Catalytic Production of Isocyanates via Orthogonal Atom and Group Transfers Employing a Shared Formal Group 6 M(II)/M(IV) Redox Cycle
Yonke, Brendan L.; Reeds, Jonathan P.; Fontaine, Philip P.; Zavalij, Peter Y.; Sita, Lawrence R.; Organometallics  (2014) 140626135101001–; doi:10.1021/om500532s

data_4083753
_publ_section_title
;
 Catalytic Production of Isocyanates via Orthogonal Atom and Group
 Transfers Employing a Shared Formal Group 6 M(II)/M(IV) Redox Cycle
;
_journal_name_full               Organometallics
_journal_page_first              140626135101001
_journal_paper_doi               10.1021/om500532s
_journal_year                    2014
_chemical_formula_moiety         'C22 H41 N3 W'
_chemical_formula_sum            'C22 H41 N3 W'
_chemical_formula_weight         531.43
_chemical_name_common            cmpd4
_chemical_name_systematic
;
cmpd4
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   17.3012(15)
_cell_length_b                   14.9156(13)
_cell_length_c                   9.1426(8)
_cell_measurement_reflns_used    19543
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.3
_cell_volume                     2359.3(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 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      610,610,610,1200
_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      -0.0012342
_diffrn_orient_matrix_UB_12      0.0612243
_diffrn_orient_matrix_UB_13      0.0445034
_diffrn_orient_matrix_UB_21      -0.0575879
_diffrn_orient_matrix_UB_22      0.0009341
_diffrn_orient_matrix_UB_23      -0.0091200
_diffrn_orient_matrix_UB_31      -0.0047550
_diffrn_orient_matrix_UB_32      -0.0273009
_diffrn_orient_matrix_UB_33      0.0994949
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            35466
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.35
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.906
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_id                'Sita/Yonke BY-9-032A 150K'
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.007
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         3562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0192
_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^)+(0.01P)^2^+4.58P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                3236
_reflns_number_total             3562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500532s_si_002.cif
_cod_data_source_block           cmpd4
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4083753