# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1063831'
_audit_update_record             
;
2015-05-07 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;
#================================================

_audit_creation_date             11-09-28
_audit_creation_method           CRYSTALS_ver_14.11

_oxford_structure_analysis_title 102fmc11
_chemical_name_systematic        Pn*TiMe2
_chemical_melting_point          'not measured'

_cell_length_a                   9.5686(2)
_cell_length_b                   10.0906(2)
_cell_length_c                   15.5541(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.1528(8)
_cell_angle_gamma                90
_cell_volume                     1490.11(5)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C16 H24 Ti1 
# Dc =      1.18 Fooo =    568.00 Mu =      5.53 M =    264.27
# Found Formula = C16 H24 Ti1 
# Dc =      1.18 FOOO =    568.00 Mu =      5.53 M =    264.27

_chemical_formula_sum            'C16 H24 Ti1'
_chemical_formula_moiety         'C16 H24 Ti1'
_chemical_compound_source        SYN
_chemical_formula_weight         264.27


_cell_measurement_reflns_used    3501
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             568
_exptl_absorpt_coefficient_mu    0.553

# Sheldrick geometric approximatio 0.90 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.95
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        'not measured'

_diffrn_ambient_temperature      150
_diffrn_reflns_number            15894
_reflns_number_total             3388
_diffrn_reflns_av_R_equivalents  0.018
# Number of reflections without Friedels Law is 6022 
# Number of reflections with Friedels Law is 3388 
# Theoretical number of reflections is about 3425 


_diffrn_reflns_theta_min         5.149
_diffrn_reflns_theta_max         27.504
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        26.679
_diffrn_measured_fraction_theta_full 0.992


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              20

_oxford_diffrn_Wilson_B_factor   2.07
_oxford_diffrn_Wilson_scale      1.69

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.38
_refine_diff_density_max         0.32


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3388
_refine_ls_number_restraints     0
_refine_ls_number_parameters     226
_oxford_refine_ls_R_factor_ref   0.0450
_refine_ls_wR_factor_ref         0.1053
_refine_ls_goodness_of_fit_ref   0.9201
_refine_ls_shift/su_max          0.0007558
_refine_ls_shift/su_mean         0.0000171


# The values computed from all data 
_oxford_reflns_number_all        3388
_refine_ls_R_factor_all          0.0450
_refine_ls_wR_factor_all         0.1053

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2989
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_gt          0.0986

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 31.7 48.7 24.7 6.68 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.36228(16) 0.20107(16) 0.39672(10) 0.0248 1.0000 Uani . . . . . .
C2 C 0.34187(16) 0.25856(16) 0.31323(10) 0.0256 1.0000 Uani . . . . . .
C3 C 0.20067(17) 0.24069(17) 0.27437(10) 0.0268 1.0000 Uani . . . . . .
C4 C 0.12898(17) 0.16657(15) 0.33463(10) 0.0242 1.0000 Uani . . . . . .
C5 C -0.00703(16) 0.18885(17) 0.36320(11) 0.0266 1.0000 Uani . . . . . .
C6 C 0.01061(16) 0.17861(16) 0.45479(10) 0.0247 1.0000 Uani . . . . . .
C7 C 0.15413(17) 0.15443(14) 0.48656(10) 0.0236 1.0000 Uani . . . . . .
C8 C 0.22962(16) 0.14250(14) 0.41217(10) 0.0222 1.0000 Uani . . . . . .
C9 C 0.49954(18) 0.1940(2) 0.45420(12) 0.0341 1.0000 Uani . . . . . .
C10 C 0.45354(19) 0.3330(2) 0.27323(13) 0.0338 1.0000 Uani . . . . . .
C11 C 0.1430(2) 0.2834(2) 0.18441(12) 0.0389 1.0000 Uani . . . . . .
C12 C -0.14478(19) 0.2113(2) 0.30733(13) 0.0384 1.0000 Uani . . . . . .
C13 C -0.10378(19) 0.19641(19) 0.51178(12) 0.0312 1.0000 Uani . . . . . .
C14 C 0.2099(2) 0.1352(2) 0.58048(11) 0.0331 1.0000 Uani . . . . . .
C15 C 0.2887(2) 0.4466(2) 0.51142(14) 0.0385 1.0000 Uani . . . . . .
C16 C 0.0475(2) 0.4963(2) 0.33599(15) 0.0396 1.0000 Uani . . . . . .
Ti1 Ti 0.17147(3) 0.34586(3) 0.404917(18) 0.0236 1.0000 Uani . . . . . .
H93 H 0.483(3) 0.167(3) 0.508(2) 0.0509 1.0000 Uiso . . . . . .
H92 H 0.547(3) 0.277(3) 0.4544(17) 0.0519 1.0000 Uiso . . . . . .
H91 H 0.554(3) 0.122(3) 0.4302(17) 0.0513 1.0000 Uiso . . . . . .
H103 H 0.413(3) 0.393(3) 0.2320(17) 0.0510 1.0000 Uiso . . . . . .
H102 H 0.514(3) 0.382(3) 0.3141(18) 0.0512 1.0000 Uiso . . . . . .
H101 H 0.512(3) 0.275(3) 0.2481(17) 0.0508 1.0000 Uiso . . . . . .
H113 H 0.043(3) 0.289(3) 0.1774(18) 0.0581 1.0000 Uiso . . . . . .
H112 H 0.178(3) 0.376(3) 0.1718(18) 0.0597 1.0000 Uiso . . . . . .
H111 H 0.175(3) 0.233(3) 0.143(2) 0.0611 1.0000 Uiso . . . . . .
H123 H -0.209(3) 0.267(3) 0.3327(18) 0.0596 1.0000 Uiso . . . . . .
H122 H -0.134(3) 0.262(3) 0.2586(19) 0.0594 1.0000 Uiso . . . . . .
H121 H -0.188(3) 0.137(3) 0.2869(19) 0.0608 1.0000 Uiso . . . . . .
H133 H -0.067(3) 0.238(3) 0.5606(18) 0.0471 1.0000 Uiso . . . . . .
H132 H -0.180(3) 0.250(3) 0.4885(17) 0.0485 1.0000 Uiso . . . . . .
H131 H -0.136(3) 0.118(3) 0.5285(16) 0.0474 1.0000 Uiso . . . . . .
H143 H 0.307(3) 0.139(3) 0.5914(16) 0.0492 1.0000 Uiso . . . . . .
H142 H 0.170(3) 0.198(3) 0.6157(18) 0.0515 1.0000 Uiso . . . . . .
H141 H 0.173(3) 0.060(3) 0.6042(17) 0.0513 1.0000 Uiso . . . . . .
H153 H 0.354(3) 0.395(3) 0.5537(18) 0.0558 1.0000 Uiso . . . . . .
H152 H 0.224(3) 0.491(3) 0.5382(18) 0.0570 1.0000 Uiso . . . . . .
H151 H 0.342(3) 0.515(3) 0.4880(18) 0.0559 1.0000 Uiso . . . . . .
H163 H -0.009(3) 0.471(3) 0.2815(19) 0.0582 1.0000 Uiso . . . . . .
H162 H -0.005(3) 0.541(3) 0.3766(18) 0.0591 1.0000 Uiso . . . . . .
H161 H 0.119(3) 0.561(3) 0.3237(18) 0.0581 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.744(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.413(2) yes
C1 . C8 . 1.447(2) yes
C1 . C9 . 1.496(2) yes
C1 . Ti1 . 2.3542(16) yes
C2 . C3 . 1.421(2) yes
C2 . C10 . 1.503(2) yes
C2 . Ti1 . 2.4591(16) yes
C3 . C4 . 1.438(2) yes
C3 . C11 . 1.502(2) yes
C3 . Ti1 . 2.3386(16) yes
C4 . C5 . 1.444(2) yes
C4 . C8 . 1.467(2) yes
C4 . Ti1 . 2.1268(15) yes
C5 . C6 . 1.417(2) yes
C5 . C12 . 1.503(2) yes
C5 . Ti1 . 2.3606(16) yes
C6 . C7 . 1.421(2) yes
C6 . C13 . 1.503(2) yes
C6 . Ti1 . 2.4732(16) yes
C7 . C8 . 1.443(2) yes
C7 . C14 . 1.504(2) yes
C7 . Ti1 . 2.3289(15) yes
C8 . Ti1 . 2.1255(14) yes
C9 . H93 . 0.91(3) no
C9 . H92 . 0.95(3) no
C9 . H91 . 1.00(3) no
C10 . H103 . 0.93(3) no
C10 . H102 . 0.94(3) no
C10 . H101 . 0.93(3) no
C11 . H113 . 0.95(3) no
C11 . H112 . 1.02(3) no
C11 . H111 . 0.90(3) no
C12 . H123 . 0.95(3) no
C12 . H122 . 0.93(3) no
C12 . H121 . 0.89(3) no
C13 . H133 . 0.90(3) no
C13 . H132 . 0.94(3) no
C13 . H131 . 0.90(3) no
C14 . H143 . 0.92(3) no
C14 . H142 . 0.95(3) no
C14 . H141 . 0.94(3) no
C15 . Ti1 . 2.1385(19) yes
C15 . H153 . 0.99(3) no
C15 . H152 . 0.91(3) no
C15 . H151 . 0.95(3) no
C16 . Ti1 . 2.1318(19) yes
C16 . H163 . 0.98(3) no
C16 . H162 . 0.97(3) no
C16 . H161 . 0.98(3) no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C8 . 107.25(13) yes
C2 . C1 . C9 . 125.41(15) yes
C8 . C1 . C9 . 127.18(15) yes
C2 . C1 . Ti1 . 77.04(9) yes
C8 . C1 . Ti1 . 62.76(8) yes
C9 . C1 . Ti1 . 128.80(12) yes
C1 . C2 . C3 . 110.73(14) yes
C1 . C2 . C10 . 124.16(15) yes
C3 . C2 . C10 . 125.07(15) yes
C1 . C2 . Ti1 . 68.90(9) yes
C3 . C2 . Ti1 . 68.18(9) yes
C10 . C2 . Ti1 . 128.18(12) yes
C2 . C3 . C4 . 107.10(13) yes
C2 . C3 . C11 . 125.41(15) yes
C4 . C3 . C11 . 127.34(15) yes
C2 . C3 . Ti1 . 77.47(9) yes
C4 . C3 . Ti1 . 63.38(8) yes
C11 . C3 . Ti1 . 127.50(13) yes
C3 . C4 . C5 . 129.85(14) yes
C3 . C4 . C8 . 107.72(13) yes
C5 . C4 . C8 . 107.29(13) yes
C3 . C4 . Ti1 . 79.43(9) yes
C5 . C4 . Ti1 . 80.29(9) yes
C8 . C4 . Ti1 . 69.77(8) yes
C4 . C5 . C6 . 107.39(13) yes
C4 . C5 . C12 . 127.19(15) yes
C6 . C5 . C12 . 125.33(15) yes
C4 . C5 . Ti1 . 62.63(8) yes
C6 . C5 . Ti1 . 77.36(9) yes
C12 . C5 . Ti1 . 127.62(13) yes
C5 . C6 . C7 . 110.54(14) yes
C5 . C6 . C13 . 125.45(15) yes
C7 . C6 . C13 . 123.96(15) yes
C5 . C6 . Ti1 . 68.64(9) yes
C7 . C6 . Ti1 . 67.30(8) yes
C13 . C6 . Ti1 . 129.13(11) yes
C6 . C7 . C8 . 107.10(13) yes
C6 . C7 . C14 . 124.76(15) yes
C8 . C7 . C14 . 127.99(15) yes
C6 . C7 . Ti1 . 78.43(9) yes
C8 . C7 . Ti1 . 63.60(8) yes
C14 . C7 . Ti1 . 126.56(11) yes
C4 . C8 . C1 . 107.18(13) yes
C4 . C8 . C7 . 107.61(13) yes
C1 . C8 . C7 . 129.49(13) yes
C4 . C8 . Ti1 . 69.87(8) yes
C1 . C8 . Ti1 . 79.98(9) yes
C7 . C8 . Ti1 . 78.94(9) yes
C1 . C9 . H93 . 108.9(18) no
C1 . C9 . H92 . 110.2(16) no
H93 . C9 . H92 . 114(2) no
C1 . C9 . H91 . 106.0(15) no
H93 . C9 . H91 . 106(2) no
H92 . C9 . H91 . 111(2) no
C2 . C10 . H103 . 110.9(16) no
C2 . C10 . H102 . 113.0(16) no
H103 . C10 . H102 . 107(2) no
C2 . C10 . H101 . 110.7(17) no
H103 . C10 . H101 . 110(2) no
H102 . C10 . H101 . 105(2) no
C3 . C11 . H113 . 111.8(17) no
C3 . C11 . H112 . 110.6(16) no
H113 . C11 . H112 . 106(2) no
C3 . C11 . H111 . 112.6(19) no
H113 . C11 . H111 . 112(3) no
H112 . C11 . H111 . 104(2) no
C5 . C12 . H123 . 114.4(17) no
C5 . C12 . H122 . 112.0(17) no
H123 . C12 . H122 . 99(2) no
C5 . C12 . H121 . 114.7(19) no
H123 . C12 . H121 . 110(2) no
H122 . C12 . H121 . 105(2) no
C6 . C13 . H133 . 108.2(16) no
C6 . C13 . H132 . 115.3(16) no
H133 . C13 . H132 . 105(2) no
C6 . C13 . H131 . 111.6(17) no
H133 . C13 . H131 . 107(2) no
H132 . C13 . H131 . 110(2) no
C7 . C14 . H143 . 113.6(16) no
C7 . C14 . H142 . 110.7(16) no
H143 . C14 . H142 . 110(2) no
C7 . C14 . H141 . 112.5(16) no
H143 . C14 . H141 . 112(2) no
H142 . C14 . H141 . 97(2) no
Ti1 . C15 . H153 . 119.4(17) no
Ti1 . C15 . H152 . 105.5(17) no
H153 . C15 . H152 . 111(2) no
Ti1 . C15 . H151 . 107.4(17) no
H153 . C15 . H151 . 108(2) no
H152 . C15 . H151 . 104(2) no
Ti1 . C16 . H163 . 117.6(17) no
Ti1 . C16 . H162 . 108.0(16) no
H163 . C16 . H162 . 114(2) no
Ti1 . C16 . H161 . 102.6(16) no
H163 . C16 . H161 . 109(2) no
H162 . C16 . H161 . 104(2) no
C7 . Ti1 . C3 . 96.97(6) yes
C7 . Ti1 . C1 . 67.86(6) yes
C3 . Ti1 . C1 . 59.60(5) yes
C7 . Ti1 . C5 . 59.66(5) yes
C3 . Ti1 . C5 . 67.50(6) yes
C1 . Ti1 . C5 . 96.20(6) yes
C7 . Ti1 . C2 . 96.69(5) yes
C3 . Ti1 . C2 . 34.35(5) yes
C1 . Ti1 . C2 . 34.07(5) yes
C5 . Ti1 . C2 . 96.28(5) yes
C7 . Ti1 . C6 . 34.27(5) yes
C3 . Ti1 . C6 . 96.26(5) yes
C1 . Ti1 . C6 . 96.35(5) yes
C5 . Ti1 . C6 . 34.00(5) yes
C2 . Ti1 . C6 . 114.89(5) yes
C7 . Ti1 . C15 . 92.18(7) yes
C3 . Ti1 . C15 . 141.31(7) yes
C1 . Ti1 . C15 . 90.09(7) yes
C5 . Ti1 . C15 . 145.46(7) yes
C2 . Ti1 . C15 . 107.33(7) yes
C7 . Ti1 . C16 . 142.38(7) yes
C3 . Ti1 . C16 . 90.33(8) yes
C1 . Ti1 . C16 . 143.26(7) yes
C5 . Ti1 . C16 . 90.10(7) yes
C2 . Ti1 . C16 . 109.33(7) yes
C7 . Ti1 . C4 . 63.43(6) yes
C3 . Ti1 . C4 . 37.20(6) yes
C1 . Ti1 . C4 . 62.88(6) yes
C5 . Ti1 . C4 . 37.09(6) yes
C2 . Ti1 . C4 . 59.69(6) yes
C7 . Ti1 . C8 . 37.46(5) yes
C3 . Ti1 . C8 . 63.20(6) yes
C1 . Ti1 . C8 . 37.26(6) yes
C5 . Ti1 . C8 . 62.76(6) yes
C2 . Ti1 . C8 . 59.79(6) yes
C6 . Ti1 . C15 . 111.61(7) yes
C6 . Ti1 . C16 . 108.35(7) yes
C15 . Ti1 . C16 . 104.84(9) yes
C6 . Ti1 . C4 . 59.61(6) yes
C15 . Ti1 . C4 . 148.31(7) yes
C16 . Ti1 . C4 . 106.78(8) yes
C6 . Ti1 . C8 . 59.57(6) yes
C15 . Ti1 . C8 . 108.01(7) yes
C16 . Ti1 . C8 . 147.13(8) yes
C4 . Ti1 . C8 . 40.36(5) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 28/09/11 at 10:49:27
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT C    (    1 ,X'S,U'S)  UNTIL TI   (    1 ) 
CONT H    (   93 ,X'S)  UNTIL H    (  161 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 28/09/11 at 10:49:27
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1063832'
_audit_update_record             
;
2015-05-07 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;
#=================================================

_audit_creation_date             11-03-04
_audit_creation_method           CRYSTALS_ver_14.11

_oxford_structure_analysis_title 020fmc11
_chemical_name_systematic        Pn*TiBz2
_chemical_melting_point          .


_cell_length_a                   9.4641(2)
_cell_length_b                   10.4852(2)
_cell_length_c                   13.1120(3)
_cell_angle_alpha                72.5421(10)
_cell_angle_beta                 79.0295(10)
_cell_angle_gamma                64.7729(11)
_cell_volume                     1119.89(4)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C28 H32 Ti1 
# Dc =      1.23 Fooo =    444.00 Mu =      3.93 M =    416.46
# Found Formula = C28 H32 Ti1 
# Dc =      1.23 FOOO =    444.00 Mu =      3.93 M =    416.46

_chemical_formula_sum            'C28 H32 Ti1'
_chemical_formula_moiety         'C28 H32 Ti1'
_chemical_compound_source        SYN
_chemical_formula_weight         416.46


_cell_measurement_reflns_used    4671
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_max          0.120

_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             444
_exptl_absorpt_coefficient_mu    0.393

# Sheldrick geometric approximatio 0.96 0.97 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  0.97
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        'not measured'

_diffrn_ambient_temperature      150
_diffrn_reflns_number            19048
_reflns_number_total             5000
_diffrn_reflns_av_R_equivalents  0.031
# Number of reflections without Friedels Law is 8757 
# Number of reflections with Friedels Law is 5000 
# Theoretical number of reflections is about 5069 


_diffrn_reflns_theta_min         5.091
_diffrn_reflns_theta_max         27.352
_diffrn_measured_fraction_theta_max 0.987

_diffrn_reflns_theta_full        25.984
_diffrn_measured_fraction_theta_full 0.991


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -11
_reflns_limit_h_max              12
_reflns_limit_k_min              -12
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.07
_oxford_diffrn_Wilson_scale      4.31

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.50
_refine_diff_density_max         0.47


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         5000
_refine_ls_number_restraints     0
_refine_ls_number_parameters     262
_oxford_refine_ls_R_factor_ref   0.0647
_refine_ls_wR_factor_ref         0.1186
_refine_ls_goodness_of_fit_ref   0.8911
_refine_ls_shift/su_max          0.0002510
_refine_ls_shift/su_mean         0.0000126


# The values computed from all data 
_oxford_reflns_number_all        5000
_refine_ls_R_factor_all          0.0647
_refine_ls_wR_factor_all         0.1186

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3780
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_gt          0.0939

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 13.5 19.4 9.15 2.30 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.2036(3) 0.4483(2) 0.11189(19) 0.0280 1.0000 Uani . . . . . .
C2 C 0.2382(3) 0.4961(2) 0.19097(19) 0.0275 1.0000 Uani . . . . . .
C3 C 0.1857(3) 0.4340(2) 0.29507(19) 0.0263 1.0000 Uani . . . . . .
C4 C 0.1093(3) 0.3476(2) 0.28170(17) 0.0240 1.0000 Uani . . . . . .
C5 C 0.1209(3) 0.2035(3) 0.33918(18) 0.0258 1.0000 Uani . . . . . .
C6 C 0.1327(3) 0.1298(3) 0.2614(2) 0.0278 1.0000 Uani . . . . . .
C7 C 0.1374(3) 0.2184(3) 0.15615(19) 0.0278 1.0000 Uani . . . . . .
C8 C 0.1199(3) 0.3570(2) 0.16686(18) 0.0247 1.0000 Uani . . . . . .
C9 C 0.2394(3) 0.4928(3) -0.0069(2) 0.0395 1.0000 Uani . . . . . .
C10 C 0.3206(3) 0.5977(3) 0.1682(3) 0.0411 1.0000 Uani . . . . . .
C11 C 0.1910(3) 0.4696(3) 0.3964(2) 0.0348 1.0000 Uani . . . . . .
C12 C 0.1060(3) 0.1436(3) 0.4583(2) 0.0347 1.0000 Uani . . . . . .
C13 C 0.1329(3) -0.0197(3) 0.2878(2) 0.0389 1.0000 Uani . . . . . .
C14 C 0.1396(3) 0.1784(3) 0.0550(2) 0.0380 1.0000 Uani . . . . . .
C15 C 0.5091(3) 0.1637(3) 0.09438(19) 0.0305 1.0000 Uani . . . . . .
C16 C 0.6072(3) 0.0105(3) 0.14237(18) 0.0271 1.0000 Uani . . . . . .
C17 C 0.5463(3) -0.0972(3) 0.1709(2) 0.0324 1.0000 Uani . . . . . .
C18 C 0.6325(3) -0.2395(3) 0.2237(2) 0.0384 1.0000 Uani . . . . . .
C19 C 0.7836(3) -0.2795(3) 0.2500(2) 0.0412 1.0000 Uani . . . . . .
C20 C 0.8467(3) -0.1747(3) 0.2218(2) 0.0379 1.0000 Uani . . . . . .
C21 C 0.7613(3) -0.0332(3) 0.1692(2) 0.0320 1.0000 Uani . . . . . .
C22 C 0.4723(3) 0.1313(3) 0.37092(18) 0.0263 1.0000 Uani . . . . . .
C23 C 0.5595(3) 0.2118(2) 0.38561(17) 0.0246 1.0000 Uani . . . . . .
C24 C 0.6529(3) 0.2635(3) 0.30159(19) 0.0286 1.0000 Uani . . . . . .
C25 C 0.7275(3) 0.3467(3) 0.3134(2) 0.0332 1.0000 Uani . . . . . .
C26 C 0.7115(3) 0.3798(3) 0.4107(2) 0.0350 1.0000 Uani . . . . . .
C27 C 0.6217(3) 0.3290(3) 0.4957(2) 0.0321 1.0000 Uani . . . . . .
C28 C 0.5468(3) 0.2463(3) 0.48364(18) 0.0281 1.0000 Uani . . . . . .
Ti1 Ti 0.34337(5) 0.22668(4) 0.22965(3) 0.0217 1.0000 Uani . . . . . .
H93 H 0.2616 0.4169 -0.0420 0.0624 1.0000 Uiso R . . . . .
H91 H 0.1537 0.5703 -0.0429 0.0634 1.0000 Uiso R . . . . .
H92 H 0.3270 0.5177 -0.0238 0.0621 1.0000 Uiso R . . . . .
H101 H 0.3726 0.5791 0.2277 0.0616 1.0000 Uiso R . . . . .
H103 H 0.2505 0.6951 0.1546 0.0630 1.0000 Uiso R . . . . .
H102 H 0.3919 0.5831 0.1092 0.0625 1.0000 Uiso R . . . . .
H112 H 0.1885 0.3924 0.4579 0.0516 1.0000 Uiso R . . . . .
H111 H 0.1046 0.5587 0.4029 0.0499 1.0000 Uiso R . . . . .
H113 H 0.2868 0.4847 0.3955 0.0511 1.0000 Uiso R . . . . .
H122 H 0.1774 0.0433 0.4773 0.0507 1.0000 Uiso R . . . . .
H123 H 0.1278 0.2009 0.4934 0.0520 1.0000 Uiso R . . . . .
H121 H -0.0006 0.1489 0.4761 0.0517 1.0000 Uiso R . . . . .
H133 H 0.1725 -0.0610 0.2275 0.0577 1.0000 Uiso R . . . . .
H131 H 0.2015 -0.0822 0.3443 0.0577 1.0000 Uiso R . . . . .
H132 H 0.0288 -0.0175 0.3106 0.0578 1.0000 Uiso R . . . . .
H141 H 0.1556 0.2462 -0.0089 0.0582 1.0000 Uiso R . . . . .
H143 H 0.2190 0.0841 0.0535 0.0581 1.0000 Uiso R . . . . .
H142 H 0.0417 0.1750 0.0512 0.0585 1.0000 Uiso R . . . . .
H171 H 0.4444 -0.0671 0.1520 0.0388 1.0000 Uiso R . . . . .
H181 H 0.5859 -0.3062 0.2404 0.0464 1.0000 Uiso R . . . . .
H191 H 0.8437 -0.3747 0.2852 0.0489 1.0000 Uiso R . . . . .
H201 H 0.9477 -0.2010 0.2403 0.0448 1.0000 Uiso R . . . . .
H211 H 0.8071 0.0348 0.1487 0.0382 1.0000 Uiso R . . . . .
H221 H 0.4129 0.1060 0.4353 0.0334 1.0000 Uiso R . . . . .
H222 H 0.5478 0.0402 0.3538 0.0321 1.0000 Uiso R . . . . .
H241 H 0.6637 0.2417 0.2356 0.0335 1.0000 Uiso R . . . . .
H251 H 0.7912 0.3793 0.2568 0.0407 1.0000 Uiso R . . . . .
H261 H 0.7627 0.4360 0.4186 0.0398 1.0000 Uiso R . . . . .
H271 H 0.6122 0.3538 0.5611 0.0388 1.0000 Uiso R . . . . .
H281 H 0.4882 0.2140 0.5433 0.0338 1.0000 Uiso R . . . . .
H152 H 0.4561 0.1761 0.0364 0.0378 1.0000 Uiso R . . . . .
H151 H 0.5686 0.2237 0.0658 0.0389 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.4729(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.419(3) yes
C1 . C8 . 1.442(3) yes
C1 . C9 . 1.502(3) yes
C1 . Ti1 . 2.353(2) yes
C2 . C3 . 1.421(3) yes
C2 . C10 . 1.504(3) yes
C2 . Ti1 . 2.483(2) yes
C3 . C4 . 1.441(3) yes
C3 . C11 . 1.499(3) yes
C3 . Ti1 . 2.357(2) yes
C4 . C5 . 1.439(3) yes
C4 . C8 . 1.466(3) yes
C4 . Ti1 . 2.129(2) yes
C5 . C6 . 1.417(3) yes
C5 . C12 . 1.503(3) yes
C5 . Ti1 . 2.373(2) yes
C6 . C7 . 1.418(3) yes
C6 . C13 . 1.499(3) yes
C6 . Ti1 . 2.518(2) yes
C7 . C8 . 1.438(3) yes
C7 . C14 . 1.501(3) yes
C7 . Ti1 . 2.376(2) yes
C8 . Ti1 . 2.131(2) yes
C9 . H93 . 0.963 no
C9 . H91 . 0.946 no
C9 . H92 . 0.941 no
C10 . H101 . 0.927 no
C10 . H103 . 0.935 no
C10 . H102 . 0.928 no
C11 . H112 . 0.961 no
C11 . H111 . 0.958 no
C11 . H113 . 0.982 no
C12 . H122 . 0.961 no
C12 . H123 . 0.960 no
C12 . H121 . 0.973 no
C13 . H133 . 0.953 no
C13 . H131 . 0.964 no
C13 . H132 . 0.967 no
C14 . H141 . 0.957 no
C14 . H143 . 0.956 no
C14 . H142 . 0.954 no
C15 . C16 . 1.478(3) yes
C15 . Ti1 . 2.191(2) yes
C15 . H152 . 0.937 no
C15 . H151 . 0.966 no
C16 . C17 . 1.402(3) yes
C16 . C21 . 1.410(3) yes
C17 . C18 . 1.389(4) yes
C17 . H171 . 0.936 no
C18 . C19 . 1.389(4) yes
C18 . H181 . 0.931 no
C19 . C20 . 1.390(4) yes
C19 . H191 . 0.934 no
C20 . C21 . 1.381(4) yes
C20 . H201 . 0.934 no
C21 . H211 . 0.935 no
C22 . C23 . 1.476(3) yes
C22 . Ti1 . 2.152(2) yes
C22 . H221 . 0.955 no
C22 . H222 . 0.979 no
C23 . C24 . 1.403(3) yes
C23 . C28 . 1.407(3) yes
C24 . C25 . 1.389(3) yes
C24 . H241 . 0.936 no
C25 . C26 . 1.385(4) yes
C25 . H251 . 0.941 no
C26 . C27 . 1.385(4) yes
C26 . H261 . 0.945 no
C27 . C28 . 1.389(3) yes
C27 . H271 . 0.945 no
C28 . H281 . 0.933 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C8 . 106.9(2) yes
C2 . C1 . C9 . 126.0(2) yes
C8 . C1 . C9 . 127.0(2) yes
C2 . C1 . Ti1 . 78.00(13) yes
C8 . C1 . Ti1 . 63.07(12) yes
C9 . C1 . Ti1 . 126.54(16) yes
C1 . C2 . C3 . 110.9(2) yes
C1 . C2 . C10 . 124.8(2) yes
C3 . C2 . C10 . 124.3(2) yes
C1 . C2 . Ti1 . 68.00(13) yes
C3 . C2 . Ti1 . 68.15(13) yes
C10 . C2 . Ti1 . 130.78(16) yes
C2 . C3 . C4 . 106.9(2) yes
C2 . C3 . C11 . 125.4(2) yes
C4 . C3 . C11 . 127.2(2) yes
C2 . C3 . Ti1 . 77.83(13) yes
C4 . C3 . Ti1 . 62.83(12) yes
C11 . C3 . Ti1 . 130.18(17) yes
C3 . C4 . C5 . 130.5(2) yes
C3 . C4 . C8 . 107.67(19) yes
C5 . C4 . C8 . 107.80(19) yes
C3 . C4 . Ti1 . 80.13(13) yes
C5 . C4 . Ti1 . 80.87(13) yes
C8 . C4 . Ti1 . 69.98(12) yes
C4 . C5 . C6 . 106.69(19) yes
C4 . C5 . C12 . 128.1(2) yes
C6 . C5 . C12 . 124.9(2) yes
C4 . C5 . Ti1 . 62.34(11) yes
C6 . C5 . Ti1 . 78.87(13) yes
C12 . C5 . Ti1 . 128.56(16) yes
C5 . C6 . C7 . 111.0(2) yes
C5 . C6 . C13 . 124.0(2) yes
C7 . C6 . C13 . 124.9(2) yes
C5 . C6 . Ti1 . 67.62(12) yes
C7 . C6 . Ti1 . 67.73(13) yes
C13 . C6 . Ti1 . 134.17(17) yes
C6 . C7 . C8 . 106.9(2) yes
C6 . C7 . C14 . 125.2(2) yes
C8 . C7 . C14 . 127.4(2) yes
C6 . C7 . Ti1 . 78.73(13) yes
C8 . C7 . Ti1 . 62.37(12) yes
C14 . C7 . Ti1 . 129.45(17) yes
C4 . C8 . C1 . 107.59(19) yes
C4 . C8 . C7 . 107.45(19) yes
C1 . C8 . C7 . 130.7(2) yes
C4 . C8 . Ti1 . 69.77(12) yes
C1 . C8 . Ti1 . 79.84(13) yes
C7 . C8 . Ti1 . 80.93(13) yes
C1 . C9 . H93 . 112.7 no
C1 . C9 . H91 . 113.2 no
H93 . C9 . H91 . 102.7 no
C1 . C9 . H92 . 112.4 no
H93 . C9 . H92 . 106.2 no
H91 . C9 . H92 . 109.0 no
C2 . C10 . H101 . 109.1 no
C2 . C10 . H103 . 112.0 no
H101 . C10 . H103 . 107.6 no
C2 . C10 . H102 . 109.4 no
H101 . C10 . H102 . 109.8 no
H103 . C10 . H102 . 109.0 no
C3 . C11 . H112 . 111.0 no
C3 . C11 . H111 . 109.8 no
H112 . C11 . H111 . 110.1 no
C3 . C11 . H113 . 111.0 no
H112 . C11 . H113 . 108.1 no
H111 . C11 . H113 . 106.8 no
C5 . C12 . H122 . 109.9 no
C5 . C12 . H123 . 108.8 no
H122 . C12 . H123 . 110.8 no
C5 . C12 . H121 . 106.4 no
H122 . C12 . H121 . 108.8 no
H123 . C12 . H121 . 112.0 no
C6 . C13 . H133 . 110.8 no
C6 . C13 . H131 . 109.4 no
H133 . C13 . H131 . 107.0 no
C6 . C13 . H132 . 111.1 no
H133 . C13 . H132 . 109.2 no
H131 . C13 . H132 . 109.3 no
C7 . C14 . H141 . 113.6 no
C7 . C14 . H143 . 111.2 no
H141 . C14 . H143 . 108.2 no
C7 . C14 . H142 . 109.6 no
H141 . C14 . H142 . 106.7 no
H143 . C14 . H142 . 107.2 no
C16 . C15 . Ti1 . 101.94(15) yes
C16 . C15 . H152 . 113.9 no
Ti1 . C15 . H152 . 110.8 no
C16 . C15 . H151 . 113.0 no
Ti1 . C15 . H151 . 113.2 no
H152 . C15 . H151 . 104.3 no
C15 . C16 . C17 . 121.0(2) yes
C15 . C16 . C21 . 122.3(2) yes
C17 . C16 . C21 . 116.6(2) yes
C16 . C17 . C18 . 121.8(2) yes
C16 . C17 . H171 . 115.8 no
C18 . C17 . H171 . 122.4 no
C17 . C18 . C19 . 120.4(3) yes
C17 . C18 . H181 . 117.9 no
C19 . C18 . H181 . 121.7 no
C18 . C19 . C20 . 118.7(3) yes
C18 . C19 . H191 . 121.8 no
C20 . C19 . H191 . 119.5 no
C19 . C20 . C21 . 121.0(2) yes
C19 . C20 . H201 . 118.9 no
C21 . C20 . H201 . 120.1 no
C16 . C21 . C20 . 121.4(2) yes
C16 . C21 . H211 . 118.9 no
C20 . C21 . H211 . 119.6 no
C23 . C22 . Ti1 . 115.23(15) yes
C23 . C22 . H221 . 111.3 no
Ti1 . C22 . H221 . 114.2 no
C23 . C22 . H222 . 108.5 no
Ti1 . C22 . H222 . 99.5 no
H221 . C22 . H222 . 107.1 no
C22 . C23 . C24 . 121.9(2) yes
C22 . C23 . C28 . 121.4(2) yes
C24 . C23 . C28 . 116.7(2) yes
C23 . C24 . C25 . 122.0(2) yes
C23 . C24 . H241 . 118.4 no
C25 . C24 . H241 . 119.6 no
C24 . C25 . C26 . 119.9(2) yes
C24 . C25 . H251 . 121.2 no
C26 . C25 . H251 . 118.9 no
C25 . C26 . C27 . 119.6(2) yes
C25 . C26 . H261 . 119.7 no
C27 . C26 . H261 . 120.6 no
C26 . C27 . C28 . 120.4(2) yes
C26 . C27 . H271 . 117.9 no
C28 . C27 . H271 . 121.7 no
C23 . C28 . C27 . 121.4(2) yes
C23 . C28 . H281 . 121.3 no
C27 . C28 . H281 . 117.3 no
C1 . Ti1 . C3 . 59.55(8) yes
C1 . Ti1 . C5 . 95.92(8) yes
C3 . Ti1 . C5 . 67.16(8) yes
C1 . Ti1 . C7 . 67.20(9) yes
C3 . Ti1 . C7 . 95.66(8) yes
C5 . Ti1 . C7 . 58.96(8) yes
C1 . Ti1 . C15 . 88.76(9) yes
C3 . Ti1 . C15 . 140.58(9) yes
C5 . Ti1 . C15 . 145.29(9) yes
C7 . Ti1 . C15 . 92.12(9) yes
C1 . Ti1 . C2 . 34.00(8) yes
C3 . Ti1 . C2 . 34.02(8) yes
C5 . Ti1 . C2 . 95.53(8) yes
C7 . Ti1 . C2 . 95.43(8) yes
C15 . Ti1 . C2 . 106.83(9) yes
C1 . Ti1 . C22 . 143.98(9) yes
C3 . Ti1 . C22 . 90.17(9) yes
C5 . Ti1 . C22 . 88.54(8) yes
C7 . Ti1 . C22 . 140.81(9) yes
C15 . Ti1 . C22 . 107.49(9) yes
C1 . Ti1 . C6 . 95.10(8) yes
C3 . Ti1 . C6 . 94.95(8) yes
C5 . Ti1 . C6 . 33.51(8) yes
C7 . Ti1 . C6 . 33.54(8) yes
C15 . Ti1 . C6 . 111.89(9) yes
C1 . Ti1 . C8 . 37.09(8) yes
C3 . Ti1 . C8 . 62.81(8) yes
C5 . Ti1 . C8 . 62.55(8) yes
C7 . Ti1 . C8 . 36.70(8) yes
C15 . Ti1 . C8 . 106.75(9) yes
C1 . Ti1 . C4 . 62.90(8) yes
C3 . Ti1 . C4 . 37.03(8) yes
C5 . Ti1 . C4 . 36.79(8) yes
C7 . Ti1 . C4 . 62.34(8) yes
C15 . Ti1 . C4 . 146.94(9) yes
C2 . Ti1 . C22 . 110.05(9) yes
C2 . Ti1 . C6 . 113.03(8) yes
C22 . Ti1 . C6 . 107.42(8) yes
C2 . Ti1 . C8 . 59.18(8) yes
C22 . Ti1 . C8 . 145.75(9) yes
C6 . Ti1 . C8 . 58.45(8) yes
C2 . Ti1 . C4 . 59.20(8) yes
C22 . Ti1 . C4 . 105.53(9) yes
C6 . Ti1 . C4 . 58.37(8) yes
C8 . Ti1 . C4 . 40.25(8) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 04/03/11 at 15:35:49
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   9,X'S) H   (  93,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 103,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 112,X'S) H   ( 111,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 123,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 133,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 143,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 152,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 04/03/11 at 15:35:49
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1063833'
_audit_update_record             
;
2015-05-07 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;
#================================================

_audit_creation_date             11-12-07
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 087fmc11
_chemical_name_systematic        Pn*Ti(O2CMe)2
_chemical_melting_point          'not measured'
_cell_length_a                   8.0338(2)
_cell_length_b                   9.4658(2)
_cell_length_c                   11.9668(3)
_cell_angle_alpha                78.4790(11)
_cell_angle_beta                 88.7238(11)
_cell_angle_gamma                75.3323(12)
_cell_volume                     862.25(4)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C18 H24 O4 Ti1 
# Dc =      1.36 Fooo =    372.00 Mu =      5.13 M =    352.29
# Found Formula = C18 H24 O4 Ti1 
# Dc =      1.36 FOOO =    372.00 Mu =      5.13 M =    352.29

_chemical_formula_sum            'C18 H24 O4 Ti1'
_chemical_formula_moiety         'C18 H24 O4 Ti1'
_chemical_compound_source        SYN
_chemical_formula_weight         352.29


_cell_measurement_reflns_used    3496
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.400

_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             372
_exptl_absorpt_coefficient_mu    0.513

# Sheldrick geometric approximatio 0.90 0.97 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_T_max  0.97
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            12188
_reflns_number_total             3922
_diffrn_reflns_av_R_equivalents  0.019
# Number of reflections without Friedels Law is 6556 
# Number of reflections with Friedels Law is 3922 
# Theoretical number of reflections is about 3958 


_diffrn_reflns_theta_min         5.140
_diffrn_reflns_theta_max         27.492
_diffrn_measured_fraction_theta_max 0.990

_diffrn_reflns_theta_full        26.392
_diffrn_measured_fraction_theta_full 0.992


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              -11
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              15

_oxford_diffrn_Wilson_B_factor   1.70
_oxford_diffrn_Wilson_scale      1.09

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.46
_refine_diff_density_max         0.42


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3922
_refine_ls_number_restraints     0
_refine_ls_number_parameters     208
_oxford_refine_ls_R_factor_ref   0.0485
_refine_ls_wR_factor_ref         0.1122
_refine_ls_goodness_of_fit_ref   0.9397
_refine_ls_shift/su_max          0.0001467
_refine_ls_shift/su_mean         0.0000110


# The values computed from all data 
_oxford_reflns_number_all        3922
_refine_ls_R_factor_all          0.0485
_refine_ls_wR_factor_all         0.1122

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3481
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_gt          0.1070

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 27.9 41.6 20.8 5.61 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ti1 Ti 0.39250(4) 0.26001(4) 0.23966(3) 0.0179 1.0000 Uani . . . . . .
O1 O 0.55585(19) 0.40977(16) 0.21303(12) 0.0243 1.0000 Uani . . . . . .
O2 O 0.44465(18) 0.35576(16) 0.37930(12) 0.0234 1.0000 Uani . . . . . .
O3 O 0.62226(18) 0.09562(16) 0.30718(12) 0.0252 1.0000 Uani . . . . . .
O4 O 0.56601(17) 0.15687(15) 0.12385(12) 0.0228 1.0000 Uani . . . . . .
C1 C 0.2144(2) 0.3399(2) 0.07259(16) 0.0201 1.0000 Uani . . . . . .
C2 C 0.1903(2) 0.4752(2) 0.11180(17) 0.0218 1.0000 Uani . . . . . .
C3 C 0.1394(2) 0.4566(2) 0.22664(17) 0.0217 1.0000 Uani . . . . . .
C4 C 0.1216(2) 0.3057(2) 0.26060(16) 0.0201 1.0000 Uani . . . . . .
C5 C 0.1764(2) 0.1952(2) 0.36329(16) 0.0213 1.0000 Uani . . . . . .
C6 C 0.2506(3) 0.0582(2) 0.32946(17) 0.0226 1.0000 Uani . . . . . .
C7 C 0.2522(2) 0.0788(2) 0.20901(17) 0.0215 1.0000 Uani . . . . . .
C8 C 0.1687(2) 0.2334(2) 0.16380(16) 0.0195 1.0000 Uani . . . . . .
C9 C 0.2698(3) 0.3172(2) -0.04469(16) 0.0252 1.0000 Uani . . . . . .
C10 C 0.2244(3) 0.6150(2) 0.04331(18) 0.0284 1.0000 Uani . . . . . .
C11 C 0.1045(3) 0.5756(2) 0.29660(19) 0.0282 1.0000 Uani . . . . . .
C12 C 0.1528(3) 0.2170(2) 0.48411(18) 0.0283 1.0000 Uani . . . . . .
C13 C 0.3238(3) -0.0879(2) 0.40910(19) 0.0308 1.0000 Uani . . . . . .
C14 C 0.3204(3) -0.0424(2) 0.14382(19) 0.0280 1.0000 Uani . . . . . .
C15 C 0.5465(3) 0.4185(2) 0.31738(17) 0.0241 1.0000 Uani . . . . . .
C16 C 0.6565(3) 0.4991(3) 0.3664(2) 0.0389 1.0000 Uani . . . . . .
C17 C 0.6698(2) 0.0880(2) 0.20611(17) 0.0222 1.0000 Uani . . . . . .
C18 C 0.8476(3) 0.0025(3) 0.1853(2) 0.0332 1.0000 Uani . . . . . .
H93 H 0.3376 0.2189 -0.0420 0.0360 1.0000 Uiso R . . . . .
H92 H 0.3408 0.3842 -0.0728 0.0376 1.0000 Uiso R . . . . .
H91 H 0.1735 0.3437 -0.0952 0.0353 1.0000 Uiso R . . . . .
H103 H 0.1873 0.6988 0.0770 0.0444 1.0000 Uiso R . . . . .
H102 H 0.3391 0.6092 0.0283 0.0431 1.0000 Uiso R . . . . .
H101 H 0.1657 0.6436 -0.0299 0.0443 1.0000 Uiso R . . . . .
H113 H 0.1097 0.5340 0.3753 0.0430 1.0000 Uiso R . . . . .
H112 H 0.1843 0.6392 0.2873 0.0423 1.0000 Uiso R . . . . .
H111 H -0.0068 0.6421 0.2820 0.0412 1.0000 Uiso R . . . . .
H123 H 0.2254 0.1305 0.5365 0.0422 1.0000 Uiso R . . . . .
H122 H 0.1890 0.3037 0.4948 0.0418 1.0000 Uiso R . . . . .
H121 H 0.0339 0.2301 0.5063 0.0418 1.0000 Uiso R . . . . .
H133 H 0.3082 -0.1683 0.3812 0.0467 1.0000 Uiso R . . . . .
H132 H 0.4456 -0.1060 0.4220 0.0473 1.0000 Uiso R . . . . .
H131 H 0.2737 -0.0892 0.4813 0.0471 1.0000 Uiso R . . . . .
H143 H 0.3663 -0.0037 0.0724 0.0407 1.0000 Uiso R . . . . .
H142 H 0.4128 -0.1181 0.1876 0.0415 1.0000 Uiso R . . . . .
H141 H 0.2272 -0.0856 0.1296 0.0416 1.0000 Uiso R . . . . .
H163 H 0.6246 0.5160 0.4403 0.0609 1.0000 Uiso R . . . . .
H162 H 0.6457 0.5924 0.3155 0.0615 1.0000 Uiso R . . . . .
H161 H 0.7728 0.4435 0.3729 0.0607 1.0000 Uiso R . . . . .
H183 H 0.9190 -0.0305 0.2546 0.0485 1.0000 Uiso R . . . . .
H182 H 0.9077 0.0575 0.1281 0.0502 1.0000 Uiso R . . . . .
H181 H 0.8460 -0.0864 0.1615 0.0502 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.938(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 . O1 . 2.1393(14) yes
Ti1 . O2 . 2.1489(14) yes
Ti1 . O3 . 2.1426(14) yes
Ti1 . O4 . 2.1406(14) yes
Ti1 . C1 . 2.3645(18) yes
Ti1 . C2 . 2.5140(19) yes
Ti1 . C3 . 2.3669(19) yes
Ti1 . C4 . 2.1279(18) yes
Ti1 . C5 . 2.3750(19) yes
Ti1 . C6 . 2.5165(19) yes
Ti1 . C7 . 2.3656(19) yes
Ti1 . C8 . 2.1249(18) yes
Ti1 . C15 . 2.489(2) yes
Ti1 . C17 . 2.482(2) yes
O1 . C15 . 1.267(2) yes
O2 . C15 . 1.271(2) yes
O3 . C17 . 1.270(2) yes
O4 . C17 . 1.263(2) yes
C1 . C2 . 1.417(3) yes
C1 . C8 . 1.440(3) yes
C1 . C9 . 1.503(3) yes
C2 . C3 . 1.415(3) yes
C2 . C10 . 1.496(3) yes
C3 . C4 . 1.447(3) yes
C3 . C11 . 1.502(3) yes
C4 . C5 . 1.441(3) yes
C4 . C8 . 1.456(2) yes
C5 . C6 . 1.417(3) yes
C5 . C12 . 1.502(3) yes
C6 . C7 . 1.416(3) yes
C6 . C13 . 1.501(3) yes
C7 . C8 . 1.444(3) yes
C7 . C14 . 1.499(3) yes
C9 . H93 . 0.946 no
C9 . H92 . 0.965 no
C9 . H91 . 0.943 no
C10 . H103 . 0.940 no
C10 . H102 . 0.925 no
C10 . H101 . 0.960 no
C11 . H113 . 0.943 no
C11 . H112 . 0.975 no
C11 . H111 . 0.951 no
C12 . H123 . 0.987 no
C12 . H122 . 0.969 no
C12 . H121 . 0.969 no
C13 . H133 . 0.926 no
C13 . H132 . 0.961 no
C13 . H131 . 0.944 no
C14 . H143 . 0.965 no
C14 . H142 . 0.968 no
C14 . H141 . 0.972 no
C15 . C16 . 1.500(3) yes
C16 . H163 . 0.948 no
C16 . H162 . 0.952 no
C16 . H161 . 0.945 no
C17 . C18 . 1.495(3) yes
C18 . H183 . 0.970 no
C18 . H182 . 0.971 no
C18 . H181 . 0.943 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Ti1 . O2 . 61.20(5) yes
O1 . Ti1 . O3 . 84.46(6) yes
O2 . Ti1 . O3 . 81.57(6) yes
O1 . Ti1 . O4 . 81.43(6) yes
O2 . Ti1 . O4 . 129.70(5) yes
O3 . Ti1 . O4 . 61.22(5) yes
O1 . Ti1 . C1 . 102.48(6) yes
O2 . Ti1 . C1 . 136.48(6) yes
O3 . Ti1 . C1 . 139.98(6) yes
O4 . Ti1 . C1 . 80.66(6) yes
O1 . Ti1 . C2 . 82.08(6) yes
O2 . Ti1 . C2 . 103.05(6) yes
O3 . Ti1 . C2 . 161.25(6) yes
O4 . Ti1 . C2 . 103.71(6) yes
C1 . Ti1 . C2 . 33.60(6) yes
O1 . Ti1 . C3 . 92.78(6) yes
O2 . Ti1 . C3 . 80.72(6) yes
O3 . Ti1 . C3 . 161.09(6) yes
O4 . Ti1 . C3 . 136.94(6) yes
C1 . Ti1 . C3 . 58.88(6) yes
O1 . Ti1 . C4 . 129.46(7) yes
O2 . Ti1 . C4 . 95.56(6) yes
O3 . Ti1 . C4 . 139.46(7) yes
O4 . Ti1 . C4 . 134.74(6) yes
C1 . Ti1 . C4 . 62.55(7) yes
O1 . Ti1 . C5 . 140.72(6) yes
O2 . Ti1 . C5 . 81.69(6) yes
O3 . Ti1 . C5 . 103.48(6) yes
O4 . Ti1 . C5 . 136.34(6) yes
C1 . Ti1 . C5 . 95.62(7) yes
O1 . Ti1 . C6 . 162.20(6) yes
O2 . Ti1 . C6 . 104.49(6) yes
O3 . Ti1 . C6 . 82.82(6) yes
O4 . Ti1 . C6 . 103.07(6) yes
C1 . Ti1 . C6 . 95.27(7) yes
O1 . Ti1 . C7 . 160.35(6) yes
O2 . Ti1 . C7 . 137.78(6) yes
O3 . Ti1 . C7 . 92.99(6) yes
O4 . Ti1 . C7 . 80.29(6) yes
C1 . Ti1 . C7 . 67.44(7) yes
O1 . Ti1 . C8 . 138.64(7) yes
O2 . Ti1 . C8 . 135.60(6) yes
O3 . Ti1 . C8 . 129.53(7) yes
O4 . Ti1 . C8 . 94.70(6) yes
C1 . Ti1 . C8 . 36.93(7) yes
O1 . Ti1 . C15 . 30.60(6) yes
O2 . Ti1 . C15 . 30.70(6) yes
O3 . Ti1 . C15 . 79.98(6) yes
O4 . Ti1 . C15 . 105.36(6) yes
C1 . Ti1 . C15 . 124.63(7) yes
O1 . Ti1 . C17 . 79.54(6) yes
O2 . Ti1 . C17 . 105.35(6) yes
O3 . Ti1 . C17 . 30.79(6) yes
O4 . Ti1 . C17 . 30.58(6) yes
C1 . Ti1 . C17 . 110.92(7) yes
C2 . Ti1 . C3 . 33.52(6) yes
C2 . Ti1 . C4 . 58.84(7) yes
C3 . Ti1 . C4 . 37.07(7) yes
C2 . Ti1 . C5 . 95.20(7) yes
C3 . Ti1 . C5 . 67.37(7) yes
C4 . Ti1 . C5 . 36.81(7) yes
C2 . Ti1 . C6 . 112.93(6) yes
C3 . Ti1 . C6 . 95.23(7) yes
C4 . Ti1 . C6 . 58.60(7) yes
C5 . Ti1 . C6 . 33.52(6) yes
C2 . Ti1 . C7 . 95.31(7) yes
C3 . Ti1 . C7 . 95.66(7) yes
C4 . Ti1 . C7 . 62.37(7) yes
C5 . Ti1 . C7 . 58.80(7) yes
C6 . Ti1 . C7 . 33.53(6) yes
C2 . Ti1 . C8 . 58.70(7) yes
C3 . Ti1 . C8 . 62.41(7) yes
C4 . Ti1 . C8 . 40.05(7) yes
C5 . Ti1 . C8 . 62.43(7) yes
C6 . Ti1 . C8 . 58.78(7) yes
C2 . Ti1 . C15 . 94.69(7) yes
C3 . Ti1 . C15 . 88.12(7) yes
C4 . Ti1 . C15 . 116.75(7) yes
C5 . Ti1 . C15 . 111.95(7) yes
C6 . Ti1 . C15 . 133.81(7) yes
C2 . Ti1 . C17 . 132.69(7) yes
C3 . Ti1 . C17 . 165.87(7) yes
C4 . Ti1 . C17 . 150.50(7) yes
C5 . Ti1 . C17 . 125.65(7) yes
C6 . Ti1 . C17 . 95.52(6) yes
C7 . Ti1 . C8 . 37.03(7) yes
C7 . Ti1 . C15 . 166.98(7) yes
C8 . Ti1 . C15 . 150.22(7) yes
C7 . Ti1 . C17 . 88.30(6) yes
C8 . Ti1 . C17 . 116.40(7) yes
C15 . Ti1 . C17 . 91.04(6) yes
Ti1 . O1 . C15 . 90.14(12) yes
Ti1 . O2 . C15 . 89.61(11) yes
Ti1 . O3 . C17 . 89.51(11) yes
Ti1 . O4 . C17 . 89.82(11) yes
Ti1 . C1 . C2 . 78.99(11) yes
Ti1 . C1 . C8 . 62.45(10) yes
C2 . C1 . C8 . 107.14(16) yes
Ti1 . C1 . C9 . 125.62(13) yes
C2 . C1 . C9 . 125.41(18) yes
C8 . C1 . C9 . 127.40(17) yes
C1 . C2 . Ti1 . 67.41(10) yes
C1 . C2 . C3 . 110.40(17) yes
Ti1 . C2 . C3 . 67.53(11) yes
C1 . C2 . C10 . 124.53(18) yes
Ti1 . C2 . C10 . 129.33(14) yes
C3 . C2 . C10 . 124.97(18) yes
Ti1 . C3 . C2 . 78.95(11) yes
Ti1 . C3 . C4 . 62.45(10) yes
C2 . C3 . C4 . 107.31(16) yes
Ti1 . C3 . C11 . 125.48(14) yes
C2 . C3 . C11 . 125.23(18) yes
C4 . C3 . C11 . 127.42(18) yes
C3 . C4 . Ti1 . 80.48(11) yes
C3 . C4 . C5 . 131.23(17) yes
Ti1 . C4 . C5 . 80.96(11) yes
C3 . C4 . C8 . 107.20(16) yes
Ti1 . C4 . C8 . 69.87(10) yes
C5 . C4 . C8 . 107.87(16) yes
Ti1 . C5 . C4 . 62.23(10) yes
Ti1 . C5 . C6 . 78.72(11) yes
C4 . C5 . C6 . 107.03(16) yes
Ti1 . C5 . C12 . 126.12(13) yes
C4 . C5 . C12 . 127.18(18) yes
C6 . C5 . C12 . 125.73(18) yes
C5 . C6 . Ti1 . 67.75(10) yes
C5 . C6 . C7 . 110.47(17) yes
Ti1 . C6 . C7 . 67.38(10) yes
C5 . C6 . C13 . 125.28(18) yes
Ti1 . C6 . C13 . 130.23(14) yes
C7 . C6 . C13 . 124.21(18) yes
Ti1 . C7 . C6 . 79.09(11) yes
Ti1 . C7 . C8 . 62.39(10) yes
C6 . C7 . C8 . 107.28(16) yes
Ti1 . C7 . C14 . 126.18(13) yes
C6 . C7 . C14 . 124.87(18) yes
C8 . C7 . C14 . 127.76(18) yes
C4 . C8 . C7 . 107.27(16) yes
C4 . C8 . C1 . 107.85(16) yes
C7 . C8 . C1 . 131.12(17) yes
C4 . C8 . Ti1 . 70.09(10) yes
C7 . C8 . Ti1 . 80.58(11) yes
C1 . C8 . Ti1 . 80.62(11) yes
C1 . C9 . H93 . 110.8 no
C1 . C9 . H92 . 107.9 no
H93 . C9 . H92 . 107.5 no
C1 . C9 . H91 . 110.5 no
H93 . C9 . H91 . 113.2 no
H92 . C9 . H91 . 106.7 no
C2 . C10 . H103 . 114.2 no
C2 . C10 . H102 . 114.6 no
H103 . C10 . H102 . 105.0 no
C2 . C10 . H101 . 111.9 no
H103 . C10 . H101 . 104.7 no
H102 . C10 . H101 . 105.6 no
C3 . C11 . H113 . 111.2 no
C3 . C11 . H112 . 115.6 no
H113 . C11 . H112 . 105.0 no
C3 . C11 . H111 . 113.2 no
H113 . C11 . H111 . 105.6 no
H112 . C11 . H111 . 105.3 no
C5 . C12 . H123 . 109.8 no
C5 . C12 . H122 . 111.2 no
H123 . C12 . H122 . 106.6 no
C5 . C12 . H121 . 112.2 no
H123 . C12 . H121 . 109.1 no
H122 . C12 . H121 . 107.8 no
C6 . C13 . H133 . 112.5 no
C6 . C13 . H132 . 112.0 no
H133 . C13 . H132 . 106.1 no
C6 . C13 . H131 . 110.8 no
H133 . C13 . H131 . 108.8 no
H132 . C13 . H131 . 106.4 no
C7 . C14 . H143 . 110.8 no
C7 . C14 . H142 . 109.7 no
H143 . C14 . H142 . 107.7 no
C7 . C14 . H141 . 108.6 no
H143 . C14 . H141 . 109.9 no
H142 . C14 . H141 . 110.1 no
Ti1 . C15 . O2 . 59.69(10) yes
Ti1 . C15 . O1 . 59.25(10) yes
O2 . C15 . O1 . 118.64(18) yes
Ti1 . C15 . C16 . 173.53(17) yes
O2 . C15 . C16 . 121.12(19) yes
O1 . C15 . C16 . 120.23(19) yes
C15 . C16 . H163 . 113.6 no
C15 . C16 . H162 . 107.0 no
H163 . C16 . H162 . 109.2 no
C15 . C16 . H161 . 110.5 no
H163 . C16 . H161 . 106.6 no
H162 . C16 . H161 . 110.0 no
Ti1 . C17 . O3 . 59.70(10) yes
Ti1 . C17 . O4 . 59.61(10) yes
O3 . C17 . O4 . 118.87(17) yes
Ti1 . C17 . C18 . 171.98(15) yes
O3 . C17 . C18 . 120.30(18) yes
O4 . C17 . C18 . 120.81(18) yes
C17 . C18 . H183 . 111.9 no
C17 . C18 . H182 . 113.9 no
H183 . C18 . H182 . 107.6 no
C17 . C18 . H181 . 111.2 no
H183 . C18 . H181 . 104.4 no
H182 . C18 . H181 . 107.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C9 . H92 . O1 2_665 157.65(5) 0.965 2.600 3.511(3) yes
C12 . H123 . O3 2_656 171.71(6) 0.987 2.599 3.578(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 07/12/11 at 13:48:59
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   9,X'S) H   (  93,X'S) H   (  92,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 103,X'S) H   ( 102,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 113,X'S) H   ( 112,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 123,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 133,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 163,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 183,X'S) H   ( 182,X'S) H   ( 181,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 07/12/11 at 13:48:59
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1063834'
_audit_update_record             
;
2015-05-07 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;
#===================================================

_audit_creation_date             11-12-07
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 106fmc11
_chemical_name_systematic        Pn*Ti(O2CBz)2
_chemical_melting_point          'not measured'

_cell_length_a                   34.4240(6)
_cell_length_b                   8.8424(2)
_cell_length_c                   19.0704(4)
_cell_angle_alpha                90
_cell_angle_beta                 119.2628(9)
_cell_angle_gamma                90
_cell_volume                     5064.08(18)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1 '
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050
1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C30 H32 O4 Ti1 
# Dc =      1.32 Fooo =   2128.00 Mu =      3.72 M =    504.48
# Found Formula = C30 H32 O4 Ti1 
# Dc =      1.32 FOOO =   2128.00 Mu =      3.72 M =    504.48

_chemical_formula_sum            'C30 H32 O4 Ti1'
_chemical_formula_moiety         'C30 H32 O4 Ti1'
_chemical_compound_source        SYN
_chemical_formula_weight         504.48


_cell_measurement_reflns_used    5655
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.400

_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2128
_exptl_absorpt_coefficient_mu    0.372

# Sheldrick geometric approximatio 0.93 0.96 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.96
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            26284
_reflns_number_total             5734
_diffrn_reflns_av_R_equivalents  0.025
# Number of reflections without Friedels Law is 10365 
# Number of reflections with Friedels Law is 5734 
# Theoretical number of reflections is about 5808 


_diffrn_reflns_theta_min         5.122
_diffrn_reflns_theta_max         27.485
_diffrn_measured_fraction_theta_max 0.985

_diffrn_reflns_theta_full        25.011
_diffrn_measured_fraction_theta_full 0.988


_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -44
_reflns_limit_h_max              38
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   2.22
_oxford_diffrn_Wilson_scale      20.16

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.49
_refine_diff_density_max         0.36


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         5733
_refine_ls_number_restraints     0
_refine_ls_number_parameters     316
_oxford_refine_ls_R_factor_ref   0.0570
_refine_ls_wR_factor_ref         0.1143
_refine_ls_goodness_of_fit_ref   0.8969
_refine_ls_shift/su_max          0.0007884
_refine_ls_shift/su_mean         0.0000337


# The values computed from all data 
_oxford_reflns_number_all        5734
_refine_ls_R_factor_all          0.0570
_refine_ls_wR_factor_all         0.1143

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4614
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_gt          0.1005

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 23.5 35.1 17.2 4.40 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.44675(6) 0.4728(2) 0.49549(12) 0.0301 1.0000 Uani . . . . . .
C2 C 0.44137(6) 0.3569(2) 0.44010(12) 0.0297 1.0000 Uani . . . . . .
C3 C 0.44973(6) 0.2130(2) 0.47756(12) 0.0288 1.0000 Uani . . . . . .
C4 C 0.46395(6) 0.2396(2) 0.56170(12) 0.0283 1.0000 Uani . . . . . .
C5 C 0.45265(6) 0.1641(2) 0.61669(12) 0.0302 1.0000 Uani . . . . . .
C6 C 0.44403(7) 0.2784(3) 0.65903(11) 0.0319 1.0000 Uani . . . . . .
C7 C 0.44755(7) 0.4233(3) 0.63169(12) 0.0320 1.0000 Uani . . . . . .
C8 C 0.46129(6) 0.4021(2) 0.57195(12) 0.0296 1.0000 Uani . . . . . .
C9 C 0.43979(7) 0.6391(3) 0.47684(15) 0.0370 1.0000 Uani . . . . . .
C10 C 0.42762(8) 0.3831(3) 0.35372(13) 0.0382 1.0000 Uani . . . . . .
C11 C 0.44581(8) 0.0661(3) 0.43562(13) 0.0352 1.0000 Uani . . . . . .
C12 C 0.45293(8) -0.0033(3) 0.62948(14) 0.0376 1.0000 Uani . . . . . .
C13 C 0.43030(8) 0.2513(3) 0.72181(13) 0.0402 1.0000 Uani . . . . . .
C14 C 0.43956(8) 0.5706(3) 0.66200(14) 0.0418 1.0000 Uani . . . . . .
C15 C 0.34211(6) 0.1318(2) 0.40525(11) 0.0255 1.0000 Uani . . . . . .
C16 C 0.30614(7) 0.0288(2) 0.34618(12) 0.0302 1.0000 Uani . . . . . .
C17 C 0.25980(7) 0.0939(2) 0.31219(12) 0.0266 1.0000 Uani . . . . . .
C18 C 0.24807(7) 0.1834(2) 0.35923(12) 0.0294 1.0000 Uani . . . . . .
C19 C 0.20500(7) 0.2374(2) 0.32876(14) 0.0339 1.0000 Uani . . . . . .
C20 C 0.17313(7) 0.2033(3) 0.24988(14) 0.0350 1.0000 Uani . . . . . .
C21 C 0.18439(7) 0.1153(3) 0.20311(13) 0.0363 1.0000 Uani . . . . . .
C22 C 0.22745(7) 0.0604(3) 0.23395(12) 0.0321 1.0000 Uani . . . . . .
C23 C 0.33515(6) 0.4528(2) 0.51183(11) 0.0276 1.0000 Uani . . . . . .
C24 C 0.29521(7) 0.5395(3) 0.50309(13) 0.0339 1.0000 Uani . . . . . .
C25 C 0.30957(6) 0.6707(2) 0.56145(12) 0.0279 1.0000 Uani . . . . . .
C26 C 0.32500(8) 0.8053(3) 0.54583(13) 0.0360 1.0000 Uani . . . . . .
C27 C 0.33995(9) 0.9223(3) 0.60161(15) 0.0409 1.0000 Uani . . . . . .
C28 C 0.33991(8) 0.9047(3) 0.67357(14) 0.0391 1.0000 Uani . . . . . .
C29 C 0.32442(9) 0.7727(3) 0.68929(14) 0.0409 1.0000 Uani . . . . . .
C30 C 0.30923(8) 0.6568(2) 0.63352(13) 0.0344 1.0000 Uani . . . . . .
Ti1 Ti 0.396258(11) 0.30589(4) 0.509349(19) 0.0233 1.0000 Uani . . . . . .
O1 O 0.34416(4) 0.26897(15) 0.38859(8) 0.0264 1.0000 Uani . . . . . .
O2 O 0.37101(5) 0.08240(15) 0.47381(8) 0.0275 1.0000 Uani . . . . . .
O3 O 0.34252(5) 0.31720(16) 0.53712(8) 0.0282 1.0000 Uani . . . . . .
O4 O 0.36242(5) 0.51409(16) 0.49349(8) 0.0283 1.0000 Uani . . . . . .
H93 H 0.4184 0.6812 0.4885 0.0561 1.0000 Uiso R . . . . .
H91 H 0.4668 0.6936 0.5070 0.0566 1.0000 Uiso R . . . . .
H92 H 0.4293 0.6576 0.4210 0.0570 1.0000 Uiso R . . . . .
H101 H 0.4228 0.2912 0.3246 0.0581 1.0000 Uiso R . . . . .
H103 H 0.4505 0.4372 0.3491 0.0584 1.0000 Uiso R . . . . .
H102 H 0.4014 0.4432 0.3277 0.0583 1.0000 Uiso R . . . . .
H112 H 0.4462 -0.0162 0.4694 0.0525 1.0000 Uiso R . . . . .
H111 H 0.4706 0.0539 0.4248 0.0532 1.0000 Uiso R . . . . .
H113 H 0.4182 0.0641 0.3857 0.0532 1.0000 Uiso R . . . . .
H122 H 0.4407 -0.0283 0.6637 0.0567 1.0000 Uiso R . . . . .
H123 H 0.4824 -0.0410 0.6553 0.0574 1.0000 Uiso R . . . . .
H121 H 0.4366 -0.0566 0.5802 0.0572 1.0000 Uiso R . . . . .
H133 H 0.4043 0.3091 0.7096 0.0611 1.0000 Uiso R . . . . .
H131 H 0.4541 0.2813 0.7740 0.0607 1.0000 Uiso R . . . . .
H132 H 0.4240 0.1463 0.7236 0.0611 1.0000 Uiso R . . . . .
H141 H 0.4379 0.6516 0.6282 0.0631 1.0000 Uiso R . . . . .
H143 H 0.4624 0.5930 0.7163 0.0638 1.0000 Uiso R . . . . .
H142 H 0.4114 0.5665 0.6622 0.0628 1.0000 Uiso R . . . . .
H162 H 0.3080 -0.0660 0.3733 0.0361 1.0000 Uiso R . . . . .
H161 H 0.3126 0.0095 0.3015 0.0366 1.0000 Uiso R . . . . .
H181 H 0.2697 0.2066 0.4127 0.0355 1.0000 Uiso R . . . . .
H191 H 0.1972 0.2970 0.3608 0.0412 1.0000 Uiso R . . . . .
H201 H 0.1437 0.2410 0.2291 0.0423 1.0000 Uiso R . . . . .
H211 H 0.1629 0.0930 0.1501 0.0448 1.0000 Uiso R . . . . .
H221 H 0.2348 -0.0003 0.2019 0.0393 1.0000 Uiso R . . . . .
H241 H 0.2760 0.4706 0.5118 0.0413 1.0000 Uiso R . . . . .
H242 H 0.2799 0.5793 0.4499 0.0411 1.0000 Uiso R . . . . .
H261 H 0.3248 0.8171 0.4961 0.0435 1.0000 Uiso R . . . . .
H271 H 0.3503 1.0128 0.5909 0.0489 1.0000 Uiso R . . . . .
H281 H 0.3503 0.9835 0.7120 0.0478 1.0000 Uiso R . . . . .
H291 H 0.3240 0.7625 0.7373 0.0497 1.0000 Uiso R . . . . .
H301 H 0.2988 0.5669 0.6444 0.0407 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.21886(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.418(3) yes
C1 . C8 . 1.433(3) yes
C1 . C9 . 1.504(3) yes
C1 . Ti1 . 2.391(2) yes
C2 . C3 . 1.418(3) yes
C2 . C10 . 1.493(3) yes
C2 . Ti1 . 2.5229(19) yes
C3 . C4 . 1.450(3) yes
C3 . C11 . 1.497(3) yes
C3 . Ti1 . 2.3496(19) yes
C4 . C5 . 1.448(3) yes
C4 . C8 . 1.459(3) yes
C4 . Ti1 . 2.1202(19) yes
C5 . C6 . 1.413(3) yes
C5 . C12 . 1.500(3) yes
C5 . Ti1 . 2.376(2) yes
C6 . C7 . 1.411(3) yes
C6 . C13 . 1.506(3) yes
C6 . Ti1 . 2.5144(19) yes
C7 . C8 . 1.443(3) yes
C7 . C14 . 1.504(3) yes
C7 . Ti1 . 2.369(2) yes
C8 . Ti1 . 2.1324(19) yes
C9 . H93 . 0.944 no
C9 . H91 . 0.952 no
C9 . H92 . 0.957 no
C10 . H101 . 0.952 no
C10 . H103 . 0.961 no
C10 . H102 . 0.953 no
C11 . H112 . 0.968 no
C11 . H111 . 0.978 no
C11 . H113 . 0.962 no
C12 . H122 . 0.959 no
C12 . H123 . 0.947 no
C12 . H121 . 0.952 no
C13 . H133 . 0.955 no
C13 . H131 . 0.966 no
C13 . H132 . 0.958 no
C14 . H141 . 0.946 no
C14 . H143 . 0.967 no
C14 . H142 . 0.973 no
C15 . C16 . 1.506(3) yes
C15 . Ti1 . 2.484(2) yes
C15 . O1 . 1.265(2) yes
C15 . O2 . 1.272(2) yes
C16 . C17 . 1.512(3) yes
C16 . H162 . 0.970 no
C16 . H161 . 0.995 no
C17 . C18 . 1.396(3) yes
C17 . C22 . 1.389(3) yes
C18 . C19 . 1.386(3) yes
C18 . H181 . 0.945 no
C19 . C20 . 1.394(3) yes
C19 . H191 . 0.941 no
C20 . C21 . 1.375(3) yes
C20 . H201 . 0.951 no
C21 . C22 . 1.388(3) yes
C21 . H211 . 0.936 no
C22 . H221 . 0.937 no
C23 . C24 . 1.510(3) yes
C23 . Ti1 . 2.492(2) yes
C23 . O3 . 1.271(2) yes
C23 . O4 . 1.272(2) yes
C24 . C25 . 1.514(3) yes
C24 . H241 . 0.970 no
C24 . H242 . 0.953 no
C25 . C26 . 1.394(3) yes
C25 . C30 . 1.386(3) yes
C26 . C27 . 1.389(3) yes
C26 . H261 . 0.950 no
C27 . C28 . 1.382(3) yes
C27 . H271 . 0.939 no
C28 . C29 . 1.376(3) yes
C28 . H281 . 0.945 no
C29 . C30 . 1.383(3) yes
C29 . H291 . 0.928 no
C30 . H301 . 0.936 no
Ti1 . O1 . 2.1421(13) yes
Ti1 . O2 . 2.1318(14) yes
Ti1 . O3 . 2.1610(14) yes
Ti1 . O4 . 2.1196(14) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C8 . 107.21(18) yes
C2 . C1 . C9 . 125.65(19) yes
C8 . C1 . C9 . 127.1(2) yes
C2 . C1 . Ti1 . 78.40(12) yes
C8 . C1 . Ti1 . 61.93(10) yes
C9 . C1 . Ti1 . 126.11(14) yes
C1 . C2 . C3 . 110.66(18) yes
C1 . C2 . C10 . 124.5(2) yes
C3 . C2 . C10 . 124.9(2) yes
C1 . C2 . Ti1 . 68.20(11) yes
C3 . C2 . Ti1 . 66.48(10) yes
C10 . C2 . Ti1 . 131.37(14) yes
C2 . C3 . C4 . 106.71(18) yes
C2 . C3 . C11 . 124.50(18) yes
C4 . C3 . C11 . 128.75(19) yes
C2 . C3 . Ti1 . 79.92(12) yes
C4 . C3 . Ti1 . 62.68(10) yes
C11 . C3 . Ti1 . 124.34(14) yes
C3 . C4 . C5 . 131.44(19) yes
C3 . C4 . C8 . 107.40(17) yes
C5 . C4 . C8 . 107.48(17) yes
C3 . C4 . Ti1 . 79.92(11) yes
C5 . C4 . Ti1 . 81.13(11) yes
C8 . C4 . Ti1 . 70.39(11) yes
C4 . C5 . C6 . 106.85(19) yes
C4 . C5 . C12 . 126.2(2) yes
C6 . C5 . C12 . 126.86(19) yes
C4 . C5 . Ti1 . 61.85(10) yes
C6 . C5 . Ti1 . 78.67(12) yes
C12 . C5 . Ti1 . 126.77(15) yes
C5 . C6 . C7 . 111.00(18) yes
C5 . C6 . C13 . 125.1(2) yes
C7 . C6 . C13 . 123.8(2) yes
C5 . C6 . Ti1 . 67.90(11) yes
C7 . C6 . Ti1 . 67.63(11) yes
C13 . C6 . Ti1 . 129.26(14) yes
C6 . C7 . C8 . 107.11(18) yes
C6 . C7 . C14 . 125.4(2) yes
C8 . C7 . C14 . 127.5(2) yes
C6 . C7 . Ti1 . 78.97(12) yes
C8 . C7 . Ti1 . 62.60(10) yes
C14 . C7 . Ti1 . 124.74(15) yes
C4 . C8 . C7 . 107.47(18) yes
C4 . C8 . C1 . 107.88(17) yes
C7 . C8 . C1 . 131.29(19) yes
C4 . C8 . Ti1 . 69.49(11) yes
C7 . C8 . Ti1 . 80.47(11) yes
C1 . C8 . Ti1 . 81.69(12) yes
C1 . C9 . H93 . 112.5 no
C1 . C9 . H91 . 110.9 no
H93 . C9 . H91 . 107.6 no
C1 . C9 . H92 . 111.1 no
H93 . C9 . H92 . 106.3 no
H91 . C9 . H92 . 108.2 no
C2 . C10 . H101 . 112.5 no
C2 . C10 . H103 . 110.3 no
H101 . C10 . H103 . 106.8 no
C2 . C10 . H102 . 111.6 no
H101 . C10 . H102 . 108.7 no
H103 . C10 . H102 . 106.6 no
C3 . C11 . H112 . 109.2 no
C3 . C11 . H111 . 110.4 no
H112 . C11 . H111 . 109.2 no
C3 . C11 . H113 . 109.4 no
H112 . C11 . H113 . 109.3 no
H111 . C11 . H113 . 109.4 no
C5 . C12 . H122 . 111.6 no
C5 . C12 . H123 . 110.6 no
H122 . C12 . H123 . 106.3 no
C5 . C12 . H121 . 112.0 no
H122 . C12 . H121 . 108.3 no
H123 . C12 . H121 . 107.8 no
C6 . C13 . H133 . 109.9 no
C6 . C13 . H131 . 109.8 no
H133 . C13 . H131 . 108.9 no
C6 . C13 . H132 . 110.3 no
H133 . C13 . H132 . 109.0 no
H131 . C13 . H132 . 108.8 no
C7 . C14 . H141 . 110.9 no
C7 . C14 . H143 . 112.5 no
H141 . C14 . H143 . 108.7 no
C7 . C14 . H142 . 109.9 no
H141 . C14 . H142 . 107.5 no
H143 . C14 . H142 . 107.2 no
C16 . C15 . Ti1 . 173.83(13) yes
C16 . C15 . O1 . 121.25(17) yes
Ti1 . C15 . O1 . 59.60(10) yes
C16 . C15 . O2 . 120.32(17) yes
Ti1 . C15 . O2 . 59.13(10) yes
O1 . C15 . O2 . 118.42(17) yes
C15 . C16 . C17 . 113.54(16) yes
C15 . C16 . H162 . 107.9 no
C17 . C16 . H162 . 109.9 no
C15 . C16 . H161 . 107.3 no
C17 . C16 . H161 . 109.2 no
H162 . C16 . H161 . 108.9 no
C16 . C17 . C18 . 121.10(17) yes
C16 . C17 . C22 . 120.19(18) yes
C18 . C17 . C22 . 118.66(19) yes
C17 . C18 . C19 . 120.79(19) yes
C17 . C18 . H181 . 119.6 no
C19 . C18 . H181 . 119.6 no
C18 . C19 . C20 . 119.62(19) yes
C18 . C19 . H191 . 120.5 no
C20 . C19 . H191 . 119.9 no
C19 . C20 . C21 . 120.0(2) yes
C19 . C20 . H201 . 119.4 no
C21 . C20 . H201 . 120.6 no
C20 . C21 . C22 . 120.3(2) yes
C20 . C21 . H211 . 119.8 no
C22 . C21 . H211 . 119.9 no
C17 . C22 . C21 . 120.63(19) yes
C17 . C22 . H221 . 119.5 no
C21 . C22 . H221 . 119.8 no
C24 . C23 . Ti1 . 173.48(14) yes
C24 . C23 . O3 . 121.53(18) yes
Ti1 . C23 . O3 . 60.11(10) yes
C24 . C23 . O4 . 120.49(19) yes
Ti1 . C23 . O4 . 58.25(10) yes
O3 . C23 . O4 . 117.97(18) yes
C23 . C24 . C25 . 110.83(16) yes
C23 . C24 . H241 . 108.7 no
C25 . C24 . H241 . 111.1 no
C23 . C24 . H242 . 107.7 no
C25 . C24 . H242 . 108.2 no
H241 . C24 . H242 . 110.3 no
C24 . C25 . C26 . 121.28(19) yes
C24 . C25 . C30 . 120.19(19) yes
C26 . C25 . C30 . 118.48(19) yes
C25 . C26 . C27 . 120.61(19) yes
C25 . C26 . H261 . 119.3 no
C27 . C26 . H261 . 120.1 no
C26 . C27 . C28 . 119.8(2) yes
C26 . C27 . H271 . 120.4 no
C28 . C27 . H271 . 119.8 no
C27 . C28 . C29 . 120.0(2) yes
C27 . C28 . H281 . 120.2 no
C29 . C28 . H281 . 119.8 no
C28 . C29 . C30 . 120.2(2) yes
C28 . C29 . H291 . 119.5 no
C30 . C29 . H291 . 120.3 no
C25 . C30 . C29 . 120.9(2) yes
C25 . C30 . H301 . 119.0 no
C29 . C30 . H301 . 120.0 no
C3 . Ti1 . C7 . 96.11(7) yes
C3 . Ti1 . C5 . 67.96(7) yes
C7 . Ti1 . C5 . 58.73(8) yes
C3 . Ti1 . C1 . 58.93(7) yes
C7 . Ti1 . C1 . 66.81(7) yes
C5 . Ti1 . C1 . 95.11(7) yes
C3 . Ti1 . C15 . 87.34(7) yes
C7 . Ti1 . C15 . 164.98(7) yes
C5 . Ti1 . C15 . 109.85(7) yes
C1 . Ti1 . C15 . 126.61(7) yes
C3 . Ti1 . C23 . 164.15(7) yes
C7 . Ti1 . C23 . 89.01(7) yes
C5 . Ti1 . C23 . 126.89(7) yes
C1 . Ti1 . C23 . 110.26(7) yes
C15 . Ti1 . C23 . 91.57(6) yes
C3 . Ti1 . C6 . 95.69(7) yes
C7 . Ti1 . C6 . 33.41(7) yes
C5 . Ti1 . C6 . 33.43(7) yes
C1 . Ti1 . C6 . 94.46(7) yes
C15 . Ti1 . C6 . 131.79(7) yes
C3 . Ti1 . C2 . 33.61(7) yes
C7 . Ti1 . C2 . 94.81(7) yes
C5 . Ti1 . C2 . 95.31(7) yes
C1 . Ti1 . C2 . 33.40(7) yes
C15 . Ti1 . C2 . 96.08(6) yes
C3 . Ti1 . C8 . 62.84(7) yes
C7 . Ti1 . C8 . 36.93(7) yes
C5 . Ti1 . C8 . 62.36(8) yes
C1 . Ti1 . C8 . 36.38(7) yes
C15 . Ti1 . C8 . 150.12(7) yes
C3 . Ti1 . C4 . 37.41(7) yes
C7 . Ti1 . C4 . 62.54(8) yes
C5 . Ti1 . C4 . 37.02(7) yes
C1 . Ti1 . C4 . 62.08(8) yes
C15 . Ti1 . C4 . 115.33(7) yes
C3 . Ti1 . O1 . 91.09(6) yes
C7 . Ti1 . O1 . 162.73(7) yes
C5 . Ti1 . O1 . 138.41(7) yes
C1 . Ti1 . O1 . 104.30(6) yes
C15 . Ti1 . O1 . 30.61(6) yes
C3 . Ti1 . O2 . 80.97(6) yes
C7 . Ti1 . O2 . 135.33(7) yes
C5 . Ti1 . O2 . 79.58(6) yes
C1 . Ti1 . O2 . 137.95(6) yes
C15 . Ti1 . O2 . 30.82(6) yes
C3 . Ti1 . O3 . 162.13(7) yes
C7 . Ti1 . O3 . 93.07(6) yes
C5 . Ti1 . O3 . 104.48(6) yes
C1 . Ti1 . O3 . 138.93(6) yes
C15 . Ti1 . O3 . 80.02(6) yes
C3 . Ti1 . O4 . 135.39(6) yes
C7 . Ti1 . O4 . 81.54(7) yes
C5 . Ti1 . O4 . 137.88(7) yes
C1 . Ti1 . O4 . 80.01(6) yes
C15 . Ti1 . O4 . 106.20(6) yes
C23 . Ti1 . C6 . 96.80(7) yes
C23 . Ti1 . C2 . 131.15(7) yes
C6 . Ti1 . C2 . 112.53(7) yes
C23 . Ti1 . C8 . 116.51(7) yes
C6 . Ti1 . C8 . 58.53(7) yes
C2 . Ti1 . C8 . 58.35(7) yes
C23 . Ti1 . C4 . 151.48(7) yes
C6 . Ti1 . C4 . 58.70(7) yes
C2 . Ti1 . C4 . 58.65(7) yes
C8 . Ti1 . C4 . 40.12(8) yes
C23 . Ti1 . O1 . 80.15(6) yes
C6 . Ti1 . O1 . 160.91(6) yes
C2 . Ti1 . O1 . 82.56(6) yes
C8 . Ti1 . O1 . 139.53(7) yes
C4 . Ti1 . O1 . 127.87(7) yes
C23 . Ti1 . O2 . 105.80(6) yes
C6 . Ti1 . O2 . 102.13(6) yes
C2 . Ti1 . O2 . 105.02(6) yes
C8 . Ti1 . O2 . 134.51(7) yes
C4 . Ti1 . O2 . 94.42(7) yes
C23 . Ti1 . O3 . 30.65(6) yes
C6 . Ti1 . O3 . 83.65(6) yes
C2 . Ti1 . O3 . 160.01(6) yes
C8 . Ti1 . O3 . 129.38(7) yes
C4 . Ti1 . O3 . 140.61(7) yes
C23 . Ti1 . O4 . 30.69(6) yes
C6 . Ti1 . O4 . 104.75(6) yes
C2 . Ti1 . O4 . 101.88(6) yes
C8 . Ti1 . O4 . 94.98(7) yes
C4 . Ti1 . O4 . 135.07(7) yes
O1 . Ti1 . O2 . 61.31(5) yes
O1 . Ti1 . O3 . 84.46(5) yes
O2 . Ti1 . O3 . 81.72(5) yes
O1 . Ti1 . O4 . 82.31(5) yes
O2 . Ti1 . O4 . 130.51(5) yes
O3 . Ti1 . O4 . 61.20(5) yes
Ti1 . O1 . C15 . 89.79(11) yes
Ti1 . O2 . C15 . 90.05(11) yes
Ti1 . O3 . C23 . 89.24(11) yes
Ti1 . O4 . C23 . 91.06(12) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C21 . H211 . O4 7_545 154.06(6) 0.936 2.532 3.398(3) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 07/12/11 at 13:56:28
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   9,X'S) H   (  93,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 103,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 112,X'S) H   ( 111,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 123,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 133,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 143,X'S) H   ( 142,X'S) 
RIDE C   (  16,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 07/12/11 at 13:56:28
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
