#------------------------------------------------------------------------------
#$Date: 2022-02-04 22:04:19 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272786 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/40/7244030.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_7244030
loop_
_publ_author_name
'Chakraborty, Pradip'
'Sy, Mouhamadou'
'Fourati, Houcem'
'Delgado, Teresa'
'Dutta, Mousumi'
'Das, Chinmoy'
'Besnard, Céline'
'Hauser, Andreas'
'Enachescu, Cristian'
'Boukheddaden, Kamel'
_publ_section_title
;
 Optical microscopy imaging of the thermally-induced spin transition and
 isothermal multi-stepped relaxation in a low-spin stabilized
 spin-crossover material.
;
_journal_issue                   2
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              982
_journal_page_last               994
_journal_paper_doi               10.1039/d1cp04321h
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C24 H48 N24 Ru1, 2(B1 F4)'
_chemical_formula_sum            'C24 H48 B2 F8 N24 Ru'
_chemical_formula_weight         947.55
_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_date             2020-06-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-03-18 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.77425(13)
_cell_length_b                   10.77425(13)
_cell_length_c                   31.8415(5)
_cell_measurement_reflns_used    10564
_cell_measurement_temperature    81(2)
_cell_measurement_theta_max      74.0700
_cell_measurement_theta_min      4.1530
_cell_volume                     3201.09(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      81(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-Arc
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00 -18.00   0.50    0.13    --  -52.43 125.00-180.00   52
  2  ω     37.00  93.00   0.50    0.13    --   68.73-125.00 120.00  112
  3  ω     37.00  67.00   0.50    0.13    --   68.73-125.00-180.00   60
  4  ω     37.00  99.00   0.50    0.13    --   69.88   0.00   0.00  124
  5  ω     49.00  77.00   0.50    0.13    --   75.25-121.00 119.37   56
  6  ω     89.00 114.00   0.50    0.13    --   75.25  53.00  63.52   50
  7  ω     56.00 101.00   0.50    0.13    --   75.25   1.00 -76.41   90
  8  ω     63.00  89.00   0.50    0.13    --   75.25  21.00 108.03   52
  9  ω     45.00  74.00   0.50    0.13    --   75.25-107.00-178.71   58
 10  ω     81.00 118.00   0.50    0.13    --   75.25  19.00 -92.53   74
 11  ω     49.00  76.00   0.50    0.13    --   75.25   6.00 157.58   54
 12  ω     46.00  81.00   0.50    0.13    --   75.25  12.00 104.34   70
 13  ω     67.00  93.00   0.50    0.13    --   75.25 172.00-101.20   52
 14  ω     43.00  87.00   0.50    0.13    --   75.25-111.00-104.07   88
 15  ω     56.00  81.00   0.50    0.13    --   75.25   8.00  -4.75   50
 16  ω     63.00  88.00   0.50    0.13    --   75.25-107.00 -15.59   50
 17  ω     66.00  96.00   0.50    0.13    --   75.25  21.00  54.03   60
 18  ω     89.00 114.00   0.50    0.13    --   75.25  11.00-165.37   50
 19  ω     63.00  98.00   0.50    0.13    --   75.25  21.00 155.88   70
 20  ω     47.00  72.00   0.50    0.13    --   75.25 -89.00  35.65   50
 21  ω     52.00 111.00   0.50    0.13    --   75.25  13.00  14.48  118
 22  ω     48.00  73.00   0.50    0.13    --   75.25  12.00 141.20   50
 23  ω     72.00 100.00   0.50    0.13    --   75.25-143.00 -89.43   56
 24  ω     86.00 112.00   0.50    0.13    --   75.25   6.00 157.58   52
 25  ω     52.00 105.00   0.50    0.13    --   75.25-153.00 130.77  106
 26  ω     32.00  57.00   0.50    0.13    --   24.00  74.00 173.51   50
 27  ω    -41.00 -13.00   0.50    0.13    --  -52.43 125.00  60.00   56
 28  ω    -66.00 -23.00   0.50    0.13    --  -52.43   0.00  90.00   86
 29  ω    -77.00 -41.00   0.50    0.13    --  -52.43 125.00 -30.00   72
 30  ω    -49.00 -24.00   0.50    0.13    --  -52.43 -15.00-120.00   50
 31  ω    -85.00 -54.00   0.50    0.13    --  -52.43 -15.00-120.00   62
 32  ω     40.00  66.00   0.50    0.13    --   68.73-125.00 -90.00   52
 33  ω     36.00  62.00   0.50    0.13    --   69.88-125.00-150.00   52
 34  ω     63.00  95.00   0.50    0.13    --   69.88-125.00-150.00   64
 35  ω     39.00  68.00   0.50    0.13    --   69.88   0.00-120.00   58
 36  ω     62.00  95.00   0.50    0.13    --   69.88-125.00 -90.00   66
 37  ω     34.00  65.00   0.50    0.13    --   69.88-125.00-120.00   62
 38  ω     45.00  95.00   0.50    0.13    --   69.88-125.00   0.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0417837000
_diffrn_orient_matrix_UB_12      0.0471348000
_diffrn_orient_matrix_UB_13      0.0407492000
_diffrn_orient_matrix_UB_21      0.0652001000
_diffrn_orient_matrix_UB_22      0.1535220000
_diffrn_orient_matrix_UB_23      -0.0173657000
_diffrn_orient_matrix_UB_31      -0.1457994000
_diffrn_orient_matrix_UB_32      -0.0382999000
_diffrn_orient_matrix_UB_33      -0.0194487000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            12059
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.166
_diffrn_reflns_theta_min         4.165
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.740
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.53a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0244
_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)+(0.0190P)²+10.1000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1459
_reflns_number_total             1460
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cp04321h25.cif
_cod_data_source_block           RuFe_batch1_80K_quenched
_cod_depositor_comments
'Adding full bibliography for 7244027--7244031.cif.'
_cod_original_cell_volume        3201.09(9)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7244030
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru1 N24 F8 B2 C24 H48'
_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.
;
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1)
2.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 1.919
_oxdiff_exptl_absorpt_empirical_full_min 0.595
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
Ru1 Ru 0.666667 0.333333 0.333333 0.01342(10) Uani 1 6 d S T P A 3
F2 F 0.90506(13) 0.86296(12) 0.33253(4) 0.0333(3) Uani 1 1 d . . . . .
F1 F 1.000000 1.000000 0.27464(6) 0.0360(5) Uani 1 3 d S T P . .
N1 N 0.71456(15) 0.50934(15) 0.37043(4) 0.0159(3) Uani 1 1 d . . . . .
N4 N 0.71991(15) 0.69029(15) 0.40045(5) 0.0170(3) Uani 1 1 d . . . . .
N2 N 0.83140(16) 0.57445(16) 0.39620(5) 0.0207(3) Uani 1 1 d . . . . .
N3 N 0.83480(16) 0.68393(16) 0.41430(5) 0.0209(3) Uani 1 1 d . . . . .
C1 C 0.64774(18) 0.58388(18) 0.37388(5) 0.0166(3) Uani 1 1 d . . . . .
H1 H 0.562297 0.564134 0.359636 0.020 Uiso 1 1 calc R U . . .
C3 C 0.6775(2) 0.8148(2) 0.45936(6) 0.0238(4) Uani 1 1 d . . . . .
H3A H 0.660916 0.895257 0.465796 0.029 Uiso 1 1 calc R U . . .
H3B H 0.766980 0.833996 0.473654 0.029 Uiso 1 1 calc R U . . .
C2 C 0.6967(2) 0.80949(19) 0.41234(6) 0.0204(4) Uani 1 1 d . . . . .
H2A H 0.610377 0.798118 0.397788 0.024 Uiso 1 1 calc R U . . .
H2B H 0.779706 0.901175 0.403047 0.024 Uiso 1 1 calc R U . . .
B1 B 1.000000 1.000000 0.31890(12) 0.0176(7) Uani 1 3 d S T P . .
C4 C 0.5535(2) 0.6769(2) 0.47672(6) 0.0288(4) Uani 1 1 d . . . . .
H4A H 0.465216 0.654673 0.461766 0.043 Uiso 1 1 calc R U . . .
H4B H 0.541846 0.688835 0.506708 0.043 Uiso 1 1 calc R U . . .
H4C H 0.573431 0.598304 0.472856 0.043 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 '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
0 0 1 0.1021
0 0 -1 0.1322
-1 0 -1 0.1642
1 0 1 0.2093
0 -1 1 0.1035
0 1 -1 0.1360
1 -1 0 0.1579
-1 0 1 0.1291
1 0 -1 0.1801
0 -1 -1 0.1256
0 1 1 0.1256
-2 2 -1 0.1304
1 0 -2 0.1655
-1 0 2 0.1013
-1 1 1 0.1124
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 Ru1 N1 90.62(5) 16_655 17 ?
N1 Ru1 N1 89.38(5) 18_545 2_655 ?
N1 Ru1 N1 90.62(5) 3_665 . ?
N1 Ru1 N1 90.62(5) 16_655 18_545 ?
N1 Ru1 N1 180.0 16_655 . ?
N1 Ru1 N1 90.62(5) 17 18_545 ?
N1 Ru1 N1 180.0 17 2_655 ?
N1 Ru1 N1 89.38(5) 16_655 3_665 ?
N1 Ru1 N1 90.62(5) 3_665 2_655 ?
N1 Ru1 N1 89.38(5) 17 3_665 ?
N1 Ru1 N1 89.38(5) 17 . ?
N1 Ru1 N1 180.0 18_545 3_665 ?
N1 Ru1 N1 90.62(5) 2_655 . ?
N1 Ru1 N1 89.38(5) 16_655 2_655 ?
N1 Ru1 N1 89.38(5) 18_545 . ?
N2 N1 Ru1 123.85(11) . . ?
C1 N1 Ru1 129.89(12) . . ?
C1 N1 N2 106.24(14) . . ?
N3 N4 C2 121.35(14) . . ?
C1 N4 N3 108.83(14) . . ?
C1 N4 C2 129.61(15) . . ?
N3 N2 N1 109.49(14) . . ?
N2 N3 N4 106.97(14) . . ?
N1 C1 H1 125.8 . . ?
N4 C1 N1 108.48(15) . . ?
N4 C1 H1 125.8 . . ?
H3A C3 H3B 107.8 . . ?
C2 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C2 C3 C4 113.05(16) . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
N4 C2 C3 111.82(14) . . ?
N4 C2 H2A 109.3 . . ?
N4 C2 H2B 109.3 . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
F2 B1 F2 110.59(15) 2_765 3_675 ?
F2 B1 F2 110.59(15) 2_765 . ?
F2 B1 F2 110.59(15) 3_675 . ?
F2 B1 F1 108.32(16) 2_765 . ?
F2 B1 F1 108.32(16) 3_675 . ?
F2 B1 F1 108.33(16) . . ?
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 . . ?
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
Ru1 N1 2.0687(14) 16_655 ?
Ru1 N1 2.0686(14) . ?
Ru1 N1 2.0686(14) 3_665 ?
Ru1 N1 2.0687(14) 17 ?
Ru1 N1 2.0686(14) 18_545 ?
Ru1 N1 2.0686(14) 2_655 ?
F2 B1 1.3800(16) . ?
F1 B1 1.409(4) . ?
N1 N2 1.366(2) . ?
N1 C1 1.324(2) . ?
N4 N3 1.348(2) . ?
N4 C1 1.320(2) . ?
N4 C2 1.476(2) . ?
N2 N3 1.297(2) . ?
C1 H1 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.516(2) . ?
C3 C4 1.521(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
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
Ru1 N1 N2 N3 178.03(11) . . . . ?
Ru1 N1 C1 N4 -177.93(11) . . . . ?
N1 N2 N3 N4 0.14(19) . . . . ?
N2 N1 C1 N4 0.12(19) . . . . ?
N3 N4 C1 N1 -0.03(19) . . . . ?
N3 N4 C2 C3 -62.3(2) . . . . ?
C1 N1 N2 N3 -0.16(19) . . . . ?
C1 N4 N3 N2 -0.07(19) . . . . ?
C1 N4 C2 C3 123.65(19) . . . . ?
C2 N4 N3 N2 -175.24(15) . . . . ?
C2 N4 C1 N1 174.61(16) . . . . ?
C4 C3 C2 N4 -57.9(2) . . . . ?
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
0.0003 -0.0004 1.0002 0.0407 -0.0174 -0.0195
-0.0003 0.0004 -1.0002 -0.0407 0.0174 0.0195
-0.9993 0.0009 -1.0003 0.0010 -0.0476 0.1651
0.9993 -0.0009 1.0003 -0.0010 0.0476 -0.1651
0.0004 -0.9987 0.9995 -0.0064 -0.1707 0.0188
-0.0004 0.9987 -0.9995 0.0064 0.1707 -0.0188
0.9990 -0.9988 -0.0006 -0.0888 -0.0882 -0.1074
-0.9987 0.0000 1.0000 0.0825 -0.0825 0.1262
0.9987 -0.0000 -1.0000 -0.0825 0.0825 -0.1262
-0.0003 -0.9979 -1.0009 -0.0878 -0.1358 0.0577
0.0003 0.9979 1.0009 0.0878 0.1358 -0.0577
-1.9984 1.9979 -0.9991 0.1370 0.1938 0.2343
0.9984 0.0004 -2.0002 -0.1232 0.0999 -0.1067
-0.9984 -0.0004 2.0002 0.1232 -0.0999 0.1067
-0.9987 0.9984 1.0007 0.1296 0.0708 0.0879
