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_7061517
_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 Fe1 N18, 7(C2 H6 O S)'
_chemical_formula_sum            'C26 H56 B2 Fe N18 O7 S7'
_chemical_formula_weight         1034.77
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-04-25
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.04.21 svn.rca3783a0 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-05-08 deposited with the CCDC.	2022-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.3415(3)
_cell_length_b                   13.3415(3)
_cell_length_c                   48.9618(11)
_cell_measurement_reflns_used    3237
_cell_measurement_temperature    159.9(2)
_cell_measurement_theta_max      28.6160
_cell_measurement_theta_min      1.9640
_cell_volume                     7547.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      159.9(2)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.910
_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      0.00  35.00   1.00  100.00    --   22.22  77.00 -30.00   35
  2  \w     18.00  88.00   1.00  100.00    --   22.22  57.00  60.00   70
  3  \w    -37.00  87.00   1.00  100.00    --   22.22   0.00  60.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            10071
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.875
_diffrn_reflns_theta_min         1.949
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense red'
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       prism
_exptl_crystal_F_000             3252
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2021
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0435P)^2^+19.4875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1677
_reflns_number_total             2021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01471h2.cif
_cod_data_source_block           shi_5192_ilgu_autored
_cod_depositor_comments
'Adding full bibliography for 7061516--7061521.cif.'
_cod_original_cell_volume        7547.4(4)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7061517
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 B1-H1A
 1.1 with sigma of 0.02
3. Others
 Fixed Sof: S1A(0.83) O1B(0.17) H3AA(0.83) H3AB(0.83) H3AC(0.83) H3BD(0.17)
 H3BE(0.17) H3BF(0.17) H4AA(0.83) H4AB(0.83) H4AC(0.83) H4BD(0.17) H4BE(0.17)
 H4BF(0.17) S1B(0.17) O1A(0.83) S2(0.16667) O2(0.16667) C5(0.33335)
 H5A(0.33335) H5B(0.33335) H5C(0.33335)
4.a Ternary CH refined with riding coordinates and stretchable bonds:
 B1(H1A)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
4.c Idealised Me refined as rotating group:
 C3(H3AA,H3AB,H3AC), C3(H3BD,H3BE,H3BF), C4(H4AA,H4AB,H4AC), C4(H4BD,H4BE,
 H4BF), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              10219
_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
;