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_7711784
_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         'C46 H54 Fe N7 P2 Ru S2, F6 P'
_chemical_formula_sum            'C46 H55 F6 Fe N7 O0.5 P3 Ru S2'
_chemical_formula_weight         1141.92
_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             2022-07-19
_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                 102.958(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8198(3)
_cell_length_b                   17.0381(3)
_cell_length_c                   19.8147(3)
_cell_measurement_reflns_used    44599
_cell_measurement_temperature    293
_cell_measurement_theta_max      34.2660
_cell_measurement_theta_min      1.9060
_cell_volume                     5204.83(16)
_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 0.976
_diffrn_measured_fraction_theta_max 0.977
_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    2.50    --  -28.00  45.00   0.00  360
  2  \w   -118.00  62.00   0.50    2.50    --  -28.00  45.00  90.00  360
  3  \w   -118.00  62.00   0.50    2.50    --  -28.00  45.00 180.00  360
  4  \w   -118.00  62.00   0.50    2.50    --  -28.00  45.00 270.00  360
;
_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      -0.0234411000
_diffrn_orient_matrix_UB_12      -0.0021629000
_diffrn_orient_matrix_UB_13      -0.0349664000
_diffrn_orient_matrix_UB_21      -0.0392430000
_diffrn_orient_matrix_UB_22      0.0067687000
_diffrn_orient_matrix_UB_23      0.0107604000
_diffrn_orient_matrix_UB_31      0.0051856000
_diffrn_orient_matrix_UB_32      0.0410079000
_diffrn_orient_matrix_UB_33      -0.0036092000
_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  0.0237
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.977
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63025
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.216
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52616
_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    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.712
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         9659
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0909P)^2^+4.4526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8583
_reflns_number_total             9659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03048a2.cif
_cod_data_source_block           cp1ru-feprln4-pf6
_cod_original_formula_sum        'C46 H55 F6 Fe N7 O0.50 P3 Ru S2'
_cod_database_code               7711784
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHSPNFFeRu
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.824
_reflns_odcompleteness_completeness 95.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.29
_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. Uiso/Uaniso restraints and constraints
C9 \\sim C4 \\sim C12 \\sim C13: within 2A with sigma of 0.05 and sigma for
terminal atoms of 0.1 within 2A
C5 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C12 \\sim C13: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C44(H44A,H44B), C36(H36A,H36B), C35(H35A,H35B),
 C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 N7(H7), N2(H2), C29(H29), C27(H27), C33(H33), C30(H30), C40(H40), C32(H32),
 C25(H25), C26(H26), C23(H23), C31(H31), C15(H15), C24(H24), C17(H17), C18(H18),
  C7(H7A), C21(H21), C20(H20), C6(H6), C19(H19), C11(H11), C8(H8), C13(H13),
 C12(H12), C14(H14), C5(H5)
3.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C34(H34A,H34B,H34C), C9(H9A,H9B,
 H9C), C46(H46A,H46B,H46C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17300
_shelx_fab_checksum              96106
_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 1.652
_oxdiff_exptl_absorpt_empirical_full_min 0.669