31.506
_diffrn_reflns_theta_max         31.517
_diffrn_reflns_theta_min         1.719
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al</i>., 2015)
;
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       plate
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.673
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         8962
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+11.3134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                6273
_reflns_number_total             8962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pj2052sup1.cif
_cod_data_source_block           1
_cod_database_code               2242495
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.902
_shelx_hkl_checksum              86342
_shelx_res_checksum              31380
_cod_database_fobs_code 2242495