#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:22:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179840 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/36/7013604.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_7013604
loop_
_publ_author_name
'Luke E. Turner'
'Matthew G. Thorn'
'R. D. Swartz II'
'Robert W. Chesnut'
'Phillip E. Fanwick'
'Ian P. Rothwell'
_publ_section_title
;
 Synthesis, stereochemistry, bonding and fluxionality of
 2-(inden-3-yl)phenols and their cyclopentadienyl titanium derivatives
;
_journal_issue                   24
_journal_name_full               'Dalton Trans.'
_journal_page_first              4580
_journal_page_last               4589
_journal_paper_doi               10.1039/b310415j
_journal_year                    2003
_chemical_formula_sum            'C31 H35 Cl2 O Ti'
_chemical_formula_weight         542.43
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             29-01-99
_audit_creation_method           from_MolEN_and_SHELXL
_audit_update_record             ' ?'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.5167(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2422(4)
_cell_length_b                   12.6093(4)
_cell_length_c                   18.9505(6)
_cell_measurement_reflns_used    24792
_cell_measurement_temperature    203
_cell_measurement_theta_max      30
_cell_measurement_theta_min      4
_cell_volume                     2855.78(16)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
ORTEP (Johnson, 1976)
Xtal_GX (Hall, 1995)
PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    PATTY_(DIRDIF92,_Beurskins,_1992)
_diffrn_ambient_temperature      203
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24792
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.9389
_exptl_absorpt_correction_T_min  0.6512
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5004
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.045
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0593P)²+1.4369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.111
_reflns_number_gt                4070
_reflns_number_total             5004
_reflns_threshold_expression     >2.0σ(I)
_cod_data_source_file            b310415j.txt
_cod_data_source_block           MT38H
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc' 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 
;
_cod_original_cell_volume        2855.8(3)
_cod_original_sg_symbol_H-M      'p 1 21/n 1'
_cod_database_code               7013604
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_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_calc_flag
Ti 0.07043(4) 0.03959(3) 0.36702(2) 0.03313(14) Uani ?
Cl(1) -0.09534(6) 0.05894(8) 0.39953(4) 0.0658(3) Uani ?
Cl(2) 0.09958(8) -0.13546(5) 0.38727(4) 0.0616(3) Uani ?
O(1) 0.03549(13) 0.05251(12) 0.27095(8) 0.0341(4) Uani ?
C(1) 0.1384(3) 0.1502(3) 0.46750(15) 0.0598(9) Uani ?
C(2) 0.2150(2) 0.0691(2) 0.46980(14) 0.0507(8) Uani ?
C(3) 0.2605(2) 0.0768(2) 0.40846(14) 0.0436(8) Uani ?
C(4) 0.2125(2) 0.1638(2) 0.36784(14) 0.0451(8) Uani ?
C(5) 0.1356(3) 0.2090(2) 0.40352(18) 0.0576(9) Uani ?
C(11) 0.04170(18) 0.08748(18) 0.20329(11) 0.0296(6) Uani ?
C(12) 0.14035(18) 0.07012(17) 0.17917(11) 0.0284(6) Uani ?
C(13) 0.14885(18) 0.11011(17) 0.11182(11) 0.0301(6) Uani ?
C(14) 0.06109(18) 0.16359(18) 0.06775(11) 0.0316(6) Uani ?
C(15) -0.03692(19) 0.1750(2) 0.09303(12) 0.0367(7) Uani ?
C(16) -0.05159(18) 0.1379(2) 0.15940(12) 0.0353(6) Uani ?
C(121) 0.23509(18) 0.00728(18) 0.22168(11) 0.0298(6) Uani ?
C(122) 0.2308(2) -0.09235(19) 0.24552(13) 0.0400(7) Uani ?
C(123) 0.3428(2) -0.1285(2) 0.28757(14) 0.0467(8) Uani ?
C(124) 0.4152(2) -0.03362(19) 0.28501(12) 0.0372(7) Uani ?
C(125) 0.5270(2) -0.0148(2) 0.31642(13) 0.0470(8) Uani ?
C(126) 0.5739(2) 0.0816(3) 0.30534(14) 0.0503(8) Uani ?
C(127) 0.5109(2) 0.1594(2) 0.26343(14) 0.0472(8) Uani ?
C(128) 0.39838(19) 0.14288(19) 0.23242(12) 0.0354(6) Uani ?
C(129) 0.35045(18) 0.04600(17) 0.24401(11) 0.0300(6) Uani ?
C(141) 0.0660(2) 0.2085(2) -0.00682(12) 0.0382(7) Uani ?
C(142) 0.1767(3) 0.1866(3) -0.02683(16) 0.0709(12) Uani ?
C(143) -0.0290(3) 0.1628(3) -0.06383(14) 0.0702(12) Uani ?
C(144) 0.0514(3) 0.3299(2) -0.00491(16) 0.0632(10) Uani ?
C(161) -0.1644(2) 0.1508(2) 0.18138(13) 0.0462(8) Uani ?
C(162) -0.1523(2) 0.2263(2) 0.24568(16) 0.0545(9) Uani ?
C(163) -0.2067(2) 0.0409(3) 0.19863(16) 0.0558(9) Uani ?
C(164) -0.2541(2) 0.1989(3) 0.12026(17) 0.0743(11) Uani ?
C(901) 0.4539(3) 0.0912(4) -0.0327(3) 0.0953(19) Uani ?
C(902) 0.4626(3) 0.0751(4) 0.0402(3) 0.0883(16) Uani ?
C(903) 0.5072(3) -0.0143(4) 0.0728(3) 0.0887(14) Uani ?
H(1) 0.0962 0.1637 0.5018 0.0780 Uiso calc
H(2) 0.2331 0.0182 0.5059 0.0660 Uiso calc
H(3) 0.3138 0.0316 0.3967 0.0570 Uiso calc
H(4) 0.2289 0.1874 0.3248 0.0590 Uiso calc
H(5) 0.0905 0.2674 0.3880 0.0750 Uiso calc
H(13) 0.2151 0.1006 0.0962 0.0390 Uiso calc
H(15) -0.0967 0.2099 0.0635 0.0480 Uiso calc
H(122) 0.1665 -0.1338 0.2371 0.0520 Uiso calc
H(125) 0.5697 -0.0666 0.3446 0.0610 Uiso calc
H(126) 0.6487 0.0945 0.3263 0.0650 Uiso calc
H(127) 0.5443 0.2235 0.2559 0.0610 Uiso calc
H(128) 0.3561 0.1953 0.2046 0.0460 Uiso calc
H(12A) 0.3399 -0.1463 0.3369 0.0610 Uiso calc
H(12B) 0.3694 -0.1895 0.2650 0.0610 Uiso calc
H(14A) 0.2361 0.2174 0.0088 0.0920 Uiso calc
H(14B) 0.1766 0.2171 -0.0733 0.0920 Uiso calc
H(14C) 0.1879 0.1114 -0.0287 0.0920 Uiso calc
H(14D) -0.0198 0.0874 -0.0666 0.0910 Uiso calc
H(14E) -0.0282 0.1941 -0.1099 0.0910 Uiso calc
H(14F) -0.0991 0.1780 -0.0511 0.0910 Uiso calc
H(14G) -0.0184 0.3463 0.0078 0.0820 Uiso calc
H(14H) 0.0518 0.3590 -0.0517 0.0820 Uiso calc
H(14I) 0.1118 0.3600 0.0303 0.0820 Uiso calc
H(16A) -0.0969 0.1992 0.2854 0.0710 Uiso calc
H(16B) -0.2227 0.2324 0.2598 0.0710 Uiso calc
H(16C) -0.1295 0.2949 0.2322 0.0710 Uiso calc
H(16D) -0.2137 -0.0042 0.1571 0.0730 Uiso calc
H(16E) -0.2783 0.0481 0.2110 0.0730 Uiso calc
H(16F) -0.1545 0.0101 0.2385 0.0730 Uiso calc
H(16G) -0.2307 0.2682 0.1085 0.0970 Uiso calc
H(16H) -0.3236 0.2045 0.1358 0.0970 Uiso calc
H(16I) -0.2642 0.1542 0.0784 0.0970 Uiso calc
H(901) 0.4222 0.1532 -0.0546 0.1240 Uiso calc
H(902) 0.4370 0.1272 0.0674 0.1150 Uiso calc
H(903) 0.5119 -0.0242 0.1220 0.1150 Uiso calc
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(1) Ti Cl(2) 104.89(6) ?
O(1) Ti Cl(1) 103.74(6) ?
Cl(2) Ti Cl(1) 100.24(4) ?
O(1) Ti C(5) 102.12(10) ?
Cl(2) Ti C(5) 144.54(8) ?
Cl(1) Ti C(5) 95.17(8) ?
O(1) Ti C(3) 109.00(8) ?
Cl(2) Ti C(3) 91.73(7) ?
Cl(1) Ti C(3) 140.80(7) ?
C(5) Ti C(3) 57.60(10) ?
O(1) Ti C(4) 87.66(8) ?
Cl(2) Ti C(4) 124.35(7) ?
Cl(1) Ti C(4) 129.58(7) ?
C(5) Ti C(4) 34.74(10) ?
C(3) Ti C(4) 34.70(9) ?
O(1) Ti C(2) 142.97(9) ?
Cl(2) Ti C(2) 87.21(8) ?
Cl(1) Ti C(2) 108.38(7) ?
C(5) Ti C(2) 57.55(11) ?
C(3) Ti C(2) 34.60(9) ?
C(4) Ti C(2) 57.66(10) ?
O(1) Ti C(1) 137.15(10) ?
Cl(2) Ti C(1) 115.19(9) ?
Cl(1) Ti C(1) 84.07(8) ?
C(5) Ti C(1) 35.09(11) ?
C(3) Ti C(1) 57.25(10) ?
C(4) Ti C(1) 57.82(10) ?
C(2) Ti C(1) 34.03(10) ?
C(11) O(1) Ti 158.73(14) ?
C(2) C(1) C(5) 107.7(3) ?
C(2) C(1) Ti 72.93(15) ?
C(5) C(1) Ti 71.31(15) ?
C(1) C(2) C(3) 108.2(3) ?
C(1) C(2) Ti 73.04(15) ?
C(3) C(2) Ti 71.77(15) ?
C(4) C(3) C(2) 108.6(2) ?
C(4) C(3) Ti 72.73(15) ?
C(2) C(3) Ti 73.63(15) ?
C(3) C(4) C(5) 107.5(3) ?
C(3) C(4) Ti 72.57(15) ?
C(5) C(4) Ti 72.37(16) ?
C(4) C(5) C(1) 108.0(3) ?
C(4) C(5) Ti 72.89(15) ?
C(1) C(5) Ti 73.59(16) ?
O(1) C(11) C(12) 118.78(19) ?
O(1) C(11) C(16) 119.59(19) ?
C(12) C(11) C(16) 121.63(19) ?
C(11) C(12) C(13) 118.9(2) ?
C(11) C(12) C(121) 122.22(19) ?
C(13) C(12) C(121) 118.9(2) ?
C(14) C(13) C(12) 121.7(2) ?
C(13) C(14) C(15) 117.2(2) ?
C(13) C(14) C(141) 123.7(2) ?
C(15) C(14) C(141) 119.1(2) ?
C(16) C(15) C(14) 124.5(2) ?
C(15) C(16) C(11) 116.0(2) ?
C(15) C(16) C(161) 120.7(2) ?
C(11) C(16) C(161) 123.3(2) ?
C(122) C(121) C(129) 108.7(2) ?
C(122) C(121) C(12) 126.8(2) ?
C(129) C(121) C(12) 124.55(19) ?
C(121) C(122) C(123) 111.5(2) ?
C(124) C(123) C(122) 102.7(2) ?
C(125) C(124) C(129) 120.0(2) ?
C(125) C(124) C(123) 131.1(2) ?
C(129) C(124) C(123) 108.8(2) ?
C(126) C(125) C(124) 119.3(2) ?
C(125) C(126) C(127) 120.9(2) ?
C(128) C(127) C(126) 120.8(3) ?
C(127) C(128) C(129) 118.5(2) ?
C(128) C(129) C(124) 120.5(2) ?
C(128) C(129) C(121) 131.2(2) ?
C(124) C(129) C(121) 108.3(2) ?
C(142) C(141) C(143) 110.0(3) ?
C(142) C(141) C(14) 112.3(2) ?
C(143) C(141) C(14) 109.8(2) ?
C(142) C(141) C(144) 107.6(2) ?
C(143) C(141) C(144) 108.6(2) ?
C(14) C(141) C(144) 108.5(2) ?
C(162) C(161) C(16) 110.1(2) ?
C(162) C(161) C(164) 106.5(3) ?
C(16) C(161) C(164) 112.0(2) ?
C(162) C(161) C(163) 111.8(2) ?
C(16) C(161) C(163) 109.0(2) ?
C(164) C(161) C(163) 107.3(2) ?
C(903) C(901) C(902) 119.2(4) ?
C(903) C(902) C(901) 121.4(4) ?
C(902) C(903) C(901) 119.4(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ti O(1) 1.7851(15) ?
Ti Cl(2) 2.2554(8) ?
Ti Cl(1) 2.2581(8) ?
Ti C(5) 2.332(3) ?
Ti C(3) 2.336(3) ?
Ti C(4) 2.338(3) ?
Ti C(2) 2.360(3) ?
Ti C(1) 2.361(3) ?
O(1) C(11) 1.374(2) ?
C(1) C(2) 1.382(4) ?
C(1) C(5) 1.415(4) ?
C(2) C(3) 1.397(4) ?
C(3) C(4) 1.394(4) ?
C(4) C(5) 1.394(4) ?
C(11) C(12) 1.398(3) ?
C(11) C(16) 1.410(3) ?
C(12) C(13) 1.397(3) ?
C(12) C(121) 1.489(3) ?
C(13) C(14) 1.385(3) ?
C(14) C(15) 1.392(3) ?
C(14) C(141) 1.535(3) ?
C(15) C(16) 1.390(3) ?
C(16) C(161) 1.536(3) ?
C(121) C(122) 1.340(3) ?
C(121) C(129) 1.467(3) ?
C(122) C(123) 1.500(4) ?
C(123) C(124) 1.496(4) ?
C(124) C(125) 1.389(4) ?
C(124) C(129) 1.404(3) ?
C(125) C(126) 1.380(4) ?
C(126) C(127) 1.386(4) ?
C(127) C(128) 1.392(3) ?
C(128) C(129) 1.393(3) ?
C(141) C(142) 1.510(4) ?
C(141) C(143) 1.519(3) ?
C(141) C(144) 1.543(4) ?
C(161) C(162) 1.528(4) ?
C(161) C(164) 1.538(4) ?
C(161) C(163) 1.539(4) ?
C(901) C(903) 1.379(6) ?
C(901) C(902) 1.377(6) ?
C(902) C(903) 1.344(6) ?
C(903) C(901) 1.379(6) ?
