Small-Molecule Activation within the Group 6 Complexes (η5-C5Me5)[N(iPr)C(Me)N(iPr)]M(CO)(L) for M = Mo, W and L = N2, NCMe, η2-Alkene, SMe2, C3H6O
Farrell, Wesley S.; Yonke, Brendan L.; Reeds, Jonathan P.; Zavalij, Peter Y.; Sita, Lawrence R.; Organometallics 35 (2016) 1132–; doi:10.1021/acs.organomet.6b00131

data_4086468
_publ_section_title
;
 Small-Molecule Activation within the Group 6 Complexes
 (\h5-C5Me5)[N(iPr)C(Me)N(iPr)]M(CO)(L) for M = Mo, W and L = N2, NCMe,
 \h2-Alkene, SMe2, C3H6O
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1132
_journal_paper_doi               10.1021/acs.organomet.6b00131
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C22 H40 N2 W'
_chemical_formula_sum            'C22 H40 N2 W'
_chemical_formula_weight         516.41
_chemical_name_systematic        W-complex
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 107.0081(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1265(19)
_cell_length_b                   9.0774(11)
_cell_length_c                   16.571(2)
_cell_measurement_reflns_used    12948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.7
_cell_measurement_theta_min      2.5
_cell_volume                     2175.8(5)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2014, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0018707
_diffrn_orient_matrix_UB_12      -0.0145240
_diffrn_orient_matrix_UB_13      -0.0593002
_diffrn_orient_matrix_UB_21      -0.0681788
_diffrn_orient_matrix_UB_22      -0.0181468
_diffrn_orient_matrix_UB_23      -0.0185008
_diffrn_orient_matrix_UB_31      -0.0112966
_diffrn_orient_matrix_UB_32      0.1076914
_diffrn_orient_matrix_UB_33      -0.0111144
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26101
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.544
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.316
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.477
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0300P)^2^+4.9500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4325
_reflns_number_total             4999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00131_si_001.cif
_cod_data_source_block           cmpd_15
_cod_depositor_comments
'Adding full bibliography for 4086460--4086471.cif.'
_cod_original_cell_volume        2175.9(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4086468
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.308
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              50625
_shelx_hkl_checksum              15738