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_7246816
_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(B1 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      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_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
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.8178(3)
_cell_length_b                   10.8178(3)
_cell_length_c                   33.0213(13)
_cell_measurement_reflns_used    3625
_cell_measurement_temperature    250.0(3)
_cell_measurement_theta_max      23.6270
_cell_measurement_theta_min      3.2740
_cell_volume                     3346.59(19)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -14.00  13.00   1.00   22.50    --    1.02  77.00-120.00   27
  2  \w      8.00  35.00   1.00   22.50    --    1.02 -99.00 150.00   27
  3  \w    -95.00 -38.00   1.00   45.00    --  -33.66 178.00 -90.00   57
  4  \w     21.00 106.00   1.00   45.00    --   35.69  57.00-180.00   85
  5  \w     55.00  80.00   1.00   45.00    --   35.69 -99.00   0.00   25
  6  \w     13.00  94.00   1.00   45.00    --   35.69  57.00-120.00   81
  7  \w    -19.00  29.00   1.00   45.00    --   35.69 -99.00   0.00   48
  8  \w     19.00  77.00   1.00   45.00    --   35.69 -99.00  90.00   58
  9  \w      9.00  99.00   1.00   45.00    --   35.69-136.00 -23.00   90
 10  \w    -17.00 111.00   1.00   45.00    --   35.69  19.00 150.00  128
;
_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      0.0082949000
_diffrn_orient_matrix_UB_12      0.0106971000
_diffrn_orient_matrix_UB_13      0.0212432000
_diffrn_orient_matrix_UB_21      -0.0584252000
_diffrn_orient_matrix_UB_22      -0.0698002000
_diffrn_orient_matrix_UB_23      0.0031765000
_diffrn_orient_matrix_UB_31      0.0474331000
_diffrn_orient_matrix_UB_32      -0.0273596000
_diffrn_orient_matrix_UB_33      0.0002035000
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            12171
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.983
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.904
_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    1.367
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             1423
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1629
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0523P)^2^+4.8683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1503
_reflns_number_total             1629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00365e1.cif
_cod_data_source_block           FeRuptz_BF4_250K
_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        3346.6(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7246816
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C24 H48 B2 F8 Fe0.64 Ru0.36 N24'
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.890
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Fe1, Ru1}
3. Restrained distances
 C3'-C4'
 1.55 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(F2') \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F1')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4') \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Fe1) = Uanis(Ru1)
5. Others
 Sof(H2AA)=Sof(H2AB)=Sof(C4')=Sof(H4'A)=Sof(H4'B)=Sof(H4'C)=Sof(C3')=Sof(H3'A)=
 Sof(H3'B)=1-FVAR(1)
 Sof(H2BC)=Sof(H2BD)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(H4C)=FVAR(1)
 Fixed Sof: Fe1(0.10833) F2'(0.36) F1(0.21333) F2(0.64) F1'(0.12) Ru1(0.05833)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2BC,H2BD), C2(H2AA,H2AB), C3(H3A,H3B), C3'(H3'A,H3'B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
6.c Idealised Me refined as rotating group:
 C4'(H4'A,H4'B,H4'C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              40588
_shelx_hkl_checksum              5302
_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 1.041
_oxdiff_exptl_absorpt_empirical_full_min 0.963