Simultaneous manipulation of iron(II) spin crossover and LIESST behaviour using pressure, temperature and light.
Handzlik, Gabriela; Dziubek, Kamil F.; Hanfland, Michael; Pinkowicz, Dawid; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7677–7681; doi:10.1039/d4dt00509k

data_7715845
_publ_section_title
;
 Simultaneous manipulation of iron(II) spin crossover and LIESST behaviour
 using pressure, temperature and light.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7677
_journal_page_last               7681
_journal_paper_doi               10.1039/d4dt00509k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H32 Fe2 N24 Nb, 4(H2 O)'
_chemical_formula_sum            'C32 H40 Fe2 N24 Nb O4'
_chemical_formula_weight         1029.49
_chemical_name_systematic
'catena-[tetrakis(m2-Cyano)-octakis(1H-pyrazole-N2)-tetracyano-di-iron(ii)-niobium(iv) tetrahydrate]'
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-15 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0910(10)
_cell_length_b                   21.0910(10)
_cell_length_c                   9.378(2)
_cell_measurement_reflns_used    792
_cell_measurement_temperature    5.00
_cell_measurement_theta_max      19.8400
_cell_measurement_theta_min      1.7660
_cell_volume                     4171.6(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_pressure         820000
_diffrn_ambient_temperature      5.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.600
_diffrn_measured_fraction_theta_max 0.338
_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    -32.00  32.00   0.50    0.20    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003739000
_diffrn_orient_matrix_UB_12      0.0072572000
_diffrn_orient_matrix_UB_13      0.0405108000
_diffrn_orient_matrix_UB_21      0.0029107000
_diffrn_orient_matrix_UB_22      0.0178649000
_diffrn_orient_matrix_UB_23      -0.0160454000
_diffrn_orient_matrix_UB_31      -0.0192294000
_diffrn_orient_matrix_UB_32      0.0025583000
_diffrn_orient_matrix_UB_33      -0.0031677000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41008
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.1281
_diffrn_reflns_Laue_measured_fraction_full 0.600
_diffrn_reflns_Laue_measured_fraction_max 0.338
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3566
_diffrn_reflns_point_group_measured_fraction_full 0.600
_diffrn_reflns_point_group_measured_fraction_max 0.338
_diffrn_reflns_theta_full        14.244
_diffrn_reflns_theta_max         20.275
_diffrn_reflns_theta_min         1.767
_diffrn_source                   'ESRF ID15B'
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1782
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0787P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1177
_reflns_number_total             1782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00509k2.cif
_cod_data_source_block           fenb_0030
_cod_depositor_comments
'Adding full bibliography for 7715833--7715849.cif.'
_cod_original_cell_volume        4171.8(11)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7715845
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C11 H10 N O'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-H1
 0.95 with sigma of 0.02
 O1-H2
 0.95 with sigma of 0.02
 H1-H2
 1.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C8 \\sim C7 \\sim C6 \\sim N5 \\sim N6: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.016 within 2A
N3 \\sim C3 \\sim C4 \\sim C5 \\sim N4: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.016 within 2A
C2 \\sim N2: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016 within 2A
Uanis(C1) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
4.a Aromatic/amide H refined with riding coordinates:
 N4(H3), N6(H7), C8(H8), C5(H4), C7(H9), C4(H5), C3(H6), C6(H10)
;
_shelx_res_checksum              9211
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   468
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.279
_oxdiff_exptl_absorpt_empirical_full_min 0.480