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_7715354
_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         'C90 H82 Fe3 N14 P4, 2(C F3 O3 S)'
_chemical_formula_sum            'C92 H82 F6 Fe3 N14 O6 P4 S2'
_chemical_formula_weight         1949.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-01
_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                90
_cell_angle_beta                 97.894(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8808(3)
_cell_length_b                   20.5335(5)
_cell_length_c                   17.2688(4)
_cell_measurement_reflns_used    12570
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.0840
_cell_measurement_theta_min      2.9060
_cell_volume                     4524.11(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_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_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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     21.00  48.00   0.50    0.24    --   73.33-125.00 -60.00   54
  2  \w     85.00 110.00   0.50    0.24    --   73.33-125.00 -60.00   50
  3  \w     32.00  78.00   0.50    0.24    --   73.33 -66.00 -38.00   92
  4  \w     78.00 126.00   0.50    0.24    --   73.33  66.00  96.00   96
  5  \w     79.00 146.00   0.50    0.24    --   73.33 125.00 -60.00  134
  6  \w    -24.00  71.00   0.50    0.06    --   -0.78  77.00 -90.00  190
  7  \w     35.00  61.00   0.50    0.06    --   -0.78  38.00-150.00   52
  8  \w    -71.00  -2.00   0.50    0.24    --  -74.89  38.00  90.00  138
  9  \w    -71.00 -18.00   0.50    0.24    --  -74.89  38.00  60.00  106
 10  \w    -28.00  -3.00   0.50    0.24    --  -74.89  66.00  96.00   50
 11  \w    -72.00 -35.00   0.50    0.24    --  -74.89  66.00  96.00   74
 12  \w      1.00  27.00   0.50    0.06    --   -0.78  66.00  96.00   52
 13  \w    -70.00 -20.00   0.50    0.24    --  -74.89  38.00-180.00  100
 14  \w    -68.00 -43.00   0.50    0.06    --   -0.78 -66.00 -38.00   50
 15  \w    -28.00   7.00   0.50    0.06    --   -0.78 -66.00 -38.00   70
 16  \w   -102.00 -75.00   0.50    0.24    --  -74.89 -66.00 -38.00   54
 17  \w   -129.00 -95.00   0.50    0.24    --  -74.89-125.00  90.00   68
 18  \w   -148.00 -89.00   0.50    0.24    --  -74.89 -99.00  90.00  118
 19  \w   -144.00 -87.00   0.50    0.24    --  -74.89-125.00  60.00  114
 20  \w   -148.00-103.00   0.50    0.24    --  -74.89 -99.00-180.00   90
;
_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      0.0378583000
_diffrn_orient_matrix_UB_12      -0.0439816000
_diffrn_orient_matrix_UB_13      0.0537634000
_diffrn_orient_matrix_UB_21      0.0631777000
_diffrn_orient_matrix_UB_22      -0.0233898000
_diffrn_orient_matrix_UB_23      -0.0488797000
_diffrn_orient_matrix_UB_31      0.0747902000
_diffrn_orient_matrix_UB_32      0.0420904000
_diffrn_orient_matrix_UB_33      0.0291585000
_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  0.0929
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33051
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         54.821
_diffrn_reflns_theta_min         2.923
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.98a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       Block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.335
_exptl_crystal_size_min          0.237
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         8573
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0869
_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^)+(0.1221P)^2^+3.4530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5773
_reflns_number_total             8573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04226j2.cif
_cod_data_source_block           Cp1Fe
_cod_database_code               7715354
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O P F Ru  Cl Fe'
_chemical_oxdiff_usercomment     'C H N O P F Ru  Cl Fe'
_reflns_odcompleteness_completeness 99.61
_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
 H6A-H5
 1.92 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C26(H26A,H26B)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C19(H19), C43(H43), C2(H2), C42(H42), C44(H44), C39(H39), C13(H13),
 C12(H12), C10(H10), C18(H18), C21(H21), C41(H41), C5(H5), C22(H22), C33(H33),
 C35(H35), C23(H23), C31(H31), C3(H3), C36(H36), C37(H37), C29(H29), C32(H32),
 C17(H17), C25(H25), C11(H11), C16(H16), C38(H38), C24(H24), C30(H30), C4(H4)
4.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B)
4.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
;
_shelx_res_checksum              46545
_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 3.273
_oxdiff_exptl_absorpt_empirical_full_min 0.329