Dipyrrolyl Precursors to Bisalkoxide Molybdenum Olefin Metathesis Catalysts
A. S. Hock; Richard R. Schrock; Amir H. Hoveyda; Journal of the American Chemical Society 128 (2006) 16373–16375; doi:10.1021/ja0665904

data_4111223
_publ_section_title
;
 Dipyrrolyl Precursors to Bisalkoxide Molybdenum Olefin Metathesis
 Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16373
_journal_page_last               16375
_journal_paper_doi               10.1021/ja0665904
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C67 H82 Mo2 N6'
_chemical_formula_weight         1163.27
_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                 106.001(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.903(12)
_cell_length_b                   12.723(5)
_cell_length_c                   19.434(9)
_cell_measurement_reflns_used    2623
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.82
_cell_measurement_theta_min      2.19
_cell_volume                     5919(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1879
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            88943
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.9546
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         7216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0172P)^2^+7.8129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                5195
_reflns_number_total             7216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0665904si20060911_055724.cif
_cod_data_source_block           06172
_cod_original_cell_volume        5919(4)
_cod_database_code               4111223