Crystal structure of 4-(5,5-difluoro-1,3,7,9-tetramethyl-3H,5H-5λ4-dipyrrolo[1,2-c:2′,1′-f][1,3,2]diazaborinin-10-yl)pyridin-1-ium tetraiodidoferrate(III), C18H19BF2FeI4N3
Gao, Yan; Xiao, Zhiyin; Zhang, Peipei; Xiang, Yali; Wang, Wei; Hu, Haimeng; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1015–1016; doi:10.1515/ncrs-2019-0226

data_8105922
_publ_section_title
;
 Crystal structure of
 4-(5,5-difluoro-1,3,7,9-tetramethyl-3H,5H-5\l4-dipyrrolo[1,2-c:2&#x2032;,1&#x2032;-f][1,3,2]diazaborinin-10-yl)pyridin-1-ium
 tetraiodidoferrate(III), C18H19BF2FeI4N3
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1015
_journal_page_last               1016
_journal_paper_doi               10.1515/ncrs-2019-0226
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'Fe I4, C18 H19 B F2 N3'
_chemical_formula_sum            'C18 H19 B F2 Fe I4 N3'
_chemical_formula_weight         889.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                106.388(5)
_cell_angle_beta                 101.841(4)
_cell_angle_gamma                95.200(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2997(3)
_cell_length_b                   11.8180(9)
_cell_length_c                   14.0849(7)
_cell_measurement_reflns_used    2720
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4650
_cell_measurement_theta_min      3.4610
_cell_volume                     1280.87(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -25.00  18.20   0.60   45.00    --  -15.74 -99.00-180.00   72
  2  \w    -14.00  12.40   0.60   45.00    --  -15.74 -99.00  30.00   44
  3  \w    -53.00  33.40   0.60   45.00    --   16.05 -38.00-120.00  144
  4  \w     44.00  86.00   0.60   45.00    --   16.05 178.00-180.00   70
  5  \w     12.00  84.00   0.60   45.00    --   16.05  38.00  60.00  120
  6  \w     10.00  40.60   0.60   45.00    --   16.05 -77.00 -60.00   51
  7  \w    -13.00  62.60   0.60   45.00    --   16.05  19.00-120.00  126
;
_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      -0.0269187000
_diffrn_orient_matrix_UB_12      -0.0388849000
_diffrn_orient_matrix_UB_13      -0.0507875000
_diffrn_orient_matrix_UB_21      -0.0037145000
_diffrn_orient_matrix_UB_22      0.0500210000
_diffrn_orient_matrix_UB_23      -0.0183201000
_diffrn_orient_matrix_UB_31      0.0841532000
_diffrn_orient_matrix_UB_32      0.0003008000
_diffrn_orient_matrix_UB_33      -0.0033250000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9106
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.733
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.433
_exptl_absorpt_correction_T_max  0.581
_exptl_absorpt_correction_T_min  0.526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.307
_exptl_crystal_description       needle
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.278
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0508P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1045
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3386
_reflns_number_total             4499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0226_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1280.88(13)
_cod_database_code               8105922
_chemical_oxdiff_formula         'C18 H19 B F2 Fe I4 N3'
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.139
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C4(H4), C2(H2), C1(H1), C12(H12)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              77980