Tuning metal to metal charge transfer properties in cyanidometal-bridged complexes by changing the auxiliary ligand on the bridge.
Xu, Qing-Dou; Zeng, Chen; Su, Shao-Dong; Yang, Yu-Ying; Hu, Sheng-Min; Li, Ting-Ya; Wu, Xin-Tao; Sheng, Tian-Lu; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6161–6169; doi:10.1039/d1dt00157d

data_7707024
_publ_section_title
;
 Tuning metal to metal charge transfer properties in cyanidometal-bridged
 complexes by changing the auxiliary ligand on the bridge.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6161
_journal_page_last               6169
_journal_paper_doi               10.1039/d1dt00157d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'4(C98 H102 Fe2 N6 P4 Ru), 12(F6 P), 6(C H2 Cl2), 3(O)'
_chemical_formula_sum            'C398 H420 Cl12 F72 Fe8 N24 O3 P28 Ru4'
_chemical_formula_weight         9099.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-12-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-12 deposited with the CCDC.	2021-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                107.8851(4)
_cell_angle_beta                 95.1931(3)
_cell_angle_gamma                90.3443(3)
_cell_formula_units_Z            1
_cell_length_a                   15.54011(5)
_cell_length_b                   20.78264(9)
_cell_length_c                   33.67197(16)
_cell_measurement_reflns_used    167545
_cell_measurement_temperature    110.6(3)
_cell_measurement_theta_max      60.5020
_cell_measurement_theta_min      2.0090
_cell_volume                     10300.28(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.6(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_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     48.00  83.00   0.25    0.10    --   72.03  77.00   0.00  140
  2  \w     48.00  73.00   0.25    0.10    --   72.03  77.00 -60.00  100
  3  \w     48.00 136.00   0.25    0.10    --   72.03  77.00-120.00  352
  4  \w     48.00 143.00   0.25    0.10    --   72.03  77.00 -90.00  380
  5  \w     48.00  76.00   0.25    0.10    --   72.03  77.00-150.00  112
  6  \w     94.00 145.00   0.25    0.10    --   72.03  77.00 -60.00  204
  7  \w    107.00 144.00   0.25    0.10    --   72.03  77.00 -30.00  148
  8  \w     48.00 118.00   0.25    0.10    --   72.03  77.00  30.00  280
  9  \w     48.00  73.00   0.25    0.10    --   72.03  77.00 -30.00  100
 10  \w     98.00 145.00   0.25    0.10    --   72.03  77.00  60.00  188
 11  \w     48.00 145.00   0.25    0.10    --   72.03  77.00 162.77  388
 12  \w     48.00 117.00   0.25    0.10    --   72.03  77.00 150.00  276
 13  \w     47.00 117.00   0.25    0.10    --   72.03  80.00 124.71  280
 14  \w     48.00  77.00   0.25    0.10    --   72.03  77.00  90.00  116
 15  \w     48.00  73.00   0.25    0.10    --   72.03  77.00  60.00  100
 16  \w     49.00  75.00   0.25    0.10    --   72.03  76.00  22.51  104
 17  \w     49.00  96.00   0.25    0.10    --   72.03  75.00 112.34  188
 18  \w    105.00 131.00   0.25    0.10    --   72.03  75.00 112.34  104
 19  \w     50.00 145.00   0.25    0.10    --   72.03  74.00  45.76  380
 20  \w     49.00  75.00   0.25    0.10    --   72.03  75.00 -14.76  104
 21  \w     53.00  79.00   0.25    0.10    --   72.03  66.00  90.03  104
 22  \w    113.00 143.00   0.25    0.10    --   72.03  66.00  90.03  120
 23  \w    108.00 138.00   0.25    0.10    --   72.03  75.00 -14.76  120
 24  \w     51.00 100.00   0.25    0.10    --   72.03  71.00 -34.91  196
 25  \w     48.00 145.00   0.25    0.10    --   72.03  77.00-180.00  388
 26  \w     42.00  69.00   0.25    0.10    --   72.03-104.00-178.00  108
 27  \w     20.00  93.00   0.25    0.10    --   72.03-125.00  30.00  292
 28  \w     20.00  58.00   0.25    0.10    --   72.03-125.00 120.00  152
 29  \w     70.00 103.00   0.25    0.10    --   72.03-125.00 120.00  132
 30  \w     24.00  66.00   0.25    0.10    --   72.03 -57.00   0.00  168
 31  \w      8.00  61.00   0.25    0.10    --   72.03 -57.00  30.00  212
 32  \w    -70.00 -34.00   0.25    0.08    --   -1.72 -57.00-150.00  144
 33  \w    -22.00   9.00   0.25    0.08    --   -1.72 -57.00-150.00  124
 34  \w    -66.00  -2.00   0.25    0.08    --   -1.72 -57.00 -60.00  256
 35  \w    -75.00 -25.00   0.25    0.08    --   -1.72 -38.00-150.00  200
 36  \w    -18.00  13.00   0.25    0.08    --   -1.72 -38.00-150.00  124
 37  \w    103.00 128.00   0.25    0.10    --   72.03 104.00 -77.00  100
 38  \w    -74.00  11.00   0.25    0.08    --   -1.72 -38.00 -30.00  340
 39  \w    -49.00  12.00   0.25    0.08    --   -1.72 -57.00  30.00  244
 40  \w    -12.00  13.00   0.25    0.08    --   -1.72 -38.00  30.00  100
 41  \w    -45.00 -19.00   0.25    0.08    --   -1.72 -38.00  30.00  104
 42  \w    -70.00  13.00   0.25    0.08    --   -1.72 -57.00 120.00  332
 43  \w   -143.00-109.00   0.25    0.10    --  -75.46 -45.00 -42.17  136
 44  \w   -132.00 -95.00   0.25    0.10    --  -75.46 -77.00 -93.37  148
 45  \w    -92.00 -55.00   0.25    0.10    --  -75.46 -69.00 -85.50  148
 46  \w    -91.00 -61.00   0.25    0.10    --  -75.46 -45.00 -42.17  120
 47  \w    -85.00 -52.00   0.25    0.10    --  -75.46 -77.00 -93.37  132
 48  \w   -101.00 -50.00   0.25    0.10    --  -75.46 -80.00-116.39  204
 49  \w   -144.00-118.00   0.25    0.10    --  -75.46-104.00-178.00  104
 50  \w    -65.00 -22.00   0.25    0.10    --  -75.46  57.00-150.00  172
 51  \w    -98.00  -2.00   0.25    0.10    --  -75.46  77.00-150.00  384
 52  \w    -65.00  -4.00   0.25    0.10    --  -75.46  57.00 -90.00  244
 53  \w    -36.00 -10.00   0.25    0.10    --  -75.46  38.00 -90.00  104
 54  \w    -43.00  -7.00   0.25    0.10    --  -75.46  38.00 150.00  144
 55  \w   -101.00 -45.00   0.25    0.10    --  -75.46 104.00 -77.00  224
 56  \w   -110.00 -20.00   0.25    0.10    --  -75.46 125.00 -90.00  360
 57  \w   -110.00 -32.00   0.25    0.10    --  -75.46 125.00  60.00  312
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0645979000
_diffrn_orient_matrix_UB_12      -0.0092122000
_diffrn_orient_matrix_UB_13      -0.0247292000
_diffrn_orient_matrix_UB_21      -0.0525313000
_diffrn_orient_matrix_UB_22      -0.0397675000
_diffrn_orient_matrix_UB_23      -0.0319490000
_diffrn_orient_matrix_UB_31      -0.0237536000
_diffrn_orient_matrix_UB_32      0.0540821000
_diffrn_orient_matrix_UB_33      -0.0114490000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            248527
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        52.048
_diffrn_reflns_theta_max         52.048
_diffrn_reflns_theta_min         2.409
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.866
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       Flaky
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.102
_refine_diff_density_max         2.089
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2531
_refine_ls_number_reflns         34905
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0948P)^2^+31.3453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32656
_reflns_number_total             34905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00157d2.cif
_cod_data_source_block           xqd-1
_cod_depositor_comments
'Adding full bibliography for 7707021--7707026.cif.'
_cod_database_code               7707024
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N P F Cl Ru Fe '
_chemical_oxdiff_usercomment     'C H O N P F Cl Ru Fe'
_reflns_odcompleteness_completeness 99.95
_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. Restrained distances
 Cl4-C198 = Cl3-C198 = Cl2_$1-C197_$1 = Cl1_$1-C197_$1 = Cl7_$2-C200_$2 =
 Cl8_$2-C200_$2
 1.7 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C197) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C198) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Cl3(0.5) Cl2(0.5) Cl4(0.5) C198(0.5) H19V(0.5) H19W(0.5) C197(0.5)
 H19X(0.5) H19Y(0.5) Cl1(0.5) O2(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C62(H62A,H62B), C195(H19D,H19E), C196(H19F,H19G), C97(H97A,
 H97B), C160(H16A,H16B), C98(H98A,H98B), C159(H15J,H15K), C200(H20D,H20E),
 C199(H19T,H19U), C198(H19V,H19W), C197(H19X,H19Y)
5.b Aromatic/amide H refined with riding coordinates:
 C105(H105), C25(H25), C10(H10), C63(H63), C103(H103), C22(H22), C110(H110),
 C68(H68), C102(H102), C108(H108), C24(H24), C65(H65), C19(H19), C67(H67),
 C17(H17), C7(H7), C50(H50), C117(H117), C4(H4), C145(H145), C123(H123),
 C120(H120), C13(H13), C114(H114), C5(H5), C162(H162), C165(H165), C12(H12),
 C122(H122), C111(H111), C144(H144), C163(H163), C143(H143), C115(H115),
 C64(H64), C49(H49), C147(H147), C148(H148), C127(H127), C177(H177), C45(H45),
 C180(H180), C85(H85), C179(H179), C184(H184), C175(H175), C16(H16), C28(H28),
 C161(H161), C135(H135), C181(H181), C31(H31), C83(H83), C37(H37), C183(H183),
 C41(H41), C29(H29), C35(H35), C46(H46), C136(H136), C86(H86), C34(H34),
 C32(H32), C77(H77), C47(H47), C82(H82), C43(H43), C126(H126), C178(H178),
 C174(H174), C133(H133), C73(H73), C171(H171), C166(H166), C79(H79), C141(H141),
  C169(H169), C129(H129), C71(H71), C81(H81), C172(H172), C132(H132),
 C130(H130), C76(H76), C38(H38), C80(H80), C39(H39), C27(H27), C131(H131),
 C33(H33), C40(H40), C173(H173), C167(H167), C44(H44), C74(H74), C125(H125),
 C70(H70), C168(H168), C142(H142), C139(H139), C69(H69), C75(H75), C137(H137),
 C138(H138)
5.c Idealised Me refined as rotating group:
 C155(H15A,H15B,H15C), C192(H19A,H19B,H19C), C156(H15D,H15E,H15F), C106(H10A,
 H10B,H10C), C157(H15G,H15H,H15I), C57(H57A,H57B,H57C), C190(H19H,H19I,H19J),
 C96(H96A,H96B,H96C), C58(H58A,H58B,H58C), C191(H19K,H19L,H19M), C118(H11A,H11B,
 H11C), C93(H93A,H93B,H93C), C60(H60A,H60B,H60C), C158(H15L,H15M,H15N),
 C92(H92A,H92B,H92C), C59(H59A,H59B,H59C), C20(H20A,H20B,H20C), C194(H19N,H19O,
 H19P), C193(H19Q,H19R,H19S), C154(H15O,H15P,H15Q), C94(H94A,H94B,H94C),
 C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C56(H56A,H56B,H56C), C8(H8A,H8B,H8C),
  C124(H12A,H12B,H12C), C95(H95A,H95B,H95C), C112(H11D,H11E,H11F)
;
_shelx_res_checksum              18626
_shelx_hkl_checksum              60078
_shelx_fab_checksum              90986
_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 12.045
_oxdiff_exptl_absorpt_empirical_full_min 0.418