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_7715355
_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             2023-12-02
_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                70.707(2)
_cell_angle_beta                 84.123(2)
_cell_angle_gamma                81.194(2)
_cell_formula_units_Z            1
_cell_length_a                   11.8086(2)
_cell_length_b                   14.1394(3)
_cell_length_c                   15.5340(4)
_cell_measurement_reflns_used    23949
_cell_measurement_temperature    100(18)
_cell_measurement_theta_max      31.6660
_cell_measurement_theta_min      2.1500
_cell_volume                     2415.41(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.94a 64-bit (release 20-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_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      N~2~
_diffrn_ambient_temperature      100(18)
_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 0.937
_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    -90.00 -43.00   0.50    1.59    --  -13.05-178.00  60.00   94
  2  \w    -87.00   9.00   0.50    1.59    --  -13.05 -57.00 -60.00  192
  3  \w    -66.00 -41.00   0.50    1.59    --  -13.05 129.00 -26.00   50
  4  \w    -74.00 -48.00   0.50    1.59    --  -13.05 142.00 145.00   52
  5  \w    -40.00  61.00   0.50    1.59    --  -13.05  77.00  60.00  202
  6  \w    -15.00  38.00   0.50    1.59    --   13.68  77.00 -90.00  106
  7  \w     62.00  87.00   0.50    1.59    --   13.68  77.00 -90.00   50
  8  \w     -8.00  51.00   0.50    1.59    --   13.68 -99.00-150.00  118
  9  \w     28.00  53.00   0.50    1.59    --   13.68-129.00 -99.00   50
 10  \w     30.00  65.00   0.50    1.59    --   13.68-142.00  88.00   70
 11  \w    -56.00 -30.00   0.50    1.59    --   13.68 -57.00 120.00   52
 12  \w     -1.00  36.00   0.50    1.59    --   13.68 -57.00 120.00   74
 13  \w     52.00  79.00   0.50    1.59    --   13.68 178.00   0.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0116617000
_diffrn_orient_matrix_UB_12      0.0528525000
_diffrn_orient_matrix_UB_13      -0.0218548000
_diffrn_orient_matrix_UB_21      -0.0127040000
_diffrn_orient_matrix_UB_22      0.0072404000
_diffrn_orient_matrix_UB_23      0.0431865000
_diffrn_orient_matrix_UB_31      0.0583831000
_diffrn_orient_matrix_UB_32      0.0050358000
_diffrn_orient_matrix_UB_33      0.0022248000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41959
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.503
_diffrn_reflns_theta_min         2.173
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       Block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.213
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         13808
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+1.1851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10676
_reflns_number_total             13808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04226j2.cif
_cod_data_source_block           Cp5Fe-100K
_cod_database_code               7715355
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Fe P S F O'
_chemical_oxdiff_usercomment     'C H N Fe P S F O'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 C51-F5 = C51-F6 = C51-F4
 1.33 with sigma of 0.02
 C51-S2
 1.82 with sigma of 0.02
 S2-O5 = S2-O4 = S2-O6
 1.44 with sigma of 0.02
 H6A-H5
 1.92 with sigma of 0.001
 C51-O6
 2.57 with sigma of 0.04
 C51-O5
 2.58 with sigma of 0.04
 C51-O4
 2.56 with sigma of 0.04
 C51-O5 \\sim C51-O4 \\sim C51-O6
 with sigma of 0.04
 C51-F5 \\sim C51-F6 \\sim C51-F4
 with sigma of 0.02
 F5-F6 \\sim F6-F4 \\sim F4-F5
 with sigma of 0.04
 S2-F5 \\sim S2-F6 \\sim S2-F4
 with sigma of 0.04
 S2-O5 \\sim S2-O4 \\sim S2-O6
 with sigma of 0.02
 O5-O4 \\sim O4-O6 \\sim O5-O6
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C51 \\sim F5 \\sim F6 \\sim F4 \\sim S2 \\sim O5 \\sim O4 \\sim O6: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C51, F5, F6, F4, S2, O5, O4, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: S1(0.92) F3(0.92) O3(0.92) F1(0.92) O2(0.92) O1(0.92) F2(0.92)
 C50(0.92) C51(0.08) F5(0.08) F6(0.08) F4(0.08) S2(0.08) O5(0.08) O4(0.08)
 O6(0.08)
6.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C26(H26A,H26B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C19(H19), C39(H39), C5(H5), C4(H4), C29(H29), C15(H15), C33(H33),
 C3(H3), C25(H25), C18(H18), C30(H30), C35(H35), C24(H24), C38(H38), C23(H23),
 C37(H37), C36(H36), C16(H16), C17(H17), C31(H31), C22(H22), C21(H21), C32(H32),
  C11(H11), C13(H13), C10(H10), C12(H12)
6.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B)
6.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C49(H49A,H49B,
 H49C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              4208
_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 1.365
_oxdiff_exptl_absorpt_empirical_full_min 0.759