Group 4 Bis(pyrimidinoxide) Complexes. Investigations of Electronic Effects in Catalytic Hydroamination
Lee, Alison V.; Schafer, Laurel L.; Organometallics 25 (2006) 5249–; doi:10.1021/om060587b

data_4074368
_publ_section_title
;
 Group 4 Bis(pyrimidinoxide) Complexes. Investigations of Electronic
 Effects in Catalytic Hydroamination
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5249
_journal_paper_doi               10.1021/om060587b
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C30 H54 N6 O2 Ti'
_chemical_formula_sum            'C30 H54 N6 O2 Ti'
_chemical_formula_weight         578.69
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2n -2ac'
_symmetry_space_group_name_H-M   'P c 21 n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5710(8)
_cell_length_b                   17.7226(14)
_cell_length_c                   17.9379(15)
_cell_measurement_reflns_used    6407
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.267
_cell_measurement_theta_min      2.2435
_cell_volume                     3360.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71080
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69514
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  0.917227
_exptl_absorpt_correction_T_min  0.00137584
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7886
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                6545
_reflns_number_total             7886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060587bsi20060630_064525.cif
_cod_data_source_block           ls056_0m
_cod_database_code               4074368