#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/17/7011762.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7011762
loop_
_publ_author_name
'Blackman, Christopher S.'
'Carmalt, Claire J.'
'Parkin, Ivan P.'
'Apostolico, Leonardo'
'Molloy, Kieran C.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Single-source CVD routes to titanium phosphide
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2702
_journal_paper_doi               10.1039/b203613b
_journal_year                    2002
_chemical_formula_sum            'C26 H24 Cl4 P2 Ti'
_chemical_formula_weight         588.09
_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                 111.254(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2287(15)
_cell_length_b                   14.560(2)
_cell_length_c                   16.047(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      22.43
_cell_measurement_theta_min      10.77
_cell_volume                     2662.8(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3479
_diffrn_reflns_theta_max         57.20
_diffrn_reflns_theta_min         3.88
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.657
_exptl_absorpt_correction_T_max  0.7627
_exptl_absorpt_correction_T_min  0.2124
_exptl_absorpt_correction_type   'Lamina [0 1 0]'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.0004(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_obs          0.0550
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0913P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1594
_refine_ls_wR_factor_obs         0.1306
_reflns_number_observed          2429
_reflns_number_total             3294
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b203613b.txt
_cod_data_source_block           IP0104
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2662.8(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C26 H24 P2 Cl4 Ti'
_cod_database_code               7011762
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti Ti 0.69152(8) 0.64753(7) 0.11808(7) 0.0246(3) Uani 1 d . .
Cl1 Cl 0.65776(12) 0.50615(10) 0.16255(11) 0.0367(4) Uani 1 d . .
Cl2 Cl 0.72537(12) 0.80254(10) 0.11691(11) 0.0357(4) Uani 1 d . .
Cl3 Cl 0.86101(12) 0.61173(12) 0.09878(11) 0.0386(4) Uani 1 d . .
Cl4 Cl 0.54635(13) 0.64420(12) -0.01705(10) 0.0404(4) Uani 1 d . .
P1 P 0.53398(11) 0.71399(10) 0.18092(10) 0.0264(4) Uani 1 d . .
P2 P 0.80921(11) 0.65862(10) 0.29195(9) 0.0246(4) Uani 1 d . .
C1 C 0.6151(5) 0.7497(5) 0.2972(4) 0.0322(13) Uani 1 d . .
H1A H 0.6593(5) 0.8069(5) 0.2981(4) 0.039 Uiso 1 calc R .
H1B H 0.5599(5) 0.7613(5) 0.3283(4) 0.039 Uiso 1 calc R .
C2 C 0.6993(5) 0.6729(4) 0.3435(4) 0.0297(13) Uani 1 d . .
H2A H 0.6552(5) 0.6148(4) 0.3386(4) 0.036 Uiso 1 calc R .
H2B H 0.7385(5) 0.6876(4) 0.4077(4) 0.036 Uiso 1 calc R .
C3 C 0.5038(3) 0.9035(3) 0.1445(2) 0.041(2) Uani 1 d G .
H3A H 0.5701(3) 0.9127(3) 0.1977(2) 0.049 Uiso 1 calc R .
C4 C 0.4519(4) 0.9779(2) 0.0903(3) 0.048(2) Uani 1 d G .
H4A H 0.4828(5) 1.0379(2) 0.1065(4) 0.058 Uiso 1 calc R .
C5 C 0.3548(4) 0.9645(3) 0.0125(3) 0.053(2) Uani 1 d G .
H5A H 0.3194(5) 1.0153(3) -0.0246(4) 0.063 Uiso 1 calc R .
C6 C 0.3096(3) 0.8767(3) -0.0112(2) 0.051(2) Uani 1 d G .
H6A H 0.2433(4) 0.8675(4) -0.0643(3) 0.062 Uiso 1 calc R .
C7 C 0.3615(3) 0.8023(2) 0.0430(3) 0.0386(15) Uani 1 d G .
H7A H 0.3306(5) 0.7423(3) 0.0269(4) 0.046 Uiso 1 calc R .
C8 C 0.4586(3) 0.8157(2) 0.1209(2) 0.0349(14) Uani 1 d G .
C9 C 0.3785(3) 0.5643(3) 0.1307(3) 0.0339(14) Uani 1 d G .
H9A H 0.4215(3) 0.5462(3) 0.0946(3) 0.041 Uiso 1 calc R .
C10 C 0.2816(3) 0.5136(3) 0.1293(3) 0.042(2) Uani 1 d G .
H10A H 0.2583(5) 0.4608(3) 0.0923(4) 0.051 Uiso 1 calc R .
C11 C 0.2187(3) 0.5402(3) 0.1821(3) 0.051(2) Uani 1 d G .
H11A H 0.1524(4) 0.5055(5) 0.1812(5) 0.061 Uiso 1 calc R .
C12 C 0.2528(4) 0.6174(4) 0.2363(3) 0.070(3) Uani 1 d G .
H12A H 0.2098(5) 0.6356(5) 0.2724(5) 0.084 Uiso 1 calc R .
C13 C 0.3497(4) 0.6681(3) 0.2377(3) 0.052(2) Uani 1 d G .
H13A H 0.3730(5) 0.7209(4) 0.2747(4) 0.063 Uiso 1 calc R .
C14 C 0.4126(3) 0.6416(3) 0.1849(3) 0.0325(14) Uani 1 d G .
C15 C 0.8504(3) 0.4891(3) 0.3831(3) 0.042(2) Uani 1 d G .
H15A H 0.7780(3) 0.4982(3) 0.3913(3) 0.051 Uiso 1 calc R .
C16 C 0.9149(3) 0.4095(3) 0.4148(3) 0.045(2) Uani 1 d G .
H16A H 0.8866(5) 0.3643(3) 0.4446(4) 0.054 Uiso 1 calc R .
C17 C 1.0208(3) 0.3961(2) 0.4028(3) 0.039(2) Uani 1 d G .
H17A H 1.0648(4) 0.3417(3) 0.4244(4) 0.047 Uiso 1 calc R .
C18 C 1.0621(3) 0.4622(3) 0.3591(3) 0.040(2) Uani 1 d G .
H18A H 1.1345(4) 0.4531(4) 0.3509(5) 0.048 Uiso 1 calc R .
C19 C 0.9977(3) 0.5418(2) 0.3275(3) 0.0352(14) Uani 1 d G .
H19A H 1.0259(4) 0.5870(3) 0.2976(4) 0.042 Uiso 1 calc R .
C20 C 0.8918(3) 0.5552(2) 0.3395(3) 0.0278(12) Uani 1 d G .
C21 C 0.9379(3) 0.7892(3) 0.4186(2) 0.0380(15) Uani 1 d G .
H21A H 0.8876(3) 0.7750(3) 0.4501(2) 0.046 Uiso 1 calc R .
C22 C 1.0314(4) 0.8493(3) 0.4556(2) 0.048(2) Uani 1 d G .
H22A H 1.0449(5) 0.8761(5) 0.5125(3) 0.057 Uiso 1 calc R .
C23 C 1.1050(3) 0.8701(3) 0.4095(3) 0.044(2) Uani 1 d G .
H23A H 1.1689(4) 0.9111(4) 0.4349(4) 0.053 Uiso 1 calc R .
C24 C 1.0852(3) 0.8308(3) 0.3264(3) 0.043(2) Uani 1 d G .
H24A H 1.1355(4) 0.8450(5) 0.2949(3) 0.051 Uiso 1 calc R .
C25 C 0.9918(3) 0.7707(3) 0.2893(2) 0.0362(14) Uani 1 d G .
H25A H 0.9782(5) 0.7438(4) 0.2325(3) 0.043 Uiso 1 calc R .
C26 C 0.9181(3) 0.7499(3) 0.3354(2) 0.0260(12) Uani 1 d G .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl4 Ti Cl3 107.74(7) . . ?
Cl4 Ti Cl1 96.53(7) . . ?
Cl3 Ti Cl1 96.57(7) . . ?
Cl4 Ti Cl2 95.44(7) . . ?
Cl3 Ti Cl2 92.78(7) . . ?
Cl1 Ti Cl2 161.79(8) . . ?
Cl4 Ti P2 163.12(6) . . ?
Cl3 Ti P2 89.05(6) . . ?
Cl1 Ti P2 79.31(6) . . ?
Cl2 Ti P2 85.28(6) . . ?
Cl4 Ti P1 86.92(6) . . ?
Cl3 Ti P1 163.79(7) . . ?
Cl1 Ti P1 88.36(6) . . ?
Cl2 Ti P1 78.63(6) . . ?
P2 Ti P1 76.66(5) . . ?
C8 P1 C14 102.9(2) . . ?
C8 P1 C1 106.8(3) . . ?
C14 P1 C1 105.8(2) . . ?
C8 P1 Ti 113.08(15) . . ?
C14 P1 Ti 120.58(14) . . ?
C1 P1 Ti 106.7(2) . . ?
C20 P2 C2 107.0(2) . . ?
C20 P2 C26 103.0(2) . . ?
C2 P2 C26 107.3(2) . . ?
C20 P2 Ti 113.54(15) . . ?
C2 P2 Ti 106.1(2) . . ?
C26 P2 Ti 119.30(13) . . ?
C2 C1 P1 108.0(4) . . ?
C1 C2 P2 109.9(4) . . ?
C4 C3 C8 120.0 . . ?
C3 C4 C5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C8 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 P1 117.7(2) . . ?
C3 C8 P1 121.8(2) . . ?
C10 C9 C14 120.0 . . ?
C11 C10 C9 120.0 . . ?
C12 C11 C10 120.0 . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 P1 119.6(2) . . ?
C9 C14 P1 120.3(2) . . ?
C16 C15 C20 120.0 . . ?
C15 C16 C17 120.0 . . ?
C18 C17 C16 120.0 . . ?
C19 C18 C17 120.0 . . ?
C18 C19 C20 120.0 . . ?
C19 C20 C15 120.0 . . ?
C19 C20 P2 117.5(2) . . ?
C15 C20 P2 122.4(2) . . ?
C22 C21 C26 120.0 . . ?
C23 C22 C21 120.0 . . ?
C22 C23 C24 120.0 . . ?
C25 C24 C23 120.0 . . ?
C26 C25 C24 120.0 . . ?
C25 C26 C21 120.0 . . ?
C25 C26 P2 118.5(2) . . ?
C21 C26 P2 120.9(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti Cl4 2.251(2) . ?
Ti Cl3 2.265(2) . ?
Ti Cl1 2.265(2) . ?
Ti Cl2 2.296(2) . ?
Ti P2 2.640(2) . ?
Ti P1 2.660(2) . ?
P1 C8 1.824(3) . ?
P1 C14 1.840(3) . ?
P1 C1 1.842(6) . ?
P2 C20 1.819(3) . ?
P2 C2 1.828(6) . ?
P2 C26 1.831(3) . ?
C1 C2 1.519(9) . ?
C3 C4 1.39 . ?
C3 C8 1.39 . ?
C4 C5 1.39 . ?
C5 C6 1.39 . ?
C6 C7 1.39 . ?
C7 C8 1.39 . ?
C9 C10 1.39 . ?
C9 C14 1.39 . ?
C10 C11 1.39 . ?
C11 C12 1.39 . ?
C12 C13 1.39 . ?
C13 C14 1.39 . ?
C15 C16 1.39 . ?
C15 C20 1.39 . ?
C16 C17 1.39 . ?
C17 C18 1.39 . ?
C18 C19 1.39 . ?
C19 C20 1.39 . ?
C21 C22 1.39 . ?
C21 C26 1.39 . ?
C22 C23 1.39 . ?
C23 C24 1.39 . ?
C24 C25 1.39 . ?
C25 C26 1.39 . ?
