#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/75/2017544.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2017544
loop_
_publ_author_name
'Broomfield, Lewis M.'
'Bochmann, Manfred'
'Wright, Joseph A.'
_publ_section_title
;2-(Diphenylphosphinoylmethyl)pyrrole--2-(diphenylphosphinomethyl)pyrrole
 (0.43/0.57) and
 tetrachlorido(5-diphenylphosphinomethyl-2H-pyrrole-κ²N,P)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-2H-pyrrole-
κ²N,P)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 et al., 2004)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al.,  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 φ and ω 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/[σ²(Fo²)+(0.0307P)²] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            em3032.cif
_cod_data_source_block           IV
_cod_database_code               2017544
_cod_database_fobs_code          2017544
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti1 0.26998(13) 0.27029(11) 0.21430(7) 0.0204(3) Uani d . 1 . .
C C1 0.2003(7) 0.6387(6) 0.1838(3) 0.0185(13) Uani d . 1 . .
H H1A 0.0814 0.6171 0.1942 0.022 Uiso calc R 1 . .
H H1B 0.2358 0.7540 0.1819 0.022 Uiso calc R 1 . .
C C2 0.2159(6) 0.5402(6) 0.0921(4) 0.0176(13) Uani d . 1 . .
C C3 0.2492(7) 0.3295(6) -0.0073(4) 0.0253(14) Uani d . 1 . .
H H3A 0.1562 0.2354 -0.0345 0.030 Uiso calc R 1 . .
H H3B 0.3593 0.2974 -0.0094 0.030 Uiso calc R 1 . .
C C4 0.2342(7) 0.4612(7) -0.0612(4) 0.0246(14) Uani d . 1 . .
H H4 0.2386 0.4575 -0.1279 0.030 Uiso calc R 1 . .
C C5 0.2135(7) 0.5852(6) -0.0017(4) 0.0250(14) Uani d . 1 . .
H H5 0.1996 0.6857 -0.0179 0.030 Uiso calc R 1 . .
C C6 0.5492(7) 0.6938(6) 0.2772(4) 0.0189(13) Uani d . 1 . .
C C7 0.6838(7) 0.6629(6) 0.3385(4) 0.0271(14) Uani d . 1 . .
H H7 0.6633 0.5861 0.3794 0.032 Uiso calc R 1 . .
C C8 0.8448(7) 0.7418(6) 0.3405(4) 0.0293(15) Uani d . 1 . .
H H8 0.9364 0.7177 0.3818 0.035 Uiso calc R 1 . .
C C9 0.8775(7) 0.8567(6) 0.2834(4) 0.0283(15) Uani d . 1 . .
H H9 0.9904 0.9124 0.2857 0.034 Uiso calc R 1 . .
C C10 0.7446(7) 0.8889(6) 0.2236(4) 0.0248(14) Uani d . 1 . .
H H10 0.7655 0.9675 0.1839 0.030 Uiso calc R 1 . .
C C11 0.5816(7) 0.8089(6) 0.2204(4) 0.0226(14) Uani d . 1 . .
H H11 0.4903 0.8329 0.1789 0.027 Uiso calc R 1 . .
C C12 0.2900(7) 0.6707(6) 0.3933(4) 0.0175(13) Uani d . 1 . .
C C13 0.3162(7) 0.8355(6) 0.4170(4) 0.0258(14) Uani d . 1 . .
H H13 0.3632 0.9005 0.3750 0.031 Uiso calc R 1 . .
C C14 0.2747(7) 0.9073(7) 0.5018(4) 0.0293(15) Uani d . 1 . .
H H14 0.2921 1.0205 0.5178 0.035 Uiso calc R 1 . .
C C15 0.2078(7) 0.8110(7) 0.5619(4) 0.0243(14) Uani d . 1 . .
H H15 0.1784 0.8583 0.6199 0.029 Uiso calc R 1 . .
C C16 0.1833(7) 0.6489(7) 0.5395(4) 0.0248(14) Uani d . 1 . .
H H16 0.1393 0.5844 0.5825 0.030 Uiso calc R 1 . .
C C17 0.2219(7) 0.5774(6) 0.4547(4) 0.0243(14) Uani d . 1 . .
H H17 0.2016 0.4641 0.4388 0.029 Uiso calc R 1 . .
Cl Cl1 0.54140(19) 0.28949(17) 0.19072(11) 0.0306(4) Uani d . 1 . .
Cl Cl2 0.00233(18) 0.30511(16) 0.23398(10) 0.0270(4) Uani d . 1 . .
Cl Cl3 0.3352(2) 0.21919(17) 0.36339(10) 0.0314(4) Uani d . 1 . .
Cl Cl4 0.1693(2) 0.02861(16) 0.11559(11) 0.0325(4) Uani d . 1 . .
N N1 0.2376(5) 0.3943(5) 0.0920(3) 0.0208(11) Uani d . 1 . .
P P1 0.33927(19) 0.58169(16) 0.27991(10) 0.0180(4) Uani d . 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ti1 Cl3 . . 162.51(12) ?
N1 Ti1 Cl1 . . 85.23(13) ?
Cl3 Ti1 Cl1 . . 92.25(7) ?
N1 Ti1 Cl4 . . 91.10(12) y
Cl3 Ti1 Cl4 . . 106.38(7) y
Cl1 Ti1 Cl4 . . 95.06(7) ?
N1 Ti1 Cl2 . . 86.30(13) ?
Cl3 Ti1 Cl2 . . 93.35(7) ?
Cl1 Ti1 Cl2 . . 168.17(7) y
Cl4 Ti1 Cl2 . . 93.35(7) ?
N1 Ti1 P1 . . 71.36(11) y
Cl3 Ti1 P1 . . 91.32(6) ?
Cl1 Ti1 P1 . . 89.10(6) y
Cl4 Ti1 P1 . . 161.60(6) ?
Cl2 Ti1 P1 . . 80.36(6) ?
C2 C1 P1 . . 106.2(3) ?
C2 C1 H1A . . 110.5 ?
P1 C1 H1A . . 110.5 ?
C2 C1 H1B . . 110.5 ?
P1 C1 H1B . . 110.5 ?
H1A C1 H1B . . 108.7 ?
N1 C2 C5 . . 112.2(5) ?
N1 C2 C1 . . 119.5(5) ?
C5 C2 C1 . . 128.2(5) ?
N1 C3 C4 . . 104.9(4) ?
N1 C3 H3A . . 110.8 ?
C4 C3 H3A . . 110.8 ?
N1 C3 H3B . . 110.8 ?
C4 C3 H3B . . 110.8 ?
H3A C3 H3B . . 108.8 ?
C5 C4 C3 . . 108.8(5) ?
C5 C4 H4 . . 125.6 ?
C3 C4 H4 . . 125.6 ?
C4 C5 C2 . . 107.4(5) ?
C4 C5 H5 . . 126.3 ?
C2 C5 H5 . . 126.3 ?
C11 C6 C7 . . 118.8(5) ?
C11 C6 P1 . . 124.4(4) ?
C7 C6 P1 . . 116.8(4) ?
C8 C7 C6 . . 120.3(6) ?
C8 C7 H7 . . 119.9 ?
C6 C7 H7 . . 119.9 ?
C7 C8 C9 . . 120.9(6) ?
C7 C8 H8 . . 119.5 ?
C9 C8 H8 . . 119.5 ?
C10 C9 C8 . . 118.9(6) ?
C10 C9 H9 . . 120.6 ?
C8 C9 H9 . . 120.6 ?
C9 C10 C11 . . 120.6(5) ?
C9 C10 H10 . . 119.7 ?
C11 C10 H10 . . 119.7 ?
C10 C11 C6 . . 120.4(5) ?
C10 C11 H11 . . 119.8 ?
C6 C11 H11 . . 119.8 ?
C17 C12 C13 . . 119.2(5) ?
C17 C12 P1 . . 121.4(4) ?
C13 C12 P1 . . 119.3(4) ?
C12 C13 C14 . . 120.7(5) ?
C12 C13 H13 . . 119.6 ?
C14 C13 H13 . . 119.6 ?
C15 C14 C13 . . 118.7(5) ?
C15 C14 H14 . . 120.7 ?
C13 C14 H14 . . 120.7 ?
C16 C15 C14 . . 120.9(5) ?
C16 C15 H15 . . 119.6 ?
C14 C15 H15 . . 119.6 ?
C15 C16 C17 . . 120.5(6) ?
C15 C16 H16 . . 119.7 ?
C17 C16 H16 . . 119.7 ?
C12 C17 C16 . . 119.9(5) ?
C12 C17 H17 . . 120.0 ?
C16 C17 H17 . . 120.0 ?
C2 N1 C3 . . 106.7(5) ?
C2 N1 Ti1 . . 128.2(4) ?
C3 N1 Ti1 . . 125.0(3) ?
C6 P1 C12 . . 104.3(2) ?
C6 P1 C1 . . 104.4(2) ?
C12 P1 C1 . . 106.5(2) ?
C6 P1 Ti1 . . 117.80(17) ?
C12 P1 Ti1 . . 123.63(18) ?
C1 P1 Ti1 . . 97.79(16) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 N1 . 2.174(5) y
Ti1 Cl3 . 2.2293(18) y
Ti1 Cl1 . 2.2663(19) y
Ti1 Cl4 . 2.2766(17) y
Ti1 Cl2 . 2.3079(19) y
Ti1 P1 . 2.6428(17) y
C1 C2 . 1.487(7) ?
C1 P1 . 1.820(5) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 N1 . 1.303(6) y
C2 C5 . 1.439(7) y
C3 N1 . 1.464(6) y
C3 C4 . 1.471(7) y
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C5 . 1.320(7) y
C4 H4 . 0.9500 ?
C5 H5 . 0.9500 ?
C6 C11 . 1.379(7) ?
C6 C7 . 1.384(7) ?
C6 P1 . 1.813(5) ?
C7 C8 . 1.357(7) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.382(8) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.367(7) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.371(7) ?
C10 H10 . 0.9500 ?
C11 H11 . 0.9500 ?
C12 C17 . 1.378(7) ?
C12 C13 . 1.384(7) ?
C12 P1 . 1.817(5) ?
C13 C14 . 1.392(7) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.376(8) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.361(7) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.380(7) ?
C16 H16 . 0.9500 ?
C17 H17 . 0.9500 ?
