Solvatomorphism, polymorphism and spin crossover in bis[hydrotris(1,2,3-triazol-1-yl)borate]iron(ii)
Horniichuk, Oleksandr Ye.; Ridier, Karl; Molnár, Gábor; Kotsyubynsky, Volodymyr O.; Shova, Sergiu; Amirkhanov, Vladimir M.; Gural'skiy, Il’ya A.; Salmon, Lionel; Bousseksou, Azzedine; New Journal of Chemistry 46 (2022) 11734–11740; doi:10.1039/D2NJ01471H

data_7061516
_publ_section_title
;
 Solvatomorphism, polymorphism and spin crossover in
 bis[hydrotris(1,2,3-triazol-1-yl)borate]iron(ii)
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11734
_journal_page_last               11740
_journal_paper_doi               10.1039/D2NJ01471H
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C12 H14 B2 Fe N18, 2(C H Cl3)'
_chemical_formula_sum            'C14 H16 B2 Cl6 Fe N18'
_chemical_formula_weight         726.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-25 deposited with the CCDC.	2022-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.973(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2460(4)
_cell_length_b                   12.1991(4)
_cell_length_c                   14.6014(6)
_cell_measurement_reflns_used    3810
_cell_measurement_temperature    180.00(14)
_cell_measurement_theta_max      28.4840
_cell_measurement_theta_min      2.2070
_cell_volume                     1412.10(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.875
_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    -69.00   0.00   1.00  125.00    --  -20.11 110.00  55.00   69
  2  \w     -2.00  73.00   1.00  125.00    --   22.22-110.00 -39.00   75
  3  \w    -95.00 -69.00   1.00  125.00    --  -20.11-178.00  90.00   26
  4  \w    -33.00  -7.00   1.00  125.00    --  -20.11 -77.00 150.00   26
  5  \w    -50.00   2.00   1.00  125.00    --  -20.11  38.00 -90.00   52
  6  \w     21.00  52.00   1.00  125.00    --  -20.11  38.00 -90.00   31
  7  \w     -1.00  90.00   1.00  125.00    --   22.22  57.00 150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0101215000
_diffrn_orient_matrix_UB_12      -0.0563568000
_diffrn_orient_matrix_UB_13      -0.0089699000
_diffrn_orient_matrix_UB_21      -0.0885132000
_diffrn_orient_matrix_UB_22      -0.0076484000
_diffrn_orient_matrix_UB_23      -0.0104977000
_diffrn_orient_matrix_UB_31      -0.0085059000
_diffrn_orient_matrix_UB_32      0.0120454000
_diffrn_orient_matrix_UB_33      -0.0486238000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9532
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.907
_diffrn_reflns_theta_min         2.212
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3251
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+1.7120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2740
_reflns_number_total             3251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01471h2.cif
_cod_data_source_block           shi_4730_ilgu
_cod_depositor_comments
'Adding full bibliography for 7061516--7061521.cif.'
_cod_original_cell_volume        1412.11(10)
_cod_database_code               7061516
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C15H15N12B1Fe1Cl3
_chemical_oxdiff_usercomment     HO-404CHCl3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.847
_diffrn_oxdiff_digest_frames
;
01c127d97795453e5699317a2692ba20be003889522
;
_diffrn_oxdiff_digest_hkl
;
01379af3ea8ebb51e6dfa1b02a51161b023ef0
;
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 B1-H1
 1.1 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C7(H7)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C6(H6), C5(H5), C2(H2), C1(H1A)
;
_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 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.786