Synthesis, catalysis, and DFT study of a ruthenium carbene complex bearing a 1,2-dicarbadodecaborane (12)-1,2-dithiolate ligand.
Wang, Tao; Wu, Botao; Guo, Weijie; Wu, Shutao; Zhang, Huiqing; Dang, Yanfeng; Wang, Jianhui; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2646–2656; doi:10.1039/c8dt04290j

data_7048677
_publ_section_title
;
 Synthesis, catalysis, and DFT study of a ruthenium carbene complex
 bearing a 1,2-dicarbadodecaborane (12)-1,2-dithiolate ligand.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2646
_journal_page_last               2656
_journal_paper_doi               10.1039/c8dt04290j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C33 H49 B10 N2 O Ru S2, C H2 Cl2'
_chemical_formula_sum            'C34 H51 B10 Cl2 N2 O Ru S2'
_chemical_formula_weight         847.96
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1mh44d
_audit_creation_date             2016-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-10-17 deposited with the CCDC.
2019-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.9977(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.21465(12)
_cell_length_b                   21.5494(2)
_cell_length_c                   17.6658(2)
_cell_measurement_reflns_used    10205
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.9190
_cell_measurement_theta_min      4.2030
_cell_volume                     4123.85(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     92.00 124.00   1.00    1.00    --  107.08  30.00   0.00   32
  2  \w     89.00 173.00   1.00    1.00    --  107.08  61.00  90.00   84
  3  \w     95.00 175.00   1.00    1.00    --  107.08 125.00 -90.00   80
  4  \w    137.00 177.00   1.00    1.00    --  107.08  45.00-150.00   40
  5  \w     88.00 116.00   1.00    1.00    --   41.49  38.00-120.00   28
  6  \w     35.00 135.00   1.00    1.00    --  107.08 -61.00   0.00  100
  7  \w     87.00 116.00   1.00    1.00    --  107.08-125.00-120.00   29
  8  \w     71.00 108.00   1.00    1.00    --  107.08 -95.00 -90.00   37
  9  \w     46.00  72.00   1.00    1.00    --  107.08-125.00-120.00   26
 10  \w     35.00  68.00   1.00    1.00    --  107.08 -95.00   0.00   33
 11  \w    -31.00  17.00   1.00    1.00    --  -41.49  38.00  30.00   48
 12  \w    -95.00 -36.00   1.00    1.00    --  -41.49 125.00  30.00   59
 13  \w   -100.00 -17.00   1.00    1.00    --  -41.49 -38.00  90.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0775323000
_diffrn_orient_matrix_UB_12      0.0239666000
_diffrn_orient_matrix_UB_13      -0.0543235000
_diffrn_orient_matrix_UB_21      -0.0314730000
_diffrn_orient_matrix_UB_22      0.0672980000
_diffrn_orient_matrix_UB_23      0.0169764000
_diffrn_orient_matrix_UB_31      0.1149791000
_diffrn_orient_matrix_UB_32      0.0022991000
_diffrn_orient_matrix_UB_33      0.0700890000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15950
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         4.103
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.359
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.086
_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     477
_refine_ls_number_reflns         7363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0481P)^2^+3.9331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6640
_reflns_number_total             7363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04290j2.cif
_cod_data_source_block           a160315a
_cod_depositor_comments          'Adding full bibliography for 7048677.cif.'
_cod_original_cell_volume        4123.86(8)
_cod_database_code               7048677
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, 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:
 C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C22(H22A,H22B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C17(H17), C25(H25), C26(H26), C27(H27), C28(H28)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C)
2.e Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3A), B4(H4), B5(H5A), B6(H6), B7(H7), B8(H8), B9(H9),
 B016(H016)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-15
_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 1.542
_oxdiff_exptl_absorpt_empirical_full_min 0.693