2-(Diphenylphosphinoylmethyl)pyrrole‒2-(diphenylphosphinomethyl)pyrrole (0.43/0.57) and tetrachlorido(5-diphenylphosphinomethyl-2<i>H</i>-pyrrole-κ^2^<i>N</i>,<i>P</i>)titanium(IV)
Broomfield, Lewis M.; Bochmann, Manfred; Wright, Joseph A.; Acta Crystallographica Section C 66 (2010) m79–m82; doi:10.1107/S0108270110004506

data_2017544
_publ_section_title
;2-(Diphenylphosphinoylmethyl)pyrrole--2-(diphenylphosphinomethyl)pyrrole
 (0.43/0.57) and
 tetrachlorido(5-diphenylphosphinomethyl-2<i>H</i>-pyrrole-\k^2^<i>N</i>,<i>P</i>)titanium(IV)
;
_journal_coeditor_code           EM3032
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m79
_journal_page_last               m82
_journal_paper_doi               10.1107/S0108270110004506
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[TiCl4 (C17 H16 N P)]'
_chemical_formula_moiety         'C17 H16 Cl4 N P Ti'
_chemical_formula_sum            'C17 H16 Cl4 N P Ti'
_chemical_formula_weight         454.98
_chemical_name_common            'Compound (VI)'
_chemical_name_systematic
;
tetrachlorido(5-diphenylphosphinomethyl-2<i>H</i>-pyrrole-
\k^2^<i>N</i>,<i>P</i>)titanium(IV)
;
_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
_cell_angle_alpha                98.159(15)
_cell_angle_beta                 98.727(16)
_cell_angle_gamma                100.588(16)
_cell_formula_units_Z            2
_cell_length_a                   8.1481(17)
_cell_length_b                   8.6323(16)
_cell_length_c                   14.202(3)
_cell_measurement_reflns_used    1842
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.4954
_cell_measurement_theta_min      3.4588
_cell_volume                     955.6(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009), WinGX
(Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1121
_diffrn_reflns_av_sigmaI/netI    0.1577
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10184
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.090
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.483
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.889
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0307P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                1864
_reflns_number_total             3347
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            em3032.cif
_cod_data_source_block           IV
_cod_database_code               2017544
_cod_database_fobs_code          2017544