Interplay of halogen and hydrogen bonding in a series of heteroleptic iron(iii) complexes
Díaz-Torres, Raúl; Echeverría, Jorge; Loveday, Oliver; Harding, Phimphaka; Harding, David J.; CrystEngComm 23 (2021) 4069–4076; doi:10.1039/D1CE00480H

data_7242861
_publ_section_title
;
 Interplay of halogen and hydrogen bonding in a series of heteroleptic
 iron(iii) complexes
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4069
_journal_page_last               4076
_journal_paper_doi               10.1039/D1CE00480H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C23 H13 Br Fe N3 O5, C H4 O'
_chemical_formula_sum            'C24 H17 Br Fe N3 O6'
_chemical_formula_weight         579.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-06
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-04-05 deposited with the CCDC.	2021-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.8010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.20560(10)
_cell_length_b                   9.30670(10)
_cell_length_c                   18.8067(2)
_cell_measurement_reflns_used    11208
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      68.2200
_cell_measurement_theta_min      4.1540
_cell_volume                     2128.83(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_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   -103.00  35.00   0.50    0.80    --  -40.91   4.00 -98.00  276
  2  \w    -21.00 117.00   0.50    0.80    --   40.91   4.00 -98.00  276
  3  \w     21.00 157.00   0.50    2.70    --   96.59  -4.00  84.00  272
  4  \w     35.00 157.00   0.50    2.70    --   96.59   4.00 -98.00  244
  5  \w    -41.00 -15.00   0.50    0.80    --  -40.91 -78.00 175.76   52
  6  \w    -53.00  23.00   0.50    0.80    --  -40.91  37.00 -30.00  152
  7  \w   -104.00 -25.00   0.50    0.80    --  -40.91 -50.00 150.00  158
  8  \w   -117.00  21.00   0.50    0.80    --  -40.91  -4.00  84.00  276
  9  \w     21.00 105.00   0.50    0.80    --   40.91  63.00  30.00  168
 10  \w     15.00  42.00   0.50    0.80    --   40.91  82.00 -28.83   54
 11  \w     15.00  42.00   0.50    0.80    --   40.91  81.00 166.72   54
 12  \w    -13.00  77.00   0.50    0.80    --   40.91-104.00  90.00  180
 13  \w     29.00 105.00   0.50    0.80    --   40.91  37.00 120.00  152
 14  \w    -35.00 103.00   0.50    0.80    --   40.91  -4.00  84.00  276
 15  \w     15.00  42.00   0.50    0.80    --   40.91  81.00   3.32   54
 16  \w     14.00  97.00   0.50    0.80    --   40.91-138.00 -30.00  166
 17  \w     88.00 157.00   0.50    2.70    --   96.59  25.00 -60.00  138
 18  \w     32.00 109.00   0.50    2.70    --   96.59-117.00  30.00  154
 19  \w     32.00 109.00   0.50    2.70    --   96.59-117.00  60.00  154
 20  \w     32.00 109.00   0.50    2.70    --   96.59-117.00 120.00  154
 21  \w     27.00 100.00   0.50    2.70    --   96.59 -96.00 150.00  146
 22  \w     37.00  93.00   0.50    2.70    --   96.59-117.00-180.00  112
 23  \w     29.00 104.00   0.50    2.70    --   96.59 -25.00 150.00  150
 24  \w     31.00 106.00   0.50    2.70    --   96.59 -33.00-120.00  150
 25  \w     64.00 107.00   0.50    2.70    --   96.59 -59.00   0.00   86
 26  \w     89.00 139.00   0.50    2.70    --   96.59  25.00   0.00  100
 27  \w     52.00 109.00   0.50    2.70    --   96.59-117.00 -30.00  114
 28  \w     67.00 104.00   0.50    2.70    --   96.59 -77.00   0.00   74
 29  \w     34.00 103.00   0.50    2.70    --   96.59 -50.00 150.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0065133000
_diffrn_orient_matrix_UB_12      -0.0085535000
_diffrn_orient_matrix_UB_13      -0.0820799000
_diffrn_orient_matrix_UB_21      0.1264976000
_diffrn_orient_matrix_UB_22      0.0012082000
_diffrn_orient_matrix_UB_23      0.0026172000
_diffrn_orient_matrix_UB_31      0.0012698000
_diffrn_orient_matrix_UB_32      -0.1652456000
_diffrn_orient_matrix_UB_33      0.0041744000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17206
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.509
_diffrn_reflns_theta_min         4.164
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
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    1.807
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.920
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         3905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0790P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3540
_reflns_number_total             3905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00480h2.cif
_cod_data_source_block           rdt116-150k
_cod_depositor_comments
'Adding full bibliography for 7242858--7242861.cif.'
_cod_database_code               7242861
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C24H17FeBrN3O6
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C14(H14),
 C15(H15), C19(H19), C20(H20), C21(H21)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
2.c Idealised tetrahedral OH refined as rotating group:
 O6(H6A)
;
_shelx_res_checksum              38683
_shelx_hkl_checksum              84115
_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 2.600
_oxdiff_exptl_absorpt_empirical_full_min 0.349