Titanium dipyrrolylmethane derivatives: rapid intermolecular alkyne hydroamination
Shi, Yanhui; Hall, Christopher; Ciszewski, James T.; Cao, Changsheng; Odom, Aaron L.; Chemical Communications (Cambridge, United Kingdom)  (2003) 586–587; doi:10.1039/b212423h

data_7113772
_publ_section_title
;
 Titanium dipyrrolylmethane derivatives: rapid intermolecular alkyne
 hydroamination
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   5
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              586
_journal_page_last               587
_journal_paper_doi               10.1039/b212423h
_journal_year                    2003
_chemical_formula_moiety         'C19 H32 N4 Ti'
_chemical_formula_sum            'C19 H32 N4 Ti'
_chemical_formula_weight         364.39
_chemical_name_common
;
bis(dimethylamido)(5,5-
dipropyldipyrrolylmethane)titanium(IV)
;
_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                 93.252(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9440(14)
_cell_length_b                   15.266(2)
_cell_length_c                   13.696(2)
_cell_measurement_temperature    446(2)
_cell_volume                     2075.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      446(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.2034
_diffrn_reflns_av_sigmaI/netI    0.1925
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9353
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.43
_refine_diff_density_max         1.194
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1837
_refine_ls_R_factor_gt           0.0876
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.3346
_reflns_number_gt                1415
_reflns_number_total             2980
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103993
_cod_data_source_file            201603.txt
_cod_data_source_block           shi60t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7113772