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_4086460
_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_absolute_configuration ad
_chemical_formula_moiety         'C21 H36 Mo N2 O'
_chemical_formula_sum            'C21 H36 Mo N2 O'
_chemical_formula_weight         428.46
_chemical_name_systematic        Mo-complex
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6431(10)
_cell_length_b                   14.9247(17)
_cell_length_c                   16.4976(19)
_cell_measurement_reflns_used    19856
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3
_cell_measurement_theta_min      2.5
_cell_volume                     2128.1(4)
_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 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
crystal_id        ' '
frame_width-CCD  -0.30
total_frames-CCD  3030
frame_size-CCD    512
frame_time-CCD    15
total_time-CCD    17.7
detector_distance 5.00
;
_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      0.0270787
_diffrn_orient_matrix_UB_12      0.0012012
_diffrn_orient_matrix_UB_13      0.0589218
_diffrn_orient_matrix_UB_21      -0.0392008
_diffrn_orient_matrix_UB_22      -0.0627010
_diffrn_orient_matrix_UB_23      0.0060083
_diffrn_orient_matrix_UB_31      0.1054365
_diffrn_orient_matrix_UB_32      -0.0235998
_diffrn_orient_matrix_UB_33      -0.0129058
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33796
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.002
_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^+0.966P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0383
_refine_ls_wR_factor_ref         0.0388
_reflns_Friedel_coverage         0.932
_reflns_number_gt                5966
_reflns_number_total             6194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00131_si_001.cif
_cod_data_source_block           cmpd_8
_cod_depositor_comments
'Adding full bibliography for 4086460--4086471.cif.'
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               4086460