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_4086462
_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         'C40 H70 N6 W2'
_chemical_formula_sum            'C40 H70 N6 W2'
_chemical_formula_weight         1002.72
_chemical_name_systematic        W-complex
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                71.624(2)
_cell_angle_beta                 70.902(2)
_cell_angle_gamma                83.656(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4346(13)
_cell_length_b                   14.3892(18)
_cell_length_c                   15.865(2)
_cell_measurement_reflns_used    22243
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.1
_cell_measurement_theta_min      2.3
_cell_volume                     2136.1(5)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
crystal_id 'Sita-Yonke BY-10-27 needles 150K'
detector_distance 5.00
total_frames-CCD  3030
frame_width-CCD  -0.30
frame_size-CCD    512
;
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0884924
_diffrn_orient_matrix_UB_12      -0.0289273
_diffrn_orient_matrix_UB_13      0.0098299
_diffrn_orient_matrix_UB_21      0.0040209
_diffrn_orient_matrix_UB_22      0.0371486
_diffrn_orient_matrix_UB_23      -0.0657361
_diffrn_orient_matrix_UB_31      0.0493865
_diffrn_orient_matrix_UB_32      -0.0560915
_diffrn_orient_matrix_UB_33      -0.0215017
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            68468
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.414
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         12384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0236
_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^)+(0.01P)^2^+2.305P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0493
_reflns_number_gt                10515
_reflns_number_total             12384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00131_si_001.cif
_cod_data_source_block           cmpd_4
_cod_depositor_comments
'Adding full bibliography for 4086460--4086471.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4086462