Synthesis of Monoalkoxide Monopyrrolyl Complexes Mo(NR)(CHR')(OR'')(pyrrolyl): Enyne Metathesis with High Oxidation State Catalysts
Rojendra Singh; Richard R. Schrock; Peter Müller; Amir H. Hoveyda; Journal of the American Chemical Society 129 (2007) 12654–12655; doi:10.1021/ja075569f

data_4110070
_publ_section_title
;
 Synthesis of Monoalkoxide Monopyrrolyl Complexes
 Mo(NR)(CHR')(OR'')(pyrrolyl): Enyne Metathesis with High Oxidation State
 Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12654
_journal_page_last               12655
_journal_paper_doi               10.1021/ja075569f
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C40 H54 Mo N2 O'
_chemical_formula_weight         674.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.454(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.762(3)
_cell_length_b                   22.614(5)
_cell_length_c                   13.619(3)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.76
_cell_measurement_theta_min      2.35
_cell_volume                     3606.1(15)
_computing_cell_refinement       'SAINT 7 (Bruker-AXS, 2005)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 7 (Bruker-AXS, 2005)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            79432
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  0.9251
_exptl_absorpt_correction_T_min  0.9076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         10117
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+2.0490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                8918
_reflns_number_total             10117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075569fsi20070824_014556.cif
_cod_data_source_block           07040
_cod_original_cell_volume        3606.0(13)
_cod_database_code               4110070