Synthesis of Molybdenum and Tungsten Alkylidene Complexes That Contain the 2,6-Bis(2,4,6-triisopropylphenyl)phenylimido (NHIPT) Ligand
Axtell, Jonathan C.; Schrock, Richard R.; Müller, Peter; Hoveyda, Amir H.; Organometallics 34 (2015) 2110–; doi:10.1021/om501213x

data_4085433
_publ_section_title
;
 Synthesis of Molybdenum and Tungsten Alkylidene Complexes That Contain
 the 2,6-Bis(2,4,6-triisopropylphenyl)phenylimido (NHIPT) Ligand
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2110
_journal_paper_doi               10.1021/om501213x
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C41 H59 Cl2 N W'
_chemical_formula_weight         820.64
_chemical_name_systematic
; 
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.2637(18)
_cell_length_b                   16.7591(18)
_cell_length_c                   24.480(3)
_cell_measurement_reflns_used    9680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.14
_cell_measurement_theta_min      2.32
_cell_volume                     7903.2(15)
_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-2014 (Sheldrick, 2014)'
_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  0.0966
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            141820
_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         30.506
_diffrn_reflns_theta_min         1.813
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    3.086
_exptl_absorpt_correction_T_max  0.4942
_exptl_absorpt_correction_T_min  '0.3487 0.4942'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.382
_refine_diff_density_min         -2.089
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         12060
_refine_ls_number_restraints     2343
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+55.5689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8889
_reflns_number_total             12060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501213x_si_005.cif
_cod_data_source_block           X14136
_cod_depositor_comments
'Adding full bibliography for 4085432--4085433.cif.'
_cod_original_cell_volume        7903.2(14)
_cod_database_code               4085433
_shelx_estimated_absorpt_t_min   0.622
_shelx_estimated_absorpt_t_max   0.802
_shelxl_version_number           2014-2
_shelx_res_checksum              29337
_shelx_hkl_checksum              49184