A 3,4-dimercapto-3-cyclobutene-1,2-dione-chelated ruthenium carbene catalyst for Z-stereoretentive/stereoselective olefin metathesis.
Wang, Tao; Xie, Qingxiao; Guo, Weijie; Wu, Shutao; Zhang, Huiqing; Wang, Jianhui; Wu, Botao; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6473–6483; doi:10.1039/c9dt01016e

data_7049552
_publ_section_title
;
 A 3,4-dimercapto-3-cyclobutene-1,2-dione-chelated ruthenium carbene
 catalyst for Z-stereoretentive/stereoselective olefin metathesis.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6473
_journal_page_last               6483
_journal_paper_doi               10.1039/c9dt01016e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C35 H39 N2 O3 Ru S2'
_chemical_formula_sum            'C35 H39 N2 O3 Ru S2'
_chemical_formula_weight         700.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-13 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.192(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3991(4)
_cell_length_b                   11.4101(2)
_cell_length_c                   31.8762(7)
_cell_measurement_reflns_used    7189
_cell_measurement_temperature    135.00(10)
_cell_measurement_theta_max      73.5220
_cell_measurement_theta_min      4.4920
_cell_volume                     6869.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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      135.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -65.00  28.00   1.00    9.50    --  -41.49  77.00  60.00   93
  2  \w    -35.00  -8.00   1.00    9.50    --  -41.49 125.00 -60.00   27
  3  \w   -114.00 -24.00   1.00    9.50    --  -41.49 -38.00  90.00   90
  4  \w     44.00 120.00   1.00   37.99    --  107.08 -61.00 -90.00   76
  5  \w     25.00 100.00   1.00   37.99    --  107.08 -95.00-180.00   75
  6  \w     79.00 145.00   1.00   37.99    --  107.08  61.00   0.00   66
  7  \w    103.00 129.00   1.00   37.99    --  107.08 125.00  90.00   26
  8  \w     26.00 101.00   1.00   37.99    --  107.08 -95.00-120.00   75
  9  \w     81.00 167.00   1.00   37.99    --  107.08  30.00  90.00   86
 10  \w     28.00  55.00   1.00   37.99    --  107.08 -95.00-150.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0722441000
_diffrn_orient_matrix_UB_12      -0.0483164000
_diffrn_orient_matrix_UB_13      0.0242592000
_diffrn_orient_matrix_UB_21      0.0305929000
_diffrn_orient_matrix_UB_22      0.0242745000
_diffrn_orient_matrix_UB_23      -0.0396978000
_diffrn_orient_matrix_UB_31      0.0222766000
_diffrn_orient_matrix_UB_32      0.1238133000
_diffrn_orient_matrix_UB_33      0.0172212000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12337
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         4.128
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
TITL A171109b  I 2/a        R = 0.07
CELL   19.3991   11.4101   31.8762     90.00    103.19     90.00
SPGR I2/a
C101 0.794 0.432 0.047 !       7.18 eA-3
C102 0.211 0.519 0.023 !       2.69 eA-3
C103 0.164 0.392 0.025 !       1.57 eA-3
C104 0.176 0.463 0.045 !       1.42 eA-3
Q105 0.033 1.002 0.053 !       0.90 eA-3
Q106 0.051 0.984 0.110 !       0.76 eA-3
Q107 0.824 0.480 0.245 !       0.69 eA-3
Q108 0.073 0.987 0.165 !       0.58 eA-3
;
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0397P)^2^+7.1794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5635
_reflns_number_total             6122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01016e2.cif
_cod_data_source_block           a171109b_sq
_cod_depositor_comments          'Adding full bibliography for 7049552.cif.'
_cod_original_cell_volume        6869.4(3)
_cod_database_code               7049552
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C17(H17), C27(H27), C28(H28), C29(H29), C30(H30)
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), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_platon_squeeze_void_probe_radius 1.20
_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 1.538
_oxdiff_exptl_absorpt_empirical_full_min 0.589