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_7061520
_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(C3 H7 N O), H2 O'
_chemical_formula_sum            'C18 H30 B2 Fe N20 O3'
_chemical_formula_weight         652.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3469(5)
_cell_length_b                   15.7421(7)
_cell_length_c                   22.5116(9)
_cell_measurement_reflns_used    1894
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.8950
_cell_measurement_theta_min      2.7450
_cell_volume                     2958.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1593
_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      1.00  28.00   1.00   30.00    --   17.79  57.00  41.00   27
  2  \w     14.00  74.00   1.00   30.00    --   17.79-134.00-152.00   60
  3  \w    -87.00 -60.00   1.00   30.00    --  -15.29 178.00 -60.00   27
  4  \w     -8.00  36.00   1.00   30.00    --  -15.29  77.00-120.00   44
  5  \w     -8.00  37.00   1.00   30.00    --   17.79  77.00 -90.00   45
;
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10062
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.588
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (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    1.464
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0352P)^2^+0.8011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1804
_reflns_number_total             2601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01471h2.cif
_cod_data_source_block           shi_4813_igfr
_cod_depositor_comments
'Adding full bibliography for 7061516--7061521.cif.'
_cod_database_code               7061520
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.857
_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 O(H) groups
2.a Riding coordinates:
 B1(H1A), O2(H2A)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C1(H1), C2(H2), C4(H4), C3(H3), C7(H7)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              44264
_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
;