A Class III asymmetric binuclear cyanido-bridged mixed-valence complex
Liu, Xiao-Lin; Li, Yi; Xu, Qing-Dou; Wei, Zi-Qin; Wu, Xin-Tao; Sheng, Tian-Lu; New Journal of Chemistry 46 (2022) 7922–7927; doi:10.1039/D2NJ00311B

data_7061412
_publ_section_title
;
 A Class III asymmetric binuclear cyanido-bridged mixed-valence complex
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7922
_journal_page_last               7927
_journal_paper_doi               10.1039/D2NJ00311B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C57 H55 Cl N5 P2 Ru2, C H2 Cl2, B F4'
_chemical_formula_sum            'C58 H57 B Cl3 F4 N5 P2 Ru2'
_chemical_formula_weight         1281.32
_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
_audit_creation_date             2022-03-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-23 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.115(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0409(3)
_cell_length_b                   12.7863(4)
_cell_length_c                   39.5972(12)
_cell_measurement_reflns_used    17041
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.4670
_cell_measurement_theta_min      2.0120
_cell_volume                     5589.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_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     76.00 112.00   0.50    0.31    --   73.53 132.00-172.00   72
  2  \w     72.00 147.00   0.50    0.31    --   73.53 137.00   4.00  150
  3  \w     69.00 147.00   0.50    0.31    --   73.53  57.00   0.00  156
  4  \w     47.00 104.00   0.50    0.31    --   73.53-132.00 118.00  114
  5  \w      1.00  64.00   0.50    0.31    --   73.53 -77.00 120.00  126
  6  \w     66.00 120.00   0.50    0.31    --   73.53-137.00 -58.00  108
  7  \w    -15.00  71.00   0.50    0.08    --   -0.62  38.00 -30.00  172
  8  \w     17.00  62.00   0.50    0.08    --   -0.62  38.00  90.00   90
  9  \w    -96.00  -3.00   0.50    0.31    --  -74.78  77.00  30.00  186
 10  \w    -71.00 -20.00   0.50    0.31    --  -74.78  38.00 -30.00  102
 11  \w    -74.00  -4.00   0.50    0.31    --  -74.78  57.00-150.00  140
 12  \w    -88.00 -63.00   0.50    0.31    --  -74.78 137.00   4.00   50
 13  \w    -94.00 -69.00   0.50    0.31    --  -74.78 132.00-172.00   50
 14  \w   -126.00 -90.00   0.50    0.31    --  -74.78 -99.00-180.00   72
 15  \w   -134.00-109.00   0.50    0.31    --  -74.78-137.00 -58.00   50
 16  \w   -147.00-103.00   0.50    0.31    --  -74.78-125.00  60.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Synergy Custom(Liquid MetalJet D2+)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            47272
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.642
_diffrn_reflns_theta_min         1.940
_exptl_absorpt_coefficient_mu    4.504
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         12488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0638P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9651
_reflns_number_total             12488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00311b2.cif
_cod_data_source_block           dppb_auto
_cod_depositor_comments
'Adding full bibliography for 7061410--7061412.cif.'
_cod_database_code               7061412
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.614
_shelx_estimated_absorpt_t_min   0.424
_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 Secondary CH2 refined with riding coordinates:
 C014(H01A,H01B), C018(H01C,H01D), C023(H02A,H02B)
2.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00K(H00K), C00L(H00L), C00M(H00M), C00O(H00O), C00P(H00P),
 C00T(H00T), C011(H011), C013(H013), C015(H015), C016(H016), C017(H017),
 C019(H019), C01A(H01E), C01B(H01F), C01C(H01G), C01D(H01H), C01E(H01I),
 C01F(H01J), C01H(H01N), C01I(H01O), C01J(H01P), C01M(H01W), C01N(H01X),
 C01O(H01Y), C01P(H01Z), C01Q(H01), C01R(H1), C01S(H2), C01T(H3), C01U(H4),
 C01V(H5), C01W(H6), C01X(H7), C020(H020), C022(H022)
2.c Idealised Me refined as rotating group:
 C01G(H01K,H01L,H01M), C01K(H01Q,H01R,H01S), C01L(H01T,H01U,H01V), C01Y(H8,H,
 HA), C01Z(H9,HB,HC)
;
_shelx_res_checksum              86856
_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
;