Cycloaddition reactions of transition metal hydrazides with alkynes and heteroalkynes: coupling of Ti=NNPh2 with PhCCMe, PhCCH, MeCN and tBuCP.
Selby, Jonathan D; Schulten, Christian; Schwarz, Andrew D; Stasch, Andreas; Clot, Eric; Jones, Cameron; Mountford, Philip; Chemical communications (Cambridge, England)  (2008) 5101–5103; doi:10.1039/b813911c

data_7103465
_publ_section_title
;
 Cycloaddition reactions of transition metal hydrazides with alkynes
 and heteroalkynes: coupling of Ti=NNPh2 with PhCCMe, PhCCH, MeCN and
 tBuCP.
;
_journal_issue                   41
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5101
_journal_page_last               5103
_journal_paper_doi               10.1039/b813911c
_journal_year                    2008
_chemical_formula_sum            'C27 H29 N2 P Ti'
_chemical_formula_weight         460.39
_chemical_name_systematic
;
Cp2Ti{N(NPh2)PCtBu}
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 110.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.654(3)
_cell_length_b                   9.4448(19)
_cell_length_c                   16.641(3)
_cell_measurement_temperature    123(2)
_cell_volume                     2303.1(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9086
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+1.2132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                3892
_reflns_number_total             4906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813911c.txt
_cod_data_source_block           Compound_7
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7103465