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_4089177
_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_moiety
'C37 H40 F3 Mo N4 O3 S, C32 H12 B F24, C H2 Cl2'
_chemical_formula_sum            'C70 H54 B Cl2 F27 Mo N4 O3 S'
_chemical_formula_weight         1721.88
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.026(3)
_cell_angle_beta                 86.625(4)
_cell_angle_gamma                80.441(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0581(6)
_cell_length_b                   17.0305(8)
_cell_length_c                   21.8889(12)
_cell_measurement_reflns_used    9116
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.59
_cell_measurement_theta_min      2.07
_cell_volume                     3602.1(3)
_computing_cell_refinement       'Bruker APEXII Software Suite, 2008'
_computing_data_collection       'Bruker APEXII Software Suite, 2008'
_computing_data_reduction        'Bruker APEXII Software Suite, 2008'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         I\mS
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47409
_diffrn_reflns_theta_full        65.59
_diffrn_reflns_theta_max         65.59
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.524
_exptl_absorpt_correction_T_max  0.8132
_exptl_absorpt_correction_T_min  0.6017
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.757
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         12191
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+0.3905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1491
_reflns_number_gt                9116
_reflns_number_total             12191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00835_si_003.cif
_cod_data_source_block           buch147b_(compound_2)
_cod_database_code               4089177