Carbon Monoxide-Induced N-N Bond Cleavage of Nitrous Oxide That Is Competitive with Oxygen Atom Transfer to Carbon Monoxide As Mediated by a Mo(II)/Mo(IV) Catalytic Cycle
Jonathan P. Reeds; Brendan L. Yonke; Peter Y. Zavalij; Lawrence R. Sita; Journal of the American Chemical Society 133 (2011) 18602–18605; doi:10.1021/ja208669s

data_4107145
_publ_section_title
;
 Carbon Monoxide-Induced N-N Bond Cleavage of Nitrous Oxide That Is
 Competitive with Oxygen Atom Transfer to Carbon Monoxide As Mediated by a
 Mo(II)/Mo(IV) Catalytic Cycle
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18602
_journal_page_last               18605
_journal_paper_doi               10.1021/ja208669s
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H32 Mo N4 O2'
_chemical_formula_sum            'C19 H32 Mo N4 O2'
_chemical_formula_weight         444.43
_chemical_name_systematic        'Cmpd 7'
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                90.00
_cell_angle_beta                 90.5680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1178(4)
_cell_length_b                   13.4299(6)
_cell_length_c                   17.0872(8)
_cell_measurement_reflns_used    15331
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.4
_cell_volume                     2092.24(16)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_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      100(2)
_diffrn_detector                 'CCD area detector'
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_diffrn_detector_type            'Bruker Smart Apex2, CCD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      610,610,610,941
_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      -0.1095281
_diffrn_orient_matrix_UB_12      -0.0044624
_diffrn_orient_matrix_UB_13      -0.0001336
_diffrn_orient_matrix_UB_21      -0.0019859
_diffrn_orient_matrix_UB_22      0.0125688
_diffrn_orient_matrix_UB_23      -0.0576637
_diffrn_orient_matrix_UB_31      0.0063875
_diffrn_orient_matrix_UB_32      -0.0732628
_diffrn_orient_matrix_UB_33      -0.0098896
_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  0.0153
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15955
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.38
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_id
;
;
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   -0.013(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5959
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0157
_refine_ls_shift/su_max          0.000
_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^+2.385P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0375
_reflns_Friedel_coverage         0.950
_reflns_number_gt                5912
_reflns_number_total             5959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208669s_si_002.cif
_cod_data_source_block           cmpd7
_cod_database_code               4107145