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_7715357
_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 Fe3 N14 P4, 2(C F3 O3 S)'
_chemical_formula_sum            'C100 H98 F6 Fe3 N14 O6 P4 S2'
_chemical_formula_weight         2061.47
_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             2023-12-01
_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                71.0090(10)
_cell_angle_beta                 84.4960(10)
_cell_angle_gamma                81.4470(10)
_cell_formula_units_Z            1
_cell_length_a                   12.00670(10)
_cell_length_b                   14.40640(10)
_cell_length_c                   15.52430(10)
_cell_measurement_reflns_used    17977
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.5350
_cell_measurement_theta_min      2.8400
_cell_volume                     2507.65(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     72.00  98.00   0.50    0.05    --   73.53  60.00-172.00   52
  2  \w    103.00 141.00   0.50    0.05    --   73.53  60.00-172.00   76
  3  \w     79.00 147.00   0.50    0.05    --   73.53 125.00 -60.00  136
  4  \w     79.00 127.00   0.50    0.05    --   73.53 125.00  60.00   96
  5  \w     99.00 125.00   0.50    0.05    --   73.53  38.00  90.00   52
  6  \w      1.00  65.00   0.50    0.05    --   73.53 -60.00  48.00  128
  7  \w     25.00  95.00   0.50    0.05    --   73.53-125.00 150.00  140
  8  \w     21.00 101.00   0.50    0.05    --   73.53-125.00  30.00  160
  9  \w      9.00 106.00   0.50    0.05    --   73.53 -99.00  30.00  194
 10  \w     42.00 103.00   0.50    0.05    --   73.53-125.00 -90.00  122
 11  \w   -148.00 -63.00   0.50    0.05    --  -74.78 -60.00  48.00  170
 12  \w   -148.00 -81.00   0.50    0.05    --  -74.78-125.00 120.00  134
 13  \w   -108.00 -83.00   0.50    0.05    --  -74.78-125.00-120.00   50
 14  \w   -142.00 -82.00   0.50    0.05    --  -74.78-125.00-180.00  120
 15  \w    -73.00   8.00   0.50    0.05    --   -0.62 -60.00  48.00  162
 16  \w    -14.00  65.00   0.50    0.05    --   -0.62  60.00-172.00  158
 17  \w     15.00  54.00   0.50    0.05    --   -0.62  38.00 -30.00   78
 18  \w    -33.00  -8.00   0.50    0.05    --  -74.78  60.00-172.00   50
 19  \w    -71.00  -6.00   0.50    0.05    --  -74.78  38.00-180.00  130
 20  \w    -67.00 -42.00   0.50    0.05    --  -74.78  60.00-172.00   50
 21  \w    -90.00 -43.00   0.50    0.05    --  -74.78 125.00 -90.00   94
 22  \w    -73.00 -22.00   0.50    0.05    --  -74.78 125.00-150.00  102
 23  \w   -109.00 -33.00   0.50    0.05    --  -74.78 125.00 150.00  152
;
_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      -0.1016092000
_diffrn_orient_matrix_UB_12      -0.0003550000
_diffrn_orient_matrix_UB_13      -0.0286384000
_diffrn_orient_matrix_UB_21      -0.0486261000
_diffrn_orient_matrix_UB_22      0.0442934000
_diffrn_orient_matrix_UB_23      0.0601808000
_diffrn_orient_matrix_UB_31      0.0081295000
_diffrn_orient_matrix_UB_32      0.0886335000
_diffrn_orient_matrix_UB_33      -0.0624714000
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31325
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         54.820
_diffrn_reflns_theta_min         2.842
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.412
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64433
_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    1.365
_exptl_crystal_description       Block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.202
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         9481
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0840P)^2^+2.3765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8307
_reflns_number_total             9481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04226j2.cif
_cod_data_source_block           Cp5Fe
_cod_database_code               7715357
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Fe P F S'
_chemical_oxdiff_usercomment     'C H O N Fe P F S'
_reflns_odcompleteness_completeness 99.45
_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
 2.35 with sigma of 0.01
 N7-H6B
 2.35 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C50) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B)
4.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C35(H35), C25(H25), C33(H33), C15(H15), C21(H21), C19(H19),
 C36(H36), C38(H38), C2(H2), C37(H37), C32(H32), C29(H29), C22(H22), C17(H17),
 C16(H16), C18(H18), C31(H31), C24(H24), C23(H23), C30(H30), C3(H3), C5(H5),
 C12(H12), C10(H10), C4(H4), C13(H13), C11(H11)
4.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B)
4.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              49939
_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 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.725