#------------------------------------------------------------------------------
#$Date: 2023-07-05 12:07:14 +0200 (Wed 05 de Jul de 2023) $
#$Revision: 284916 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/68/7246817.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7246817
loop_
_publ_author_name
'Valverde-Muñoz, Francisco Javier'
'Torres Ramírez, Ricardo Guillermo'
'Ulhe, Abhilash'
'Trzop, Elzbieta'
'Dutta, Mousumi'
'Das, Chinmoy'
'Chakraborty, Pradip'
'Collet, Eric'
_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
_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                   10.7307(2)
_cell_length_b                   10.7307(2)
_cell_length_c                   31.9228(9)
_cell_measurement_reflns_used    4793
_cell_measurement_temperature    80.40(12)
_cell_measurement_theta_max      33.3460
_cell_measurement_theta_min      3.3530
_cell_volume                     3183.37(12)
_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      80.40(12)
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00  40.00   1.00   22.50    --    1.02 -99.00 -60.00   27
  2  ω    -20.00   7.00   1.00   22.50    --    1.02  77.00 -60.00   27
  3  ω     11.00  37.00   1.00   45.00    --  -33.66  77.00 120.00   26
  4  ω     53.00 104.00   1.00   45.00    --   35.69  57.00   0.00   51
  5  ω     80.00 106.00   1.00   45.00    --   35.69  57.00-120.00   26
  6  ω    -20.00  64.00   1.00   45.00    --   35.69 -99.00 -30.00   84
  7  ω     -7.00  79.00   1.00   45.00    --   35.69 -99.00  60.00   86
  8  ω    -34.00  46.00   1.00   45.00    --   35.69 -57.00-150.00   80
  9  ω     47.00  75.00   1.00   45.00    --   35.69 178.00 -90.00   28
 10  ω     14.00  69.00   1.00   45.00    --   35.69 -77.00 120.00   55
 11  ω     41.00  66.00   1.00   45.00    --   35.69 178.00-120.00   25
 12  ω     89.00 114.00   1.00   45.00    --   35.69 178.00 -30.00   25
 13  ω     37.00 109.00   1.00   45.00    --   35.69  38.00 120.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0060669897
_diffrn_orient_matrix_UB_12      0.0112332589
_diffrn_orient_matrix_UB_13      0.0219712157
_diffrn_orient_matrix_UB_21      -0.0593648414
_diffrn_orient_matrix_UB_22      -0.0702161080
_diffrn_orient_matrix_UB_23      0.0031017260
_diffrn_orient_matrix_UB_31      0.0476138318
_diffrn_orient_matrix_UB_32      -0.0277614263
_diffrn_orient_matrix_UB_33      0.0010471512
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0230
_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       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            11126
_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         26.995
_diffrn_reflns_theta_min         3.365
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.903
_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    1.437
_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         0.722
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0302
_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/[σ²(Fo²)+(0.0189P)²+4.7171P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1471
_reflns_number_total             1545
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce00365e1.cif
_cod_data_source_block           FeRuptz_BF4_80K_quench
_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        3183.37(15)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7246817
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C24 H48 B2 F8 Fe0.65 Ru0.35 N24'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.885
_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(Fe1) = Uanis(Ru1)
4. Others
 Fixed Sof: Fe1(0.10833) Ru1(0.05833)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_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 1.054
_oxdiff_exptl_absorpt_empirical_full_min 0.935
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.6667 0.3333 0.3333 0.00646(10) Uani 0.65 6 d S T P A 3
F2 F 0.90472(10) 0.86256(10) 0.33234(3) 0.0306(3) Uani 1 1 d . . . . .
N1 N 0.71458(12) 0.50648(12) 0.36959(4) 0.0136(3) Uani 1 1 d . . . . .
F1 F 1.0000 1.0000 0.27463(5) 0.0335(4) Uani 1 3 d S T P . .
N4 N 0.72096(13) 0.68820(12) 0.39991(4) 0.0144(3) Uani 1 1 d . . . . .
N3 N 0.83555(13) 0.68072(14) 0.41378(4) 0.0191(3) Uani 1 1 d . . . . .
N2 N 0.83148(13) 0.57066(13) 0.39554(4) 0.0182(3) Uani 1 1 d . . . . .
C1 C 0.64830(15) 0.58185(15) 0.37306(4) 0.0141(3) Uani 1 1 d . . . . .
H1 H 0.5630 0.5630 0.3587 0.017 Uiso 1 1 calc R U . . .
C2 C 0.69834(17) 0.80788(16) 0.41188(5) 0.0183(3) Uani 1 1 d . . . . .
H2A H 0.6114 0.7965 0.3976 0.022 Uiso 1 1 calc R U . . .
H2B H 0.7815 0.8997 0.4024 0.022 Uiso 1 1 calc R U . . .
C3 C 0.68056(18) 0.81420(17) 0.45870(5) 0.0216(3) Uani 1 1 d . . . . .
H3A H 0.6652 0.8958 0.4651 0.026 Uiso 1 1 calc R U . . .
H3B H 0.7705 0.8327 0.4728 0.026 Uiso 1 1 calc R U . . .
C4 C 0.55574(19) 0.67701(19) 0.47634(5) 0.0275(4) Uani 1 1 d . . . . .
H4A H 0.4668 0.6558 0.4618 0.041 Uiso 1 1 calc R U . . .
H4B H 0.5457 0.6896 0.5063 0.041 Uiso 1 1 calc R U . . .
H4C H 0.5741 0.5971 0.4723 0.041 Uiso 1 1 calc R U . . .
B1 B 1.0000 1.0000 0.31801(10) 0.0165(6) Uani 1 3 d S T P . .
Ru1 Ru 0.6667 0.3333 0.3333 0.00646(10) Uani 0.35 6 d S T P A 4
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -12 -6 0.1599
1 13 1 0.1166
-14 12 -2 0.0885
-14 2 -3 0.0916
12 1 3 0.1091
15 -9 2 0.0939
-1 0 45 0.0098
1 0 -45 0.0180
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 90.56(5) 16_655 17 ?
N1 Fe1 N1 89.43(5) 17 3_665 ?
N1 Fe1 N1 180.0 17 2_655 ?
N1 Fe1 N1 90.57(5) 3_665 2_655 ?
N1 Fe1 N1 90.57(5) 2_655 . ?
N1 Fe1 N1 89.43(5) 16_655 2_655 ?
N1 Fe1 N1 90.57(5) 16_655 18_545 ?
N1 Fe1 N1 89.43(5) 18_545 2_655 ?
N1 Fe1 N1 180.0 16_655 . ?
N1 Fe1 N1 89.43(5) 18_545 . ?
N1 Fe1 N1 89.43(5) 17 . ?
N1 Fe1 N1 90.57(5) 3_665 . ?
N1 Fe1 N1 180.0 18_545 3_665 ?
N1 Fe1 N1 89.43(5) 16_655 3_665 ?
N1 Fe1 N1 90.57(5) 17 18_545 ?
N2 N1 Fe1 123.81(9) . . ?
C1 N1 Fe1 129.92(10) . . ?
C1 N1 N2 106.25(12) . . ?
N3 N4 C2 121.38(12) . . ?
C1 N4 N3 108.85(12) . . ?
C1 N4 C2 129.55(12) . . ?
N2 N3 N4 106.90(12) . . ?
N3 N2 N1 109.57(11) . . ?
N1 C1 N4 108.43(13) . . ?
N1 C1 H1 125.8 . . ?
N4 C1 H1 125.8 . . ?
N4 C2 H2A 109.2 . . ?
N4 C2 H2B 109.2 . . ?
N4 C2 C3 112.04(12) . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
C2 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C2 C3 C4 113.13(13) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
F2 B1 F2 109.68(13) 2_765 . ?
F2 B1 F2 109.68(13) 3_675 . ?
F2 B1 F2 109.68(13) 2_765 3_675 ?
F1 B1 F2 109.26(13) . . ?
F1 B1 F2 109.26(13) . 2_765 ?
F1 B1 F2 109.26(13) . 3_675 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.0252(12) 16_655 ?
Fe1 N1 2.0252(12) 3_665 ?
Fe1 N1 2.0252(12) 2_655 ?
Fe1 N1 2.0252(12) 18_545 ?
Fe1 N1 2.0252(12) 17 ?
Fe1 N1 2.0252(12) . ?
F2 B1 1.3862(14) . ?
N1 N2 1.3676(17) . ?
N1 C1 1.3219(18) . ?
F1 B1 1.385(3) . ?
N4 N3 1.3465(17) . ?
N4 C1 1.3249(18) . ?
N4 C2 1.4717(18) . ?
N3 N2 1.2976(17) . ?
C1 H1 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.513(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.519(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
B1 F2 1.3861(14) 3_675 ?
B1 F2 1.3861(14) 2_765 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 N2 N3 178.35(9) . . . . ?
Fe1 N1 C1 N4 -178.37(9) . . . . ?
N4 N3 N2 N1 0.27(16) . . . . ?
N4 C2 C3 C4 -58.40(17) . . . . ?
N3 N4 C1 N1 0.07(16) . . . . ?
N3 N4 C2 C3 -61.46(18) . . . . ?
N2 N1 C1 N4 0.10(16) . . . . ?
C1 N1 N2 N3 -0.23(16) . . . . ?
C1 N4 N3 N2 -0.21(16) . . . . ?
C1 N4 C2 C3 124.61(16) . . . . ?
C2 N4 N3 N2 -175.27(13) . . . . ?
C2 N4 C1 N1 174.59(13) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.5385 -12.1485 -5.9168 -0.2758 0.9260 0.2578
0.5427 12.8155 1.2031 0.1737 -0.9283 -0.3287
-13.9190 12.0601 -1.9836 0.0074 -0.0267 -0.9996
-14.0933 2.3611 -2.8432 -0.1214 0.6620 -0.7396
12.2950 1.4395 2.7769 0.1518 -0.8224 0.5484
15.0311 -8.8028 2.4998 0.0472 -0.2665 0.9627
-0.7744 0.0331 44.9401 0.9831 0.1830 0.0093
0.7744 -0.0331 -44.9401 -0.9831 -0.1830 -0.0093
