Carbon-Nitrogen Bond Formation via the Reaction of Terminal Alkynes with a Dinuclear Side-on Dinitrogen Complex
Lara Morello; Jason B. Love; Brian O. Patrick; Michael D. Fryzuk; Journal of the American Chemical Society 126 (2004) 9480–9481; doi:10.1021/ja049490b

data_4112843
_publ_section_title
;
 Carbon-Nitrogen Bond Formation via the Reaction of Terminal Alkynes with
 a Dinuclear Side-on Dinitrogen Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9480
_journal_page_last               9481
_journal_paper_doi               10.1021/ja049490b
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C69 H107 N6 P4 Si8 Zr2'
_chemical_formula_weight         1551.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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
_cell_angle_alpha                91.876(2)
_cell_angle_beta                 103.2790(10)
_cell_angle_gamma                107.544(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5329(7)
_cell_length_b                   13.3989(5)
_cell_length_c                   25.9965(18)
_cell_measurement_reflns_used    18902
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.76
_cell_volume                     4026.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15659
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7231
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1630
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         15659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+10.5122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                12548
_reflns_number_total             15659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049490bsi20040210_020115_2.cif
_cod_data_source_block           mf449
_cod_database_code               4112843