Fine-tuning of thermally induced SCO behaviors of trinuclear cyanido-bridged complexes by regulating the electron donating ability of C<sub>CN</sub>-terminal fragments.
Huang, Ying-Ying; He, Yong; Liu, Yang; Fu, Jin-Hui; Liu, Xiao-Lin; Wu, Xin-Tao; Sheng, Tian-Lu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3777–3784; doi:10.1039/d3dt04226j

data_7715358
_publ_section_title
;
 Fine-tuning of thermally induced SCO behaviors of trinuclear
 cyanido-bridged complexes by regulating the electron donating ability of
 C<sub>CN</sub>-terminal fragments.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3777
_journal_page_last               3784
_journal_paper_doi               10.1039/d3dt04226j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C98 H98 Fe N14 P4 Ru2, 2(C F3 O3 S)'
_chemical_formula_sum            'C100 H98 F6 Fe N14 O6 P4 Ru2 S2'
_chemical_formula_weight         2151.91
_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_date             2023-12-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-09 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                71.000(2)
_cell_angle_beta                 83.364(2)
_cell_angle_gamma                79.993(2)
_cell_formula_units_Z            1
_cell_length_a                   12.1314(2)
_cell_length_b                   14.6758(3)
_cell_length_c                   15.4174(3)
_cell_measurement_reflns_used    23307
_cell_measurement_temperature    293.00(12)
_cell_measurement_theta_max      60.0190
_cell_measurement_theta_min      2.7910
_cell_volume                     2550.72(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.00(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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     81.00 154.00   0.50    0.05    --   75.32  32.00 127.00  146
  2  \w     59.00 147.00   0.50    0.05    --   75.32  77.00   0.00  176
  3  \w     90.00 116.00   0.50    0.05    --   75.32  57.00-150.00   52
  4  \w    122.00 149.00   0.50    0.05    --   75.32  57.00-150.00   54
  5  \w     99.00 149.00   0.50    0.05    --   75.32 125.00-180.00  100
  6  \w     -2.00  24.00   0.50    0.05    --   75.32 -32.00 -30.00   52
  7  \w     41.00  92.00   0.50    0.05    --   75.32-125.00 -60.00  102
  8  \w     20.00 111.00   0.50    0.05    --   75.32-125.00 -30.00  182
  9  \w      8.00 106.00   0.50    0.05    --   75.32 -99.00 -30.00  196
 10  \w     20.00  98.00   0.50    0.05    --   75.32-125.00  60.00  156
 11  \w   -107.00 -10.00   0.50    0.05    --  -78.14  77.00-180.00  194
 12  \w    -88.00  -4.00   0.50    0.05    --  -78.14  57.00-180.00  168
 13  \w    -68.00  -9.00   0.50    0.05    --  -78.14  38.00 -60.00  118
 14  \w    -27.00  -1.00   0.50    0.05    --  -78.14  38.00   0.00   52
 15  \w    -71.00 -46.00   0.50    0.05    --  -78.14  38.00   0.00   50
 16  \w    -58.00 -33.00   0.50    0.05    --  -78.14  32.00 127.00   50
 17  \w    -35.00  -4.00   0.50    0.05    --  -78.14  57.00 120.00   62
 18  \w     27.00  78.00   0.50    0.05    --   -1.41  32.00 127.00  102
 19  \w    -11.00  23.00   0.50    0.05    --   -1.41  32.00 127.00   68
 20  \w    -79.00 -51.00   0.50    0.05    --   -1.41 -32.00 -30.00   56
 21  \w    -48.00  17.00   0.50    0.05    --   -1.41 -32.00 -30.00  130
 22  \w   -110.00 -21.00   0.50    0.05    --  -78.14 125.00-180.00  178
 23  \w   -156.00 -57.00   0.50    0.05    --  -78.14 -32.00 -30.00  198
 24  \w   -152.00 -84.00   0.50    0.05    --  -78.14-125.00 -60.00  136
 25  \w     -7.00  27.00   0.50    0.05    --   -1.41 -99.00   0.00   68
 26  \w      1.00  28.00   0.50    0.05    --   -1.41 -99.00 -90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0395371000
_diffrn_orient_matrix_UB_12      0.0671084000
_diffrn_orient_matrix_UB_13      0.0246071000
_diffrn_orient_matrix_UB_21      0.0916044000
_diffrn_orient_matrix_UB_22      -0.0636946000
_diffrn_orient_matrix_UB_23      0.0293690000
_diffrn_orient_matrix_UB_31      0.0515916000
_diffrn_orient_matrix_UB_32      0.0308813000
_diffrn_orient_matrix_UB_33      -0.0837001000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28796
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         54.822
_diffrn_reflns_theta_min         2.798
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       Block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.342
_exptl_crystal_size_min          0.304
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         9569
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+1.9259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8516
_reflns_number_total             9569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04226j2.cif
_cod_data_source_block           Cp5Ru
_cod_database_code               7715358
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONFRuFeS
_chemical_oxdiff_usercomment     CHONFRuFeS
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H6B-N7
 2.35 with sigma of 0.01
 H6A-H5
 2.35 with sigma of 0.01
3. Rigid bond restraints
 N1, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C50) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C26(H26A,H26B)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C2(H2), C19(H19), C30(H30), C17(H17), C29(H29), C21(H21), C35(H35),
 C16(H16), C31(H31), C5(H5), C38(H38), C39(H39), C18(H18), C25(H25), C3(H3),
 C23(H23), C36(H36), C33(H33), C22(H22), C37(H37), C10(H10), C24(H24), C32(H32),
  C13(H13), C4(H4), C11(H11), C12(H12)
5.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B)
5.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C49(H49A,H49B,
 H49C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              36029
_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 2.207
_oxdiff_exptl_absorpt_empirical_full_min 0.585