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_4083755
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H41 N3 O2 W'
_chemical_formula_sum            'C24 H41 N3 O2 W'
_chemical_formula_weight         587.45
_chemical_name_common            cmpd14
_chemical_name_systematic
;
cmpd14
;
_space_group_IT_number           1
_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                80.3400(10)
_cell_angle_beta                 79.0430(10)
_cell_angle_gamma                71.1220(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7965(7)
_cell_length_b                   9.5886(8)
_cell_length_c                   15.9747(14)
_cell_measurement_reflns_used    6899
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.3
_cell_volume                     1243.46(18)
_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_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      0.1012397
_diffrn_orient_matrix_UB_12      0.0256104
_diffrn_orient_matrix_UB_13      0.0007360
_diffrn_orient_matrix_UB_21      -0.0636132
_diffrn_orient_matrix_UB_22      0.0806215
_diffrn_orient_matrix_UB_23      0.0366019
_diffrn_orient_matrix_UB_31      0.0212311
_diffrn_orient_matrix_UB_32      -0.0717899
_diffrn_orient_matrix_UB_33      0.0527186
_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  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10425
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.668
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.051
_refine_diff_density_min         -5.313
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.490(19)
_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     446
_refine_ls_number_reflns         8385
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0464
_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^+18.4P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.914
_reflns_number_gt                7142
_reflns_number_total             8385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500532s_si_002.cif
_cod_data_source_block           cmpd14
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4083755