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_7715356
_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         'C96 H94 Fe3 N14 P4, 2(C F3 O3 S)'
_chemical_formula_sum            'C98 H94 F6 Fe3 N14 O6 P4 S2'
_chemical_formula_weight         2033.42
_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                 101.0760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2516(2)
_cell_length_b                   20.5089(3)
_cell_length_c                   19.4786(3)
_cell_measurement_reflns_used    20962
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.2930
_cell_measurement_theta_min      3.4290
_cell_volume                     4803.16(13)
_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_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 0.999
_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     32.00 114.00   0.50    0.09    --   73.53-147.00 147.00  164
  2  \w     41.00  66.00   0.50    0.09    --   73.53-124.00 -46.00   50
  3  \w      3.00  70.00   0.50    0.09    --   73.53 -38.00 -30.00  134
  4  \w     83.00 114.00   0.50    0.09    --   73.53 124.00  31.00   62
  5  \w     81.00 106.00   0.50    0.09    --   73.53 147.00-162.00   50
  6  \w    -17.00  64.00   0.50    0.05    --   -0.62  57.00-180.00  162
  7  \w     41.00  69.00   0.50    0.05    --   -0.62  38.00 -90.00   56
  8  \w    -57.00 -31.00   0.50    0.09    --  -74.78  38.00  60.00   52
  9  \w    -29.00  -3.00   0.50    0.09    --  -74.78  38.00  60.00   52
 10  \w    -89.00  -5.00   0.50    0.09    --  -74.78  57.00  60.00  168
 11  \w    -90.00 -65.00   0.50    0.09    --  -74.78 124.00  31.00   50
 12  \w   -106.00 -38.00   0.50    0.09    --  -74.78 125.00 150.00  136
 13  \w   -127.00 -35.00   0.50    0.09    --  -74.78 147.00-162.00  184
 14  \w   -146.00 -81.00   0.50    0.09    --  -74.78-125.00-180.00  130
 15  \w   -138.00-113.00   0.50    0.09    --  -74.78-124.00 -46.00   50
 16  \w   -148.00 -88.00   0.50    0.09    --  -74.78 -99.00 -30.00  120
 17  \w   -130.00-105.00   0.50    0.09    --  -74.78-147.00 147.00   50
 18  \w   -133.00 -88.00   0.50    0.09    --  -74.78 -99.00  60.00   90
 19  \w    -19.00   7.00   0.50    0.05    --   -0.62 -38.00   0.00   52
;
_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      -0.0071991000
_diffrn_orient_matrix_UB_12      0.0643055000
_diffrn_orient_matrix_UB_13      -0.0120125000
_diffrn_orient_matrix_UB_21      0.0200228000
_diffrn_orient_matrix_UB_22      -0.0097788000
_diffrn_orient_matrix_UB_23      -0.0644386000
_diffrn_orient_matrix_UB_31      -0.1092926000
_diffrn_orient_matrix_UB_32      -0.0060143000
_diffrn_orient_matrix_UB_33      -0.0247219000
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41673
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         54.821
_diffrn_reflns_theta_min         2.747
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82800
_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    1.406
_exptl_crystal_description       Block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.327
_exptl_crystal_size_min          0.216
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9106
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0728P)^2^+3.7233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7781
_reflns_number_total             9106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04226j2.cif
_cod_data_source_block           Cp4Fe
_cod_database_code               7715356
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N P F Fe'
_chemical_oxdiff_usercomment     'C H O N P F  Fe'
_reflns_odcompleteness_completeness 99.81
_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
 H5-H6A
 1.92 with sigma of 0.001
3. Rigid bond restraints
 C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B)
4.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C33(H33), C39(H39), C25(H25), C15(H15), C2(H2), C21(H21), C35(H35),
 C29(H29), C10(H10), C12(H12), C38(H38), C16(H16), C22(H22), C36(H36), C19(H19),
  C11(H11), C30(H30), C17(H17), C32(H32), C24(H24), C5(H5), C13(H13), C37(H37),
 C23(H23), C31(H31), C3(H3), C18(H18), 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), C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C48(H48A,H48B,
 H48C)
;
_shelx_res_checksum              67634
_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 1.428
_oxdiff_exptl_absorpt_empirical_full_min 0.793