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_7711783
_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         '2(C44 H50 Fe N7 P2 Ru S2), 2(F6 P), C H2 Cl2'
_chemical_formula_sum            'C89 H102 Cl2 F12 Fe2 N14 P6 Ru2 S4'
_chemical_formula_weight         2294.64
_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
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3525(5)
_cell_length_b                   15.8856(7)
_cell_length_c                   21.9881(7)
_cell_measurement_reflns_used    14079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.8330
_cell_measurement_theta_min      1.8840
_cell_volume                     5362.5(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
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  42.00   0.50    3.00    --  -28.00  45.00   0.00  320
  2  \w   -118.00  22.00   0.50    3.00    --  -28.00  45.00  90.00  280
;
_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      0.0139911000
_diffrn_orient_matrix_UB_12      0.0080095000
_diffrn_orient_matrix_UB_13      -0.0302078000
_diffrn_orient_matrix_UB_21      0.0430676000
_diffrn_orient_matrix_UB_22      -0.0114799000
_diffrn_orient_matrix_UB_23      0.0081712000
_diffrn_orient_matrix_UB_31      -0.0090340000
_diffrn_orient_matrix_UB_32      -0.0423671000
_diffrn_orient_matrix_UB_33      -0.0080003000
_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  0.0530
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27482
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.845
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43870
_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    1.421
_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          0.05
_refine_diff_density_max         0.989
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10065
_refine_ls_number_restraints     316
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1261P)^2^+0.3505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1922
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                8119
_reflns_number_total             10065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03048a2.cif
_cod_data_source_block           cp1ru-feetln4-pf6-1
_cod_database_code               7711783
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         FeRuCHSNPF
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.820
_reflns_odcompleteness_completeness 91.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.30
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(5)
 0.03(5)
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
 C44-C43
 1.55 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C12 \\sim C22 \\sim C16 \\sim C39 \\sim C11 \\sim C5 \\sim C27 \\sim
C21 \\sim N6 \\sim C14 \\sim C8 \\sim C7 \\sim C4 \\sim C42 \\sim C15 \\sim C36
\\sim C23 \\sim C28 \\sim C26 \\sim C24 \\sim C38 \\sim C13 \\sim C25 \\sim C20
\\sim C2 \\sim C10 \\sim C3 \\sim C6 \\sim C31 \\sim C17 \\sim C18 \\sim C41
\\sim C32 \\sim C29 \\sim C37 \\sim C40 \\sim C19 \\sim C43 \\sim C30 \\sim C33
\\sim C35 \\sim C44 \\sim C34 \\sim C9 \\sim C45: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C1 \\sim C12 \\sim C22 \\sim C16 \\sim C39 \\sim C11 \\sim C5 \\sim C27 \\sim
C21 \\sim C14 \\sim C8 \\sim C7 \\sim C4 \\sim C42 \\sim C15 \\sim C36 \\sim
C23 \\sim C28 \\sim C26 \\sim C24 \\sim C38 \\sim C13 \\sim C25 \\sim C20 \\sim
C2 \\sim C10 \\sim C3 \\sim C6 \\sim C31 \\sim C17 \\sim C18 \\sim C41 \\sim
C32 \\sim C29 \\sim C37 \\sim C40 \\sim C19 \\sim C43 \\sim C30 \\sim C33 \\sim
C35 \\sim C44 \\sim C34 \\sim C9 \\sim C45: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
S1 \\sim C35: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
S2 \\sim C43: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C43 \\sim C44: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.0005 and sigma for
terminal atoms of 0.001
5. Rigid body (RIGU) restrains
 P3, F2, F4, F5, F3, F1, F6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: Cl2(0.5) Cl1(0.5) C45(0.5) H45A(0.5) H45B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C43(H43A,H43B), C35(H35A,H35B), C45(H45A,H45B)
7.b Aromatic/amide H refined with riding coordinates:
 N7(H7), N2(H2), C12(H12), C39(H39), C11(H11), C5(H5), C27(H27), C21(H21),
 C14(H14), C7(H7A), C4(H4), C15(H15), C23(H23), C26(H26), C24(H24), C13(H13),
 C25(H25), C20(H20), C6(H6), C17(H17), C18(H18), C32(H32), C31(H31), C30(H30),
 C29(H29), C33(H33), C19(H19)
7.c Fitted hexagon refined as free rotating group:
 C32(C31,C30,C29,C28,C33)
7.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C34(H34A,H34B,
 H34C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              2424
_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 2.587
_oxdiff_exptl_absorpt_empirical_full_min 0.628