Insertion Reactions of trans-Mo(dmpe)2(H)(NO) with Imines
Fupei Liang; Helmut W. Schmalle; Heinz Berke; Inorganic Chemistry 43 (2004) 993–999; doi:10.1021/ic030139l

data_4310492
_publ_contact_author             'Helmut W. Schmalle'
_publ_contact_author_email       schmalle@aci.unizh.ch
_publ_section_title
;
 Insertion Reactions of trans-Mo(dmpe)2(H)(NO) with Imines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              993
_journal_page_last               999
_journal_paper_doi               10.1021/ic030139l
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C25 H44 Mo N2 O P4'
_chemical_formula_weight         608.44
_chemical_name_systematic
;
Nitrosyl-bis(dimethylphosphinoethane)-N-phenylbenzylamine-
molybdenum
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.615(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1592(6)
_cell_length_b                   15.9501(7)
_cell_length_c                   20.6001(13)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.3
_cell_measurement_theta_min      2.65
_cell_volume                     2989.4(3)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_molecular_graphics    'PLATON, PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'STOE IPDS diffractometer'
_diffrn_measurement_method       '\f oscillation scan'
_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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31734
_diffrn_reflns_theta_full        30.31
_diffrn_reflns_theta_max         30.31
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ' image'
_diffrn_standards_interval_time  6.0
_diffrn_standards_number         '50 to 200'
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  0.9241
_exptl_absorpt_correction_T_min  0.8238
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Coppens et al. 1965'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.521
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         8864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0486
_reflns_number_gt                6060
_reflns_number_total             8864
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ic030139l.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4310492