Synthesis of Molybdenum and Tungsten Alkylidene Complexes that Contain atert-Butylimido Ligand
Jeong, Hyangsoo; Schrock, Richard R.; Müller, Peter; Organometallics 34 (2015) 4408–; doi:10.1021/acs.organomet.5b00633

data_4087831
_publ_section_title
;
 Synthesis of Molybdenum and Tungsten Alkylidene Complexes that Contain
 atert-Butylimido Ligand
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4408
_journal_paper_doi               10.1021/acs.organomet.5b00633
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C24 H28 F18 Mo N2 O3'
_chemical_formula_weight         830.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5372(8)
_cell_length_b                   17.6547(9)
_cell_length_c                   21.0898(11)
_cell_measurement_reflns_used    9529
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.56
_cell_measurement_theta_min      2.50
_cell_volume                     6157.4(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            133122
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.301
_diffrn_reflns_theta_min         1.931
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.060
_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     644
_refine_ls_number_reflns         10068
_refine_ls_number_restraints     3442
_refine_ls_restrained_S_all      1.265
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+4.0154P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8708
_reflns_number_total             10068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00633_si_001.cif
_cod_data_source_block           x13120
_cod_database_code               4087831
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.849
_shelxl_version_number           2012-9
_shelx_hkl_checksum              24115