Molybdenum Imido Alkylidene Complexes Containing N- and C-Chelating N-Heterocyclic Carbenes
Elser, Iris; Frey, Wolfgang; Wurst, Klaus; Buchmeiser, Michael R.; Organometallics 35 (2016) 4106–; doi:10.1021/acs.organomet.6b00835

data_4089178
_publ_section_title
;
 Molybdenum Imido Alkylidene Complexes Containing N- and C-Chelating
 N-Heterocyclic Carbenes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              4106
_journal_paper_doi               10.1021/acs.organomet.6b00835
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C41 H48 Cl2 F3 Mo N3 O3 S'
_chemical_formula_weight         886.72
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                103.513(2)
_cell_angle_beta                 91.108(2)
_cell_angle_gamma                118.335(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3566(5)
_cell_length_b                   11.3694(4)
_cell_length_c                   19.1687(8)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.3
_cell_volume                     2093.50(16)
_computing_cell_refinement       'Bruker SAINT-V 8.34A'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT-V 8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL-XT-2014/4 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45519
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.061
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker (SADABS-2014/5)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       prism
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7374
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+3.3077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6078
_reflns_number_total             7374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00835_si_003.cif
_cod_data_source_block           bu162
_cod_original_cell_volume        2093.50(15)
_cod_database_code               4089178
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              72778
_shelx_hkl_checksum              46743