Synthesis of Molybdenum and Tungsten Alkylidene Complexes That Contain Sterically Demanding Arenethiolate Ligands.
Townsend, Erik M.; Hyvl, Jakub; Forrest, William P.; Schrock, Richard R.; Müller, Peter; Hoveyda, Amir H.; Organometallics 33 (2014) 5334–5341; doi:10.1021/om500655n

data_4084383
_publ_section_title
;
 Synthesis of Molybdenum and Tungsten Alkylidene Complexes That Contain
 Sterically Demanding Arenethiolate Ligands.
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5334
_journal_page_last               5341
_journal_paper_doi               10.1021/om500655n
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C61 H61 Mo N2 S'
_chemical_formula_weight         950.11
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                109.152(5)
_cell_angle_beta                 103.201(6)
_cell_angle_gamma                100.459(5)
_cell_formula_units_Z            2
_cell_length_a                   10.842(2)
_cell_length_b                   14.437(3)
_cell_length_c                   17.924(4)
_cell_measurement_reflns_used    9730
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.60
_cell_measurement_theta_min      2.50
_cell_volume                     2477.9(9)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14892
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         1.265
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.746251
_exptl_absorpt_correction_T_min  0.677014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         14892
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0480P)^2^+1.8151P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14212
_reflns_number_total             14892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500655n_si_001.cif
_cod_data_source_block           X8_13174_t5
_cod_depositor_comments
'Adding full bibliography for 4084383--4084386.cif.'
_cod_database_code               4084383
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2012-9
_shelx_res_checksum              75798
_shelx_hkl_checksum              51637