Crystal structure of tris(2,2′-bipyridine-κ2 N,N′)iron(II) triiodide – dichloromethane (2/1), C61H50Cl2Fe2I12N12
Cui, Chuanguo; Zhang, Jinxiao; Xiao, Zhiyin; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 541–543; doi:10.1515/ncrs-2023-0075

data_8107489
_publ_section_title
;
 Crystal structure of tris(2,2&#x2032;-bipyridine-\k2 N,N&#x2032;)iron(II)
 triiodide&#x00A0;-- dichloromethane (2/1), C61H50Cl2Fe2I12N12
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              541
_journal_page_last               543
_journal_paper_doi               10.1515/ncrs-2023-0075
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         '2(C30 H24 Fe N6), C H2 Cl2, 4(I3)'
_chemical_formula_sum            'C61 H50 Cl2 Fe2 I12 N12'
_chemical_formula_weight         2656.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0247(4)
_cell_length_b                   17.0204(5)
_cell_length_c                   34.1475(9)
_cell_measurement_reflns_used    13138
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9390
_cell_measurement_theta_min      3.3910
_cell_volume                     7570.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -10.00  22.10   0.30    3.64    --  -15.74 -99.00 -30.00  107
  2  \w    -19.00   7.10   0.30    3.64    --  -15.74 -99.00 150.00   87
  3  \w    -22.00  20.00   0.30    3.64    --  -15.74 -99.00-120.00  140
  4  \w     -1.00  84.20   0.30    3.64    --   16.05  38.00 150.00  284
  5  \w     41.00  87.20   0.30    3.64    --   16.05 178.00 -60.00  154
  6  \w    -44.00  22.00   0.30    3.64    --   16.05 -57.00 -30.00  220
  7  \w     36.00  64.20   0.30    3.64    --   16.05-178.00   0.00   94
  8  \w    -14.00  38.20   0.30    3.64    --   16.05 -19.00 -30.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0543007000
_diffrn_orient_matrix_UB_12      0.0025435000
_diffrn_orient_matrix_UB_13      -0.0009464000
_diffrn_orient_matrix_UB_21      0.0032015000
_diffrn_orient_matrix_UB_22      0.0415628000
_diffrn_orient_matrix_UB_23      0.0010548000
_diffrn_orient_matrix_UB_31      0.0026564000
_diffrn_orient_matrix_UB_32      0.0019726000
_diffrn_orient_matrix_UB_33      -0.0207157000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            56694
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.853
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.331
_exptl_crystal_description       block
_exptl_crystal_F_000             4888
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0469P)^2^+81.1965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6480
_reflns_number_total             7815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0075_suppl_001.cif
_cod_data_source_block           230219
_cod_database_code               8107489
_chemical_oxdiff_formula         'Fe I C H O N'
_shelx_estimated_absorpt_t_max   0.498
_shelx_estimated_absorpt_t_min   0.112
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: H31a(0.5) H31b(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C31(H31a,H31b)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30)
;
_shelx_res_checksum              40784
_shelx_hkl_checksum              85595
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.814
_oxdiff_exptl_absorpt_empirical_full_min 0.692