MMCT energy change in cyanidometal-bridged trinuclear complexes by changing the ligand electron donating ability
Qian, Wang; Liu, Xiao-Lin; Tan, Bing-Chang; Song, Ying; Jiang, Long-Long; Wu, Xin-Tao; Sheng, Tian-Lu; New Journal of Chemistry 47 (2023) 7134–7142; doi:10.1039/D2NJ06104J

data_7062366
_publ_section_title
;
 MMCT energy change in cyanidometal-bridged trinuclear complexes by
 changing the ligand electron donating ability
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7134
_journal_page_last               7142
_journal_paper_doi               10.1039/D2NJ06104J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C98 H105 Fe2 N6 P4 Ru, 2(F6 P), C H2 Cl2'
_chemical_formula_sum            'C99 H107 Cl2 F12 Fe2 N6 P6 Ru'
_chemical_formula_weight         2078.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.015(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2693(2)
_cell_length_b                   16.9532(2)
_cell_length_c                   19.1955(3)
_cell_measurement_reflns_used    19186
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      59.9720
_cell_measurement_theta_min      2.6150
_cell_volume                     4776.16(12)
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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      0.00  70.00   0.50    0.05    --   76.11 -37.00 167.00  140
  2  \w     61.00 105.00   0.50    0.05    --   76.11-125.00  60.00   88
  3  \w     22.00  50.00   0.50    0.05    --   76.11-125.00  60.00   56
  4  \w      1.00  62.00   0.50    0.05    --   76.11 -38.00-120.00  122
  5  \w     79.00 104.00   0.50    0.05    --   76.11  37.00 -36.00   50
  6  \w    -15.00  77.00   0.50    0.05    --   -0.94  37.00 -36.00  184
  7  \w    -57.00  -5.00   0.50    0.05    --  -77.99  38.00  60.00  104
  8  \w    -69.00  -1.00   0.50    0.05    --  -77.99  38.00 120.00  136
  9  \w    -65.00   0.00   0.50    0.05    --  -77.99  37.00 -36.00  130
 10  \w    -78.00 -52.00   0.50    0.05    --  -77.99  57.00 150.00   52
 11  \w    -37.00  -9.00   0.50    0.05    --  -77.99  57.00 150.00   56
 12  \w    -71.00  -4.00   0.50    0.05    --  -77.99  38.00 150.00  134
 13  \w   -155.00 -56.00   0.50    0.05    --  -77.99 -37.00 167.00  198
 14  \w   -113.00 -87.00   0.50    0.05    --  -77.99-125.00 -60.00   52
 15  \w   -142.00 -89.00   0.50    0.05    --  -77.99 -99.00 -90.00  106
 16  \w   -152.00-127.00   0.50    0.05    --  -77.99-125.00 -60.00   50
 17  \w    -62.00 -21.00   0.50    0.05    --   -0.94 -37.00 167.00   82
 18  \w     -7.00  38.00   0.50    0.05    --   -0.94 -99.00-180.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Synergy Custom(Liquid MetalJet D2+)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0359251000
_diffrn_orient_matrix_UB_12      0.0153796000
_diffrn_orient_matrix_UB_13      -0.0705507000
_diffrn_orient_matrix_UB_21      -0.0721460000
_diffrn_orient_matrix_UB_22      0.0337667000
_diffrn_orient_matrix_UB_23      0.0148490000
_diffrn_orient_matrix_UB_31      0.0427955000
_diffrn_orient_matrix_UB_32      0.0697125000
_diffrn_orient_matrix_UB_33      0.0084258000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39077
_diffrn_reflns_point_group_measured_fraction_full 0.766
_diffrn_reflns_point_group_measured_fraction_max 0.728
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.174
_diffrn_reflns_theta_min         2.082
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29338
_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            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             2142
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.482
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 3780 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         15784
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1011P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.441
_reflns_Friedel_fraction_full    0.515
_reflns_Friedel_fraction_max     0.461
_reflns_number_gt                14015
_reflns_number_total             15784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj06104j2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7062365--7062373.cif.'
_cod_database_code               7062366
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P F Cl Ru Fe '
_chemical_oxdiff_usercomment     'C H N P F Cl Ru Fe '
_shelx_estimated_absorpt_t_max   0.697
_shelx_estimated_absorpt_t_min   0.443
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C01S(H01S), C02F(H02J), C037(H037)
2.b Secondary CH2 refined with riding coordinates:
 C016(H01A,H01B), C028(H02A,H02B), C02Z(H2,HB), C03A(H03D,H03E), C03C(H03V,H03W)
2.c Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00S(H00S), C00T(H00T), C00W(H00W), C00Y(H00Y), C010(H010),
 C011(H011), C013(H013), C014(H014), C019(H019), C01A(H01C), C01B(H01D),
 C01C(H01E), C01D(H01F), C01E(H01G), C01G(H01K), C01J(H01L), C01L(H01M),
 C01M(H01N), C01N(H01O), C01O(H01P), C01R(H01R), C01T(H01T), C01V(H01V),
 C01W(H01W), C01X(H01X), C01Y(H01Y), C020(H020), C021(H021), C023(H023),
 C024(H024), C025(H025), C026(H026), C027(H027), C029(H029), C02A(H02C),
 C02B(H02D), C02C(H02E), C02E(H02I), C02G(H02K), C02H(H02L), C02I(H02M),
 C02J(H02N), C02K(H02O), C02L(H02P), C02M(H02Q), C02N(H02R), C02P(H02S),
 C02Q(H02T), C02R(H02U), C02S(H02V), C02T(H02W), C02U(H02X), C02V(H02Y),
 C02W(H02Z), C02Y(H1), C030(H030), C031(H031), C032(H032), C033(H033),
 C036(H036), C038(H038), C039(H039), C03E(H03L)
2.d Idealised Me refined as rotating group:
 C01F(H01H,H01I,H01J), C02D(H02F,H02G,H02H), C02X(H02,H,HA), C035(H03A,H03B,
 H03C), C03B(H03F,H03G,H03H), C03D(H03I,H03J,H03K), C03F(H03M,H03N,H03O),
 C03H(H03P,H03Q,H03R), C03I(H03S,H03T,H03U), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              94375
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.599
_oxdiff_exptl_absorpt_empirical_full_min 0.550