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_7061521
_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 H4 O)'
_chemical_formula_sum            'C14 H22 B2 Fe N18 O2'
_chemical_formula_weight         551.96
_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   mixed
_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                 99.208(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4567(8)
_cell_length_b                   8.2415(5)
_cell_length_c                   13.9101(8)
_cell_measurement_reflns_used    1952
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      25.6300
_cell_measurement_theta_min      2.2670
_cell_volume                     1183.31(14)
_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 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)'
_diffrn_ambient_temperature      180
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -63.00   7.00   1.00   30.00    --  -15.37 114.00 124.00   70
  2  \w      4.00  29.00   1.00   30.00    --   17.79-114.00  33.00   25
  3  \w    -19.00  10.00   1.00   30.00    --  -15.37 -77.00 -60.00   29
  4  \w      1.00  27.00   1.00   30.00    --   17.79  57.00 -60.00   26
  5  \w     13.00  85.00   1.00   30.00    --   17.79  57.00  30.00   72
  6  \w     -9.00  39.00   1.00   30.00    --   17.79  77.00 -60.00   48
  7  \w     34.00  73.00   1.00   30.00    --   17.79  57.00-120.00   39
  8  \w     41.00  67.00   1.00   30.00    --   17.79  57.00 -60.00   26
  9  \w      4.00  30.00   1.00   30.00    --   17.79  57.00-120.00   26
;
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8240
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.271
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94350
_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    1.549
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2322
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0233P)^2^+0.6937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1868
_reflns_number_total             2322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01471h2.cif
_cod_data_source_block           shi_4731_ilgu
_cod_depositor_comments
'Adding full bibliography for 7061516--7061521.cif.'
_cod_database_code               7061521
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.819
_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. Restrained distances
 B1-H1
 1.1 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C1(H1A), C2(H2), C4(H4), C3(H3)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1B)
;
_shelx_res_checksum              27321
_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
;