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_7711787
_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         'C45 H52 Fe N7 P2 Ru S2, F6 P'
_chemical_formula_sum            'C45 H52 F6 Fe N7 P3 Ru S2'
_chemical_formula_weight         1118.88
_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             2022-06-15
_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                 101.990(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7191(3)
_cell_length_b                   17.2564(4)
_cell_length_c                   19.6213(4)
_cell_measurement_reflns_used    36298
_cell_measurement_temperature    293
_cell_measurement_theta_max      34.0600
_cell_measurement_theta_min      1.9640
_cell_volume                     5206.26(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
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    3.00    --  -28.00  45.00   0.00  360
  2  \w   -118.00  22.00   0.50    3.00    --  -28.00  45.00  90.00  280
  3  \w   -118.00  22.00   0.50    3.00    --  -28.00  45.00 180.00  280
  4  \w   -118.00 -38.00   0.50    3.00    --  -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      -0.0188313000
_diffrn_orient_matrix_UB_12      -0.0038681000
_diffrn_orient_matrix_UB_13      -0.0359328000
_diffrn_orient_matrix_UB_21      -0.0358596000
_diffrn_orient_matrix_UB_22      0.0228977000
_diffrn_orient_matrix_UB_23      0.0045880000
_diffrn_orient_matrix_UB_31      0.0221214000
_diffrn_orient_matrix_UB_32      0.0339216000
_diffrn_orient_matrix_UB_33      -0.0071842000
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45953
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.122
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57285
_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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.292
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9819
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+5.4171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8652
_reflns_number_total             9819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03048a2.cif
_cod_data_source_block           cpru-feprln4-pf6
_cod_database_code               7711787
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SHCNPFFeRu
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.844
_reflns_odcompleteness_completeness 95.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.24
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C35-C34
 1.45 with sigma of 0.02
 C34-C33
 1.45 with sigma of 0.02
 C33-C34
 1.4 with sigma of 0.02
3. Rigid bond restraints
 C35, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C33, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C33, C34, C35
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C15 \\sim C9 \\sim C20 \\sim C40 \\sim C16 \\sim C27 \\sim C10 \\sim
C2 \\sim C42 \\sim C11 \\sim C21 \\sim C12 \\sim C38 \\sim C17 \\sim C19 \\sim
C36 \\sim C39 \\sim C3 \\sim C28 \\sim C13 \\sim C14 \\sim C18 \\sim C26 \\sim
C31 \\sim C30 \\sim C22 \\sim C32 \\sim C29 \\sim C41 \\sim C37 \\sim C43 \\sim
C24 \\sim C5 \\sim C25 \\sim C23 \\sim C8 \\sim C4 \\sim C6 \\sim C7 \\sim C44
\\sim C45: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C34 \\sim C35: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C43(H43A,H43B), C44(H44A,H44B), C33(H33A,H33B),
 C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N7(H7), C20(H20), C16(H16), C10(H10), C11(H11), C12(H12), C17(H17),
 C19(H19), C39(H39), C28(H28), C13(H13), C14(H14), C18(H18), C26(H26), C31(H31),
  C30(H30), C22(H22), C32(H32), C29(H29), C24(H24), C5(H5), C25(H25), C23(H23),
 C8(H8), C4(H4), C6(H6), C7(H7A)
5.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C35(H35A,H35B,
 H35C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31338
_shelx_fab_checksum              35469
_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 1.482
_oxdiff_exptl_absorpt_empirical_full_min 0.475