Synthesis, Structure, and Characterization of the Hydrogen-Substituted Imido Complex TiCl2(NH)(OPPh3)2
Peggy J. McKarns; Glenn P. A. Yap; Arnold L. Rheingold; Charles H. Winter; Inorganic Chemistry 35 (1996) 5968–5969; doi:10.1021/ic960595s

data_4323947
_publ_contact_author
;
        Prof. C.H. Winter
        Wayne State University
        Department of Chemistry
        Detroit, Michigan 48202

;
_publ_contact_author_email       cwinter@sun.science.wayne.edu
_publ_contact_author_fax         '313 577 2099'
_publ_contact_author_phone       '313 577 3097'
_publ_section_title
;
 Synthesis, Structure, and Characterization of the Hydrogen-Substituted
 Imido Complex TiCl2(NH)(OPPh3)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5968
_journal_page_last               5969
_journal_paper_doi               10.1021/ic960595s
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C36 H31 Cl2 N O2 P2 Ti'
_chemical_formula_weight         690.36
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.341(6)
_cell_length_b                   18.390(6)
_cell_length_c                   11.308(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     3568(2)
_computing_cell_refinement       P4
_computing_data_collection       P4
_computing_data_reduction        XDISK
_computing_molecular_graphics    XP
_computing_publication_material  XPUBL
_computing_structure_refinement  'SHELXL V4.2 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       Wyckoff
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0934
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4399
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       Block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.700
_refine_ls_goodness_of_fit_obs   1.700
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.700
_refine_ls_restrained_S_obs      1.700
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_obs          0.0850
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo) + 0.001(Fo)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1134
_refine_ls_wR_factor_obs         0.0936
_reflns_number_observed          2287
_reflns_number_total             4163
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960595s.cif
_cod_data_source_block           win01
_cod_database_code               4323947