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_4083756
_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         'C21 H35 Mo N3 O'
_chemical_formula_sum            'C21 H35 Mo N3 O'
_chemical_formula_weight         441.46
_chemical_name_common            cmpd15
_chemical_name_systematic
;
cmpd15
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   14.5544(6)
_cell_length_b                   15.7135(6)
_cell_length_c                   19.3095(7)
_cell_measurement_reflns_used    24540
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.2
_cell_volume                     4416.1(3)
_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  'Sita-Reeds JPR-4-33A 150K'
total frames 1830
frame time     60 sec
total time     33.5 h
frame width    -0.3 deg
detector dist.  5.0 cm
frame_size    512 pix
;
_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      0.0394096
_diffrn_orient_matrix_UB_12      0.0509027
_diffrn_orient_matrix_UB_13      0.0091514
_diffrn_orient_matrix_UB_21      -0.0119761
_diffrn_orient_matrix_UB_22      -0.0058390
_diffrn_orient_matrix_UB_23      0.0507747
_diffrn_orient_matrix_UB_31      0.0549934
_diffrn_orient_matrix_UB_32      -0.0377475
_diffrn_orient_matrix_UB_33      0.0044953
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0118
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44649
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.343
_exptl_crystal_size_min          0.314
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.049
_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     259
_refine_ls_number_reflns         6433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0200
_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^+3.34P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0450
_reflns_number_gt                5724
_reflns_number_total             6433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500532s_si_002.cif
_cod_data_source_block           cmpd15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4083756