Ferroelastic phase transition and the role of volume strain in the structural trapping of a metastable quenched low-spin high-symmetry phase in [Ru0.35Fe0.65(ptz)6](BF4)2
Valverde-Muñoz, Francisco Javier; Torres Ramírez, Ricardo Guillermo; Ulhe, Abhilash; Trzop, Elzbieta; Dutta, Mousumi; Das, Chinmoy; Chakraborty, Pradip; Collet, Eric; CrystEngComm 25 (2023) 3588–3597; doi:10.1039/D3CE00365E

data_7246818
_publ_section_title
;
 Ferroelastic phase transition and the role of volume strain in the
 structural trapping of a metastable quenched low-spin high-symmetry phase
 in [Ru0.35Fe0.65(ptz)6](BF4)2
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              3588
_journal_page_last               3597
_journal_paper_doi               10.1039/D3CE00365E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C24 H48 Fe0.65 N24 Ru0.35, 2(B F4)'
_chemical_formula_sum            'C24 H48 B2 F8 Fe0.65 N24 Ru0.35'
_chemical_formula_weight         918.16
_chemical_melting_point          ?
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-04-13 deposited with the CCDC.	2023-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.927(7)
_cell_angle_beta                 131.808(15)
_cell_angle_gamma                89.563(7)
_cell_formula_units_Z            2
_cell_length_a                   11.7873(13)
_cell_length_b                   10.8372(6)
_cell_length_c                   21.595(3)
_cell_measurement_reflns_used    2716
_cell_measurement_temperature    80.7(7)
_cell_measurement_theta_max      26.2510
_cell_measurement_theta_min      3.3930
_cell_volume                     2055.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Mercury 2022.3.0 (Macrae et al., 2020)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      80.7(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.995
_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   22.50    --    1.02  77.00  60.00   27
  2  \w   -115.00 -71.00   1.00   45.00    --  -33.81 178.00   0.00   44
  3  \w      0.00  35.00   1.00   45.00    --  -33.81  57.00   0.00   35
  4  \w   -104.00 -71.00   1.00   45.00    --  -33.81 -57.00-150.00   33
  5  \w     25.00 103.00   1.00   45.00    --   35.84  57.00  90.00   78
  6  \w    -37.00  17.00   1.00   45.00    --   35.84 -77.00-120.00   54
  7  \w    -14.00  81.00   1.00   45.00    --   35.84 -99.00-180.00   95
  8  \w      9.00 106.00   1.00   45.00    --   35.84  38.00 -30.00   97
  9  \w     37.00  68.00   1.00   45.00    --   35.84 -77.00-120.00   31
 10  \w     12.00  65.00   1.00   45.00    --   35.84 -77.00 -30.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0308191699
_diffrn_orient_matrix_UB_12      -0.0079126153
_diffrn_orient_matrix_UB_13      -0.0189401549
_diffrn_orient_matrix_UB_21      -0.0560058694
_diffrn_orient_matrix_UB_22      0.0401936050
_diffrn_orient_matrix_UB_23      -0.0322572751
_diffrn_orient_matrix_UB_31      0.0493046407
_diffrn_orient_matrix_UB_32      0.0510573930
_diffrn_orient_matrix_UB_33      0.0232998059
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1395
_diffrn_reflns_av_unetI/netI     0.2120
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16124
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.838
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.462
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             949
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.362
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         7181
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1539
_refine_ls_R_factor_gt           0.0753
_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^)+(0.0557P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3516
_reflns_number_total             7181
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -119.4745\% 
around [-0.44 -0.01 0.90] (reciprocal) or [-0.74 -0.02 0.67] (direct)
Component 3 rotated by 179.5295\% 
around [0.53 -0.58 0.62] (reciprocal) or [0.82 -0.40 0.41] (direct)
;
_cod_data_source_file            d3ce00365e1.cif
_cod_data_source_block           FeRuptz_BF4_80K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7246816--7246818.cif.
;
_cod_original_cell_volume        2055.9(5)
_cod_database_code               7246818
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C24 H48 B2 F8 Fe0.64 N24 Ru0.36'
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.881
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Fe1, Ru1}
3. Uiso/Uaniso restraints and constraints
Uanis(N1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2D) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Fe1) = Uanis(Ru1)
4. Others
 Fixed Sof: Fe1(0.65) Ru1(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C3F(H3FA,H3FB), C3E(H3EA,H3EB), C2A(H2AA,H2AB), C2F(H2FA,H2FB), C2E(H2EA,
 H2EB), C2D(H2DA,H2DB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3D(H3DA,H3DB),
 C3C(H3CA,H3CB), C3B(H3BA,H3BB), C2C(H2CA,H2CB)
5.b Aromatic/amide H refined with riding coordinates:
 C1E(H1E), C1F(H1F), C1B(H1B), C1D(H1D), C1C(H1C), C1A(H1A)
5.c Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C4B(H4BA,H4BB,H4BC), C4C(H4CA,H4CB,H4CC), C4E(H4EA,H4EB,
 H4EC), C4D(H4DA,H4DB,H4DC), C4F(H4FA,H4FB,H4FC)
;
_shelx_res_checksum              96951
_shelx_hkl_checksum              51732
_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 1.065
_oxdiff_exptl_absorpt_empirical_full_min 0.949
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3