#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:31:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179332 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/29/4322983.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_4322983
loop_
_publ_author_name
'Andrea V. Firth'
'Douglas W. Stephan'
_publ_section_title
;
 Cyclopentadienyl-Bis-Aryloxide Titanium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4732
_journal_page_last               4734
_journal_paper_doi               10.1021/ic9800841
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C35 H45 O2 P Ti'
_chemical_formula_weight         576.58
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   10.8826(2)
_cell_length_b                   10.8826(2)
_cell_length_c                   49.7421(11)
_cell_measurement_temperature    293(2)
_cell_volume                     5101.76(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.1469
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            14195
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.325
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.545
_refine_ls_goodness_of_fit_obs   1.601
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4897
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.560
_refine_ls_restrained_S_obs      1.600
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_obs          0.0925
_refine_ls_shift/esd_max         0.879
_refine_ls_shift/esd_mean        0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2411
_refine_ls_wR_factor_obs         0.2294
_reflns_number_observed          4236
_reflns_number_total             4900
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9800841_3.cif
_cod_data_source_block           CpTi(OR)2PHPh
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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        5101.8(2)
_cod_database_code               4322983
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
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
Ti1 Ti 0.80186(14) 0.26442(14) 0.09251(3) 0.0460(4) Uani 1 d . .
P1 P 0.9935(3) 0.3879(3) 0.12800(6) 0.0742(8) Uani 1 d . .
H45 H 1.1300(169) 0.4591(157) 0.1074(30) 0.135(49) Uiso 1 d . .
O1 O 0.7581(5) 0.4034(5) 0.08712(12) 0.0509(13) Uani 1 d . .
O2 O 0.6652(5) 0.1377(5) 0.11450(11) 0.0484(13) Uani 1 d . .
C1 C 0.7635(15) 0.1223(14) 0.0547(3) 0.099(4) Uani 1 d . .
H1A H 0.6717(15) 0.0448(14) 0.0485(3) 0.118 Uiso 1 calc R .
C2 C 0.8328(15) 0.2599(15) 0.0449(2) 0.083(3) Uani 1 d . .
H2A H 0.7956(15) 0.2980(15) 0.0313(2) 0.100 Uiso 1 calc R .
C3 C 0.9636(16) 0.3281(14) 0.0553(3) 0.099(4) Uani 1 d . .
H3A H 1.0354(16) 0.4257(14) 0.0508(3) 0.119 Uiso 1 calc R .
C4 C 0.9884(16) 0.2405(22) 0.0712(3) 0.104(5) Uani 1 d . .
H4A H 1.0791(16) 0.2614(22) 0.0792(3) 0.125 Uiso 1 calc R .
C5 C 0.8601(23) 0.1088(16) 0.0715(3) 0.110(6) Uani 1 d . .
H5A H 0.8471(23) 0.0200(16) 0.0791(3) 0.132 Uiso 1 calc R .
C6 C 0.7336(8) 0.4961(8) 0.0720(2) 0.043(2) Uani 1 d . .
C7 C 0.6093(9) 0.4461(9) 0.0573(2) 0.053(2) Uani 1 d . .
C8 C 0.5934(11) 0.5477(11) 0.0427(2) 0.069(3) Uani 1 d . .
H8A H 0.5120(11) 0.5192(11) 0.0325(2) 0.083 Uiso 1 calc R .
C9 C 0.6991(13) 0.6930(11) 0.0433(2) 0.075(3) Uani 1 d . .
H9A H 0.6873(13) 0.7581(11) 0.0332(2) 0.090 Uiso 1 calc R .
C10 C 0.8143(9) 0.7370(9) 0.0582(2) 0.056(2) Uani 1 d . .
H10A H 0.8806(9) 0.8334(9) 0.0587(2) 0.067 Uiso 1 calc R .
C11 C 0.8392(9) 0.6420(8) 0.0732(2) 0.052(2) Uani 1 d . .
C12 C 0.4941(9) 0.2912(11) 0.0572(2) 0.073(3) Uani 1 d . .
H12A H 0.5225(9) 0.2403(11) 0.0697(2) 0.087 Uiso 1 calc R .
C13 C 0.4737(17) 0.2229(15) 0.0295(3) 0.112(5) Uani 1 d . .
H13A H 0.4001(17) 0.1253(15) 0.0304(3) 0.168 Uiso 1 calc R .
H13B H 0.5607(17) 0.2283(15) 0.0239(3) 0.168 Uiso 1 calc R .
H13C H 0.4476(17) 0.2722(15) 0.0168(3) 0.168 Uiso 1 calc R .
C14 C 0.3519(12) 0.2764(18) 0.0676(4) 0.121(5) Uani 1 d . .
H14A H 0.2794(12) 0.1782(18) 0.0674(4) 0.182 Uiso 1 calc R .
H14B H 0.3242(12) 0.3292(18) 0.0561(4) 0.182 Uiso 1 calc R .
H14C H 0.3647(12) 0.3127(18) 0.0855(4) 0.182 Uiso 1 calc R .
C15 C 0.9711(10) 0.6914(9) 0.0910(2) 0.067(2) Uani 1 d . .
H15A H 1.0039(10) 0.6229(9) 0.0891(2) 0.080 Uiso 1 calc R .
C16 C 0.9349(15) 0.6944(15) 0.1200(3) 0.098(4) Uani 1 d . .
H16A H 1.0184(15) 0.7255(15) 0.1308(3) 0.146 Uiso 1 calc R .
H16B H 0.8638(15) 0.6009(15) 0.1256(3) 0.146 Uiso 1 calc R .
H16C H 0.8993(15) 0.7586(15) 0.1223(3) 0.146 Uiso 1 calc R .
C17 C 1.0965(12) 0.8422(12) 0.0824(3) 0.097(4) Uani 1 d . .
H17A H 1.1192(12) 0.8398(12) 0.0638(3) 0.145 Uiso 1 calc R .
H17B H 1.1784(12) 0.8664(12) 0.0932(3) 0.145 Uiso 1 calc R .
H17C H 1.0681(12) 0.9119(12) 0.0848(3) 0.145 Uiso 1 calc R .
C18 C 0.5555(7) 0.0559(8) 0.1321(2) 0.043(2) Uani 1 d . .
C19 C 0.4827(9) -0.0915(9) 0.1298(2) 0.053(2) Uani 1 d . .
C20 C 0.3683(8) -0.1691(9) 0.1473(2) 0.058(2) Uani 1 d . .
H20A H 0.3178(8) -0.2675(9) 0.1460(2) 0.070 Uiso 1 calc R .
C21 C 0.3292(9) -0.1037(10) 0.1662(2) 0.063(2) Uani 1 d . .
H21A H 0.2508(9) -0.1569(10) 0.1771(2) 0.076 Uiso 1 calc R .
C22 C 0.4074(10) 0.0422(11) 0.1689(2) 0.065(2) Uani 1 d . .
H22A H 0.3839(10) 0.0858(11) 0.1824(2) 0.078 Uiso 1 calc R .
C23 C 0.5206(8) 0.1258(8) 0.1519(2) 0.053(2) Uani 1 d . .
C24 C 0.5271(11) -0.1691(9) 0.1093(2) 0.066(2) Uani 1 d . .
H24A H 0.6101(11) -0.0956(9) 0.0997(2) 0.079 Uiso 1 calc R .
C25 C 0.4163(27) -0.2482(35) 0.0887(5) 0.213(14) Uani 1 d . .
H25A H 0.3882(27) -0.1860(35) 0.0806(5) 0.320 Uiso 1 calc R .
H25B H 0.3355(27) -0.3265(35) 0.0970(5) 0.320 Uiso 1 calc R .
H25C H 0.4537(27) -0.2834(35) 0.0751(5) 0.320 Uiso 1 calc R .
C26 C 0.5699(34) -0.2618(32) 0.1214(4) 0.217(14) Uani 1 d . .
H26A H 0.6413(34) -0.2105(32) 0.1347(4) 0.325 Uiso 1 calc R .
H26B H 0.6075(34) -0.2965(32) 0.1079(4) 0.325 Uiso 1 calc R .
H26C H 0.4893(34) -0.3403(32) 0.1298(4) 0.325 Uiso 1 calc R .
C27 C 0.6047(10) 0.2902(10) 0.1551(2) 0.071(3) Uani 1 d . .
H27A H 0.6915(10) 0.3241(10) 0.1444(2) 0.085 Uiso 1 calc R .
C28 C 0.6527(20) 0.3337(18) 0.1842(4) 0.130(5) Uani 1 d . .
H28A H 0.7020(20) 0.2866(18) 0.1904(4) 0.194 Uiso 1 calc R .
H28B H 0.5713(20) 0.3072(18) 0.1954(4) 0.194 Uiso 1 calc R .
H28C H 0.7149(20) 0.4345(18) 0.1851(4) 0.194 Uiso 1 calc R .
C29 C 0.5240(19) 0.3585(16) 0.1428(4) 0.133(6) Uani 1 d . .
H29A H 0.4976(19) 0.3258(16) 0.1246(4) 0.200 Uiso 1 calc R .
H29B H 0.5837(19) 0.4599(16) 0.1428(4) 0.200 Uiso 1 calc R .
H29C H 0.4402(19) 0.3327(16) 0.1532(4) 0.200 Uiso 1 calc R .
C30 C 1.0068(9) 0.2357(9) 0.1413(2) 0.055(2) Uani 1 d . .
C31 C 0.9017(12) 0.1377(12) 0.1593(2) 0.069(2) Uani 1 d . .
H31A H 0.8241(12) 0.1476(12) 0.1638(2) 0.083 Uiso 1 calc R .
C32 C 0.9148(15) 0.0288(15) 0.1701(3) 0.098(4) Uani 1 d . .
H32A H 0.8482(15) -0.0333(15) 0.1823(3) 0.118 Uiso 1 calc R .
C33 C 1.0296(14) 0.0112(12) 0.1624(3) 0.087(3) Uani 1 d . .
H33A H 1.0358(14) -0.0658(12) 0.1688(3) 0.104 Uiso 1 calc R .
C34 C 1.1333(12) 0.1077(11) 0.1453(2) 0.074(3) Uani 1 d . .
H34A H 1.2118(12) 0.0992(11) 0.1410(2) 0.089 Uiso 1 calc R .
C35 C 1.1185(10) 0.2161(11) 0.1350(2) 0.067(2) Uani 1 d . .
H35A H 1.1872(10) 0.2794(11) 0.1232(2) 0.080 Uiso 1 calc R .
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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O1 105.4(2) . . ?
O2 Ti1 C5 97.9(4) . . ?
O1 Ti1 C5 144.8(4) . . ?
O2 Ti1 C1 100.1(4) . . ?
O1 Ti1 C1 113.4(5) . . ?
C5 Ti1 C1 35.0(6) . . ?
O2 Ti1 C2 130.8(4) . . ?
O1 Ti1 C2 88.2(3) . . ?
C5 Ti1 C2 56.6(4) . . ?
C1 Ti1 C2 34.0(5) . . ?
O2 Ti1 C3 153.0(4) . . ?
O1 Ti1 C3 96.0(4) . . ?
C5 Ti1 C3 55.8(4) . . ?
C1 Ti1 C3 55.6(5) . . ?
C2 Ti1 C3 32.4(5) . . ?
O2 Ti1 C4 126.8(5) . . ?
O1 Ti1 C4 127.5(5) . . ?
C5 Ti1 C4 34.6(6) . . ?
C1 Ti1 C4 57.1(5) . . ?
C2 Ti1 C4 55.3(4) . . ?
C3 Ti1 C4 32.9(5) . . ?
O2 Ti1 P1 97.3(2) . . ?
O1 Ti1 P1 98.6(2) . . ?
C5 Ti1 P1 104.3(6) . . ?
C1 Ti1 P1 137.4(4) . . ?
C2 Ti1 P1 127.6(4) . . ?
C3 Ti1 P1 95.3(4) . . ?
C4 Ti1 P1 81.4(4) . . ?
C30 P1 Ti1 100.7(3) . . ?
C6 O1 Ti1 155.6(5) . . ?
C18 O2 Ti1 171.6(5) . . ?
C2 C1 C5 106.8(12) . . ?
C2 C1 Ti1 75.3(7) . . ?
C5 C1 Ti1 72.3(7) . . ?
C3 C2 C1 108.5(12) . . ?
C3 C2 Ti1 74.2(7) . . ?
C1 C2 Ti1 70.7(7) . . ?
C2 C3 C4 111.3(13) . . ?
C2 C3 Ti1 73.4(7) . . ?
C4 C3 Ti1 74.1(7) . . ?
C3 C4 C5 105.8(12) . . ?
C3 C4 Ti1 73.0(7) . . ?
C5 C4 Ti1 69.4(6) . . ?
C1 C5 C4 107.5(10) . . ?
C1 C5 Ti1 72.6(6) . . ?
C4 C5 Ti1 75.9(7) . . ?
O1 C6 C7 120.3(7) . . ?
O1 C6 C11 116.7(7) . . ?
C7 C6 C11 123.0(7) . . ?
C6 C7 C8 116.3(8) . . ?
C6 C7 C12 122.6(7) . . ?
C8 C7 C12 121.0(8) . . ?
C7 C8 C9 121.2(9) . . ?
C10 C9 C8 120.7(8) . . ?
C9 C10 C11 121.7(8) . . ?
C10 C11 C6 117.1(8) . . ?
C10 C11 C15 122.5(7) . . ?
C6 C11 C15 120.4(7) . . ?
C7 C12 C13 112.5(10) . . ?
C7 C12 C14 109.8(10) . . ?
C13 C12 C14 110.6(11) . . ?
C16 C15 C11 110.7(9) . . ?
C16 C15 C17 109.8(9) . . ?
C11 C15 C17 112.2(9) . . ?
O2 C18 C19 119.9(7) . . ?
O2 C18 C23 118.2(7) . . ?
C19 C18 C23 121.9(7) . . ?
C18 C19 C20 117.6(7) . . ?
C18 C19 C24 122.0(7) . . ?
C20 C19 C24 120.4(8) . . ?
C21 C20 C19 121.7(8) . . ?
C20 C21 C22 119.3(8) . . ?
C21 C22 C23 121.8(9) . . ?
C22 C23 C18 117.5(8) . . ?
C22 C23 C27 120.5(8) . . ?
C18 C23 C27 122.1(8) . . ?
C26 C24 C25 109.6(18) . . ?
C26 C24 C19 114.0(10) . . ?
C25 C24 C19 112.7(11) . . ?
C28 C27 C29 114.7(12) . . ?
C28 C27 C23 111.5(10) . . ?
C29 C27 C23 111.4(9) . . ?
C35 C30 C31 118.1(8) . . ?
C35 C30 P1 121.8(7) . . ?
C31 C30 P1 120.1(7) . . ?
C32 C31 C30 120.0(10) . . ?
C31 C32 C33 119.7(11) . . ?
C34 C33 C32 120.4(10) . . ?
C35 C34 C33 118.9(10) . . ?
C34 C35 C30 122.9(10) . . ?
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
Ti1 O2 1.805(5) . ?
Ti1 O1 1.819(5) . ?
Ti1 C5 2.333(9) . ?
Ti1 C1 2.336(12) . ?
Ti1 C2 2.394(11) . ?
Ti1 C3 2.403(12) . ?
Ti1 C4 2.417(11) . ?
Ti1 P1 2.543(3) . ?
P1 C30 1.855(8) . ?
O1 C6 1.385(9) . ?
O2 C18 1.386(9) . ?
C1 C2 1.39(2) . ?
C1 C5 1.41(2) . ?
C2 C3 1.34(2) . ?
C3 C4 1.36(2) . ?
C4 C5 1.41(2) . ?
C6 C7 1.389(12) . ?
C6 C11 1.421(11) . ?
C7 C8 1.403(13) . ?
C7 C12 1.516(13) . ?
C8 C9 1.42(2) . ?
C9 C10 1.321(15) . ?
C10 C11 1.407(12) . ?
C11 C15 1.538(14) . ?
C12 C13 1.53(2) . ?
C12 C14 1.56(2) . ?
C15 C16 1.50(2) . ?
C15 C17 1.581(14) . ?
C18 C19 1.394(12) . ?
C18 C23 1.407(12) . ?
C19 C20 1.404(12) . ?
C19 C24 1.546(13) . ?
C20 C21 1.370(14) . ?
C21 C22 1.383(14) . ?
C22 C23 1.393(13) . ?
C23 C27 1.558(12) . ?
C24 C26 1.44(2) . ?
C24 C25 1.49(2) . ?
C27 C28 1.53(2) . ?
C27 C29 1.53(2) . ?
C30 C35 1.371(13) . ?
C30 C31 1.425(14) . ?
C31 C32 1.37(2) . ?
C32 C33 1.41(2) . ?
C33 C34 1.38(2) . ?
C34 C35 1.368(15) . ?
