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_4112842
_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            'C67 H103 N6 P4 Si8 Zr2'
_chemical_formula_weight         1523.59
_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                100.987(7)
_cell_angle_beta                 107.008(6)
_cell_angle_gamma                81.744(7)
_cell_formula_units_Z            2
_cell_length_a                   13.5924(11)
_cell_length_b                   24.6866(19)
_cell_length_c                   12.5430(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      16.2
_cell_measurement_theta_min      11.1
_cell_volume                     3933.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       'scintillation counter'
_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  0.03515
_diffrn_reflns_av_sigmaI/netI    0.090
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23796
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        -2.57
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
The scan width was (1.01+0.35tan\q)\% with an \w
scan speed of 16\% per minute 
(up to 10 scans to achieve I/\s(I) > 40).
Stationary background counts were recorded at each end of the
scan, and the scan time:background time ratio was 2:1.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       prism
_exptl_crystal_F_000             1598
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         22899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                13212
_reflns_number_total             22899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049490bsi20040210_020115_1.cif
_cod_data_source_block           mf305/Zr(PhCCH)
_cod_database_code               4112842