Influence of the electronic effect of an ancillary ligand on MMCT and LMCT in localized cyanide-bridged complexes containing non-innocent ligands.
He, Yong; Huang, Ying-Ying; Fu, Jin-Hui; Liu, Yang; Wu, Xin-Tao; Sheng, Tian-Lu; Dalton transactions (Cambridge, England : 2003)  (2022) –; doi:10.1039/d2dt03048a

data_7711788
_publ_section_title
;
 Influence of the electronic effect of an ancillary ligand on MMCT and
 LMCT in localized cyanide-bridged complexes containing non-innocent
 ligands.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt03048a
_journal_year                    2022
_chemical_formula_moiety         'C52 H66 Fe N7 P2 Ru S2, I'
_chemical_formula_sum            'C52 H66 Fe I N7 P2 Ru S2'
_chemical_formula_weight         1198.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-20 deposited with the CCDC.	2022-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1864(3)
_cell_length_b                   15.4588(3)
_cell_length_c                   23.6654(6)
_cell_measurement_reflns_used    26978
_cell_measurement_temperature    293
_cell_measurement_theta_max      34.3630
_cell_measurement_theta_min      2.0060
_cell_volume                     5555.8(2)
_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
_diffrn_detector                 'CCD plate'
_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   -118.00  62.00   0.50    6.50    --  -28.00  45.00   0.00  360
  2  \w   -118.00  42.00   0.50    6.50    --  -28.00  45.00  90.00  320
  3  \w   -118.00  22.00   0.50    6.50    --  -28.00  45.00 180.00  280
  4  \w   -118.00 -38.00   0.50    6.50    --  -28.00  45.00 270.00  160
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0072818000
_diffrn_orient_matrix_UB_12      0.0026326000
_diffrn_orient_matrix_UB_13      -0.0295564000
_diffrn_orient_matrix_UB_21      -0.0090130000
_diffrn_orient_matrix_UB_22      -0.0448293000
_diffrn_orient_matrix_UB_23      -0.0026077000
_diffrn_orient_matrix_UB_31      -0.0452553000
_diffrn_orient_matrix_UB_32      0.0093496000
_diffrn_orient_matrix_UB_33      -0.0042558000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            65078
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         1.593
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59786
_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_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         12739
_refine_ls_number_restraints     302
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0435P)^2^+2.8673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10673
_reflns_number_total             12739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03048a2.cif
_cod_data_source_block           cp5ru-febuln4-i
_cod_database_code               7711788
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHSPFFeNRu
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.743
_reflns_odcompleteness_completeness 96.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.38
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(3)
 0.49(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C52-C51
 1.6 with sigma of 0.02
 C38-C39
 1.6 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C42 \\sim C20 \\sim C14 \\sim C32 \\sim C1 \\sim C33 \\sim C21 \\sim C8 \\sim
C27 \\sim C26 \\sim C29 \\sim C28 \\sim C34 \\sim C46 \\sim C18 \\sim C15 \\sim
C19 \\sim C6 \\sim C37 \\sim C7 \\sim C47 \\sim C22 \\sim C23 \\sim C5 \\sim
C17 \\sim C30 \\sim C4 \\sim C36 \\sim C25 \\sim C31 \\sim C35 \\sim C2 \\sim
C11 \\sim C3 \\sim C44 \\sim C45 \\sim C48 \\sim C10 \\sim C24 \\sim C9 \\sim
C49 \\sim C13 \\sim C16 \\sim C41 \\sim C40 \\sim C43 \\sim C39 \\sim C38 \\sim
C50 \\sim C12 \\sim C51 \\sim C52: within 2A with sigma of 0.1 and sigma for
terminal atoms of 0.2 within 2A
C51 \\sim C52 \\sim C40 \\sim C39: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C52) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C49(H49A,H49B), C41(H41A,H41B), C40(H40A,H40B),
 C39(H39A,H39B), C50(H50A,H50B), C51(H51A,H51B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N7(H7), C33(H33), C21(H21), C27(H27), C29(H29), C28(H28), C34(H34),
 C18(H18), C15(H15), C19(H19), C37(H37), C22(H22), C23(H23), C17(H17), C30(H30),
  C36(H36), C25(H25), C31(H31), C35(H35), C45(H45), C24(H24), C16(H16)
5.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C9(H9A,H9B,
 H9C), C13(H13A,H13B,H13C), C43(H43A,H43B,H43C), C38(H38A,H38B,H38C), C12(H12A,
 H12B,H12C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              50532
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.563
_oxdiff_exptl_absorpt_empirical_full_min 0.736