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_7711780
_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_absolute_configuration ad
_chemical_formula_moiety         'C42 H46 Fe N7 P2 Ru S2, F6 P'
_chemical_formula_sum            'C42 H46 F6 Fe N7 P3 Ru S2'
_chemical_formula_weight         1076.81
_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             2022-08-16
_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                   15.1069(4)
_cell_length_b                   15.3402(5)
_cell_length_c                   21.6504(6)
_cell_measurement_reflns_used    33664
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.1360
_cell_measurement_theta_min      2.0290
_cell_volume                     5017.3(3)
_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                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.972
_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    2.00    --  -28.00  45.00   0.00  360
  2  \w   -118.00  42.00   0.50    2.00    --  -28.00  45.00  90.00  320
  3  \w   -118.00  22.00   0.50    2.00    --  -28.00  45.00 180.00  280
  4  \w   -118.00 -38.00   0.50    2.00    --  -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      0.0456213000
_diffrn_orient_matrix_UB_12      0.0108467000
_diffrn_orient_matrix_UB_13      0.0010227000
_diffrn_orient_matrix_UB_21      0.0006534000
_diffrn_orient_matrix_UB_22      0.0034679000
_diffrn_orient_matrix_UB_23      -0.0326641000
_diffrn_orient_matrix_UB_31      -0.0110339000
_diffrn_orient_matrix_UB_32      0.0448204000
_diffrn_orient_matrix_UB_33      0.0022656000
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49028
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.675
_diffrn_reflns_theta_min         2.315
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54661
_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    1.426
_exptl_crystal_description       needle
_exptl_crystal_F_000             2192
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.830
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         9279
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0638
_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^)+(0.1355P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1667
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                8645
_reflns_number_total             9279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03048a2.cif
_cod_data_source_block           cp1ru-me
_cod_database_code               7711780
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNSPFRuFe
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.865
_reflns_odcompleteness_completeness 96.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.91(4)
 0.09(4)
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
 P3-F3 = P3-F6 = P3-F4
 1.6 with sigma of 0.02
 P3-F3 = P3-F6 = P3-F4 = P3-F2 = P3-F1 = P3-F5
 1.65 with sigma of 0.02
 F3-F6 \\sim F6-F4
 with sigma of 0.04
 P3-F3 \\sim P3-F6 \\sim P3-F4
 with sigma of 0.02
 P3-F3 \\sim P3-F6 \\sim P3-F4 \\sim P3-F2 \\sim P3-F1 \\sim P3-F5
 with sigma of 0.02
 F3-F6 \\sim F3-F2 \\sim F3-F1 \\sim F3-F5 \\sim F6-F4 \\sim F6-F1 \\sim F6-F5
\\sim F4-F2 \\sim F4-F1 \\sim F4-F5
 \\sim F2-F1 \\sim F2-F5
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
F3 \\sim F6 \\sim F4: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
Uanis(F3) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of
0.0001 and sigma for terminal atoms of 0.0002
Uanis(F6) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of 0.0002
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of
0.0001 and sigma for terminal atoms of 0.0002
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 N7(H7), C23(H23), C24(H24), C33(H33), C4(H4), C38(H38), C20(H20), C19(H19),
 N2(H2), C32(H32), C21(H21), C12(H12), C18(H18), C25(H25), C27(H27), C17(H17),
 C7(H7A), C13(H13), C5(H5), C31(H31), C11(H11), C29(H29), C26(H26), C6(H6),
 C30(H30), C15(H15), C14(H14)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C34(H34A,H34B,
 H34C), C9(H9A,H9B,H9C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24029
_shelx_fab_checksum              25160
_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 1.529
_oxdiff_exptl_absorpt_empirical_full_min 0.759