Bis[tris(1-methyl-1<i>H</i>-imidazol-2-yl)phosphine-κ^3^<i>N</i>^3^]iron(II) tetrachloroferrate(II) methanol tetrasolvate (<i>ca</i> 153K) and bis[tris(1-methyl-1<i>H</i>-imidazol-2-yl)methanol-κ^3^<i>N</i>^3^]iron(III) bis[tetrachloroferrate(III)] chloride (redetermination, <i>ca</i> 153K)
Batten, Michael P.; Canty, Allan J.; Cavell, Kingsley J.; Rüther, Thomas; Skelton, Brian W.; White, Allan H.; Acta Crystallographica Section C 60 (2004) m311–m313; doi:10.1107/S0108270104010868

data_2014271
_publ_section_title
;Bis[tris(1-methyl-1<i>H</i>-imidazol-2-yl)phosphine-\k^3^<i>N</i>^3^]iron(II)
 tetrachloroferrate(II) methanol tetrasolvate (<i>ca</i> 153K) and
 bis[tris(1-methyl-1<i>H</i>-imidazol-2-yl)methanol-\k^3^<i>N</i>^3^]iron(III)
 bis[tetrachloroferrate(III)] chloride (redetermination, <i>ca</i> 153K)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m311
_journal_page_last               m313
_journal_paper_doi               10.1107/S0108270104010868
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Fe (C13 H16 N6 O)2] [Fe Cl4]2 Cl'
_chemical_formula_moiety         'C26 H32 Fe N12 O2 3+, 2Cl4 Fe -, Cl 1-'
_chemical_formula_sum            'C26 H32 Cl9 Fe3 N12 O2'
_chemical_formula_weight         1031.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00000
_cell_angle_beta                 93.835(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   9.7792(9)
_cell_length_b                   14.8534(10)
_cell_length_c                   13.3529(17)
_cell_measurement_reflns_used    7062
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      2.4
_cell_volume                     1935.2(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    Xtal3.5
_computing_publication_material  'BONDLA and CIFIO in Xtal3.5'
_computing_structure_refinement  'CRYLSQ in Xtal3.5'
_computing_structure_solution
;
Xtal3.5 (Hall et al., 1995)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max .98
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .033
_diffrn_reflns_av_sigmaI/netI    .055
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38960
_diffrn_reflns_theta_full        37.5
_diffrn_reflns_theta_max         37.7
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.777
_exptl_absorpt_correction_T_max  .80
_exptl_absorpt_correction_T_min  .68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 (SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.77
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          .45
_exptl_crystal_size_mid          .45
_exptl_crystal_size_min          .4
_refine_diff_density_max         1.435
_refine_diff_density_min         -.78
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   .993
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     238
_refine_ls_number_reflns         7754
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .056
_refine_ls_R_factor_gt           .037
_refine_ls_shift/su_max          .007
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 w = 1/(\s^2^(F) +  0.003F^2^)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .075
_refine_ls_wR_factor_ref         .067
_reflns_number_gt                7754
_reflns_number_total             10066
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ta1445.cif
_cod_data_source_block           II
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2014271