Dinitrogen Complexation and Extent of N\τbN Activation within the Group 6 "End-On-Bridged" Dinuclear Complexes, {(η5-C5Me5)M[N(i-Pr)C(Me)N(i-Pr)]}2(μ-η1:η1-N2) (M = Mo and W)
Philip P. Fontaine; Brendan L. Yonke; Peter Y. Zavalij; Lawrence R. Sita; Journal of the American Chemical Society 132 (2010) 12273–12285; doi:10.1021/ja100469f

data_4102986
_publ_section_title
;
 Dinitrogen Complexation and Extent of N\\tbN Activation within the Group
 6 "End-On-Bridged" Dinuclear Complexes,
 {(\h5-C5Me5)M[N(i-Pr)C(Me)N(i-Pr)]}2(\m-\h1:\h1-N2) (M = Mo and W)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12273
_journal_page_last               12285
_journal_paper_doi               10.1021/ja100469f
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C36 H64 N6 W2, 2(C36 H64 Cl2 N6 W2)'
_chemical_formula_sum            'C108 H192 Cl4 N18 W6'
_chemical_formula_weight         2987.70
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.4931(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.2729(11)
_cell_length_b                   16.9680(10)
_cell_length_c                   18.6155(11)
_cell_measurement_reflns_used    7886
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.2
_cell_volume                     5916.4(6)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      610,610,610,330
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'cactus needle'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0503004
_diffrn_orient_matrix_UB_12      0.0121515
_diffrn_orient_matrix_UB_13      -0.0048814
_diffrn_orient_matrix_UB_21      0.0291453
_diffrn_orient_matrix_UB_22      -0.0192381
_diffrn_orient_matrix_UB_23      0.0497649
_diffrn_orient_matrix_UB_31      0.0009269
_diffrn_orient_matrix_UB_32      -0.0543647
_diffrn_orient_matrix_UB_33      -0.0187068
_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  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50144
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.37
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.950
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       needle
_exptl_crystal_F_000             2956
_exptl_crystal_id
;
;
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.006
_refine_diff_density_max         3.643
_refine_diff_density_min         -2.772
_refine_diff_density_rms         0.196
_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     652
_refine_ls_number_reflns         10400
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0428
_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^)+(0.009P)^2^+88.4P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                7435
_reflns_number_total             10400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja100469f_si_009.cif
_cod_data_source_block           rac_12
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4102986