# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_LitBuPOCOP
_database_code_depnum_ccdc_archive 'CCDC 2204753'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_cell_length_a                   21.9510(7)
_cell_length_b                   14.8413(5)
_cell_length_c                   15.1618(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4939.4(3)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21 '
_symmetry_space_group_name_Hall  'P 2c -2n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z+1/2
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,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 0.0181 0.0091 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'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 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'
Li 0.0008 0.0003 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610
0.0377 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C44 H74 Li2 O4 P4 
# Dc =      1.08 Fooo =   1744.00 Mu =     16.80 M =    804.85
# Found Formula = C44 H78 Li2 O4 P4 
# Dc =      1.09 FOOO =   1760.00 Mu =     16.81 M =    808.88

_chemical_formula_sum            'C44 H78 Li2 O4 P4'
_chemical_formula_moiety         'C44 H78 Li2 O4 P4'
_chemical_compound_source        .
_chemical_formula_weight         808.88


_cell_measurement_reflns_used    1789
_cell_measurement_theta_min      4
_cell_measurement_theta_max      72
_cell_measurement_temperature    173

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_max          0.100

_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1760
_exptl_absorpt_coefficient_mu    1.681

# Sheldrick geometric approximatio 0.85 0.85 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.85
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_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      173
_diffrn_reflns_number            10545
_diffrn_reflns_av_unetI/netI     0.115
_reflns_number_total             7239
_diffrn_reflns_av_R_equivalents  0.063
# Number of reflections without Friedels Law is 7239 
# Number of reflections with Friedels Law is 4978 
# Theoretical number of reflections is about 4959 


_diffrn_reflns_theta_min         3.595
_diffrn_reflns_theta_max         73.278
_diffrn_measured_fraction_theta_max 0.965

_diffrn_reflns_theta_full        73.278
_diffrn_measured_fraction_theta_full 0.965


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              0
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              -18
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.73
_oxford_diffrn_Wilson_scale      0.89

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

_refine_diff_density_min         -0.42
_refine_diff_density_max         0.51


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     1
_refine_ls_number_parameters     487
_refine_ls_number_reflns         7239
_oxford_refine_ls_R_factor_ref   0.0930
_refine_ls_wR_factor_ref         0.1615
_refine_ls_goodness_of_fit_ref   0.9939
_refine_ls_shift/su_max          0.0002180
_refine_ls_shift/su_mean         0.0000138


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        7239
_refine_ls_R_factor_all          0.0930
_refine_ls_wR_factor_all         0.1615

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5360
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_gt          0.1339

# For an explanation, see Cooper & Watkin, Acta Cryst. (2016). B72, 661-683 
_oxford_Hooft_y                  -0.04(4) # for 1943 Friedel pairs 
_oxford_Bijvoet_difference       -0.00(4) # for 1943 Friedel pairs 
# (Similar to the Parsons(q).) 
_refine_ls_abs_structure_Flack   -0.00(4)
_refine_ls_abs_structure_details 
; 
 Parsons, Flack & Wagner (2013), 
 1943 Friedel Pairs 
;

# 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 ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 5.18P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.4560(2) 0.3025(4) 0.2478(4) 0.0324 1.0000 Uani . . . . . .
C2 C 0.4967(3) 0.2366(4) 0.2773(4) 0.0355 1.0000 Uani . . . . . .
C3 C 0.5433(3) 0.2507(4) 0.3381(4) 0.0440 1.0000 Uani . . . . . .
C4 C 0.5507(3) 0.3352(5) 0.3728(4) 0.0462 1.0000 Uani . . . . . .
C5 C 0.5125(3) 0.4043(4) 0.3490(4) 0.0418 1.0000 Uani . . . . . .
C6 C 0.4672(2) 0.3859(4) 0.2876(4) 0.0335 1.0000 Uani . . . . . .
C7 C 0.5529(3) 0.1070(4) 0.0987(5) 0.0458 1.0000 Uani . . . . . .
C8 C 0.5960(3) 0.0437(6) 0.1481(6) 0.0672 1.0000 Uani . . . . . .
C9 C 0.5779(4) 0.2025(6) 0.1005(6) 0.0671 1.0000 Uani . . . . . .
C10 C 0.5468(4) 0.0778(5) 0.0020(5) 0.0597 1.0000 Uani . . . . . .
C11 C 0.4429(3) 0.0032(4) 0.1755(5) 0.0443 1.0000 Uani . . . . . .
C12 C 0.4753(4) -0.0468(5) 0.2503(5) 0.0679 1.0000 Uani . . . . . .
C13 C 0.3770(3) 0.0235(5) 0.2051(6) 0.0667 1.0000 Uani . . . . . .
C14 C 0.4393(4) -0.0546(4) 0.0938(6) 0.0603 1.0000 Uani . . . . . .
C15 C 0.3810(3) 0.6084(4) 0.3394(5) 0.0431 1.0000 Uani . . . . . .
C16 C 0.4001(4) 0.5781(5) 0.4328(5) 0.0602 1.0000 Uani . . . . . .
C17 C 0.3814(3) 0.7119(4) 0.3364(6) 0.0558 1.0000 Uani . . . . . .
C18 C 0.3179(3) 0.5720(5) 0.3216(6) 0.0582 1.0000 Uani . . . . . .
C19 C 0.4338(3) 0.5936(4) 0.1522(5) 0.0492 1.0000 Uani . . . . . .
C20 C 0.4576(4) 0.6902(5) 0.1405(6) 0.0670 1.0000 Uani . . . . . .
C21 C 0.3685(4) 0.5855(6) 0.1170(5) 0.0650 1.0000 Uani . . . . . .
C22 C 0.4752(4) 0.5299(6) 0.1010(5) 0.0661 1.0000 Uani . . . . . .
C23 C 0.3004(3) 0.2481(4) 0.1965(4) 0.0319 1.0000 Uani . . . . . .
C24 C 0.2868(2) 0.2255(4) 0.1088(4) 0.0285 1.0000 Uani . . . . . .
C25 C 0.2420(3) 0.1652(4) 0.0834(4) 0.0413 1.0000 Uani . . . . . .
C26 C 0.2058(3) 0.1248(5) 0.1451(5) 0.0486 1.0000 Uani . . . . . .
C27 C 0.2162(3) 0.1440(4) 0.2338(4) 0.0451 1.0000 Uani . . . . . .
C28 C 0.2624(3) 0.2017(4) 0.2559(4) 0.0333 1.0000 Uani . . . . . .
C29 C 0.3768(3) 0.2318(5) -0.1132(4) 0.0502 1.0000 Uani . . . . . .
C30 C 0.3784(4) 0.1301(5) -0.0952(6) 0.0660 1.0000 Uani . . . . . .
C31 C 0.4357(3) 0.2744(6) -0.0790(6) 0.0652 1.0000 Uani . . . . . .
C32 C 0.3721(4) 0.2469(7) -0.2134(5) 0.0770 1.0000 Uani . . . . . .
C33 C 0.2919(3) 0.3931(4) -0.0795(5) 0.0494 1.0000 Uani . . . . . .
C34 C 0.2487(4) 0.4198(5) -0.0048(7) 0.0770 1.0000 Uani . . . . . .
C35 C 0.3474(4) 0.4537(5) -0.0798(6) 0.0648 1.0000 Uani . . . . . .
C36 C 0.2582(4) 0.4029(6) -0.1682(6) 0.0789 1.0000 Uani . . . . . .
C37 C 0.2281(3) 0.3495(4) 0.4404(5) 0.0419 1.0000 Uani . . . . . .
C38 C 0.1979(3) 0.3914(5) 0.3583(5) 0.0545 1.0000 Uani . . . . . .
C39 C 0.1824(3) 0.2840(5) 0.4818(5) 0.0541 1.0000 Uani . . . . . .
C40 C 0.2440(4) 0.4250(5) 0.5063(5) 0.0589 1.0000 Uani . . . . . .
C41 C 0.3427(3) 0.2380(5) 0.4857(5) 0.0524 1.0000 Uani . . . . . .
C42 C 0.3058(4) 0.1883(5) 0.5541(5) 0.0607 1.0000 Uani . . . . . .
C43 C 0.3836(5) 0.3078(7) 0.5285(7) 0.0914 1.0000 Uani . . . . . .
C44 C 0.3817(4) 0.1680(7) 0.4377(6) 0.0839 1.0000 Uani . . . . . .
P2 P 0.44481(7) 0.56291(9) 0.27051(12) 0.0339 1.0000 Uani . . . . . .
O2 O 0.42344(16) 0.4537(2) 0.2670(3) 0.0337 1.0000 Uani . . . . . .
O1 O 0.49258(19) 0.1456(3) 0.2507(3) 0.0389 1.0000 Uani . . . . . .
P1 P 0.47480(7) 0.11707(10) 0.14909(12) 0.0346 1.0000 Uani . . . . . .
P3 P 0.30415(7) 0.26912(10) -0.06192(12) 0.0362 1.0000 Uani . . . . . .
O3 O 0.32618(17) 0.2657(3) 0.0444(3) 0.0355 1.0000 Uani . . . . . .
O4 O 0.2695(2) 0.2088(3) 0.3483(3) 0.0460 1.0000 Uani . . . . . .
P4 P 0.29950(7) 0.29711(10) 0.39634(12) 0.0353 1.0000 Uani . . . . . .
Li1 Li 0.3967(4) 0.2499(7) 0.1429(7) 0.0374 1.0000 Uani . . . . . .
Li2 Li 0.3593(4) 0.3474(6) 0.2613(7) 0.0361 1.0000 Uani . . . . . .
H31 H 0.5694 0.2034 0.3542 0.0539 1.0000 Uiso R . . . . .
H41 H 0.5816 0.3458 0.4135 0.0572 1.0000 Uiso R . . . . .
H51 H 0.5175 0.4620 0.3737 0.0513 1.0000 Uiso R . . . . .
H81 H 0.5847 -0.0180 0.1358 0.1031 1.0000 Uiso R . . . . .
H82 H 0.6371 0.0542 0.1285 0.1030 1.0000 Uiso R . . . . .
H83 H 0.5923 0.0550 0.2106 0.1028 1.0000 Uiso R . . . . .
H93 H 0.5485 0.2436 0.0765 0.1029 1.0000 Uiso R . . . . .
H92 H 0.6147 0.2061 0.0663 0.1029 1.0000 Uiso R . . . . .
H91 H 0.5865 0.2193 0.1610 0.1032 1.0000 Uiso R . . . . .
H101 H 0.5212 0.1203 -0.0290 0.0901 1.0000 Uiso R . . . . .
H102 H 0.5866 0.0766 -0.0241 0.0899 1.0000 Uiso R . . . . .
H103 H 0.5291 0.0184 -0.0006 0.0899 1.0000 Uiso R . . . . .
H121 H 0.5137 -0.0703 0.2292 0.1038 1.0000 Uiso R . . . . .
H122 H 0.4816 -0.0052 0.2985 0.1041 1.0000 Uiso R . . . . .
H123 H 0.4499 -0.0960 0.2699 0.1039 1.0000 Uiso R . . . . .
H133 H 0.3546 0.0525 0.1582 0.1021 1.0000 Uiso R . . . . .
H132 H 0.3784 0.0628 0.2556 0.1021 1.0000 Uiso R . . . . .
H131 H 0.3567 -0.0312 0.2219 0.1022 1.0000 Uiso R . . . . .
H141 H 0.4256 -0.0183 0.0454 0.0952 1.0000 Uiso R . . . . .
H142 H 0.4787 -0.0789 0.0807 0.0951 1.0000 Uiso R . . . . .
H143 H 0.4112 -0.1034 0.1027 0.0948 1.0000 Uiso R . . . . .
H163 H 0.4025 0.5129 0.4344 0.0911 1.0000 Uiso R . . . . .
H162 H 0.4401 0.6021 0.4474 0.0911 1.0000 Uiso R . . . . .
H161 H 0.3707 0.5984 0.4764 0.0911 1.0000 Uiso R . . . . .
H171 H 0.3653 0.7318 0.2809 0.0878 1.0000 Uiso R . . . . .
H172 H 0.4228 0.7342 0.3429 0.0880 1.0000 Uiso R . . . . .
H173 H 0.3562 0.7356 0.3831 0.0879 1.0000 Uiso R . . . . .
H181 H 0.3059 0.5915 0.2632 0.0911 1.0000 Uiso R . . . . .
H182 H 0.2896 0.5949 0.3650 0.0911 1.0000 Uiso R . . . . .
H183 H 0.3190 0.5070 0.3244 0.0908 1.0000 Uiso R . . . . .
H203 H 0.4974 0.6952 0.1674 0.1029 1.0000 Uiso R . . . . .
H202 H 0.4296 0.7319 0.1679 0.1031 1.0000 Uiso R . . . . .
H201 H 0.4609 0.7041 0.0786 0.1029 1.0000 Uiso R . . . . .
H211 H 0.3511 0.5282 0.1342 0.0970 1.0000 Uiso R . . . . .
H212 H 0.3423 0.6332 0.1395 0.0971 1.0000 Uiso R . . . . .
H213 H 0.3689 0.5891 0.0533 0.0971 1.0000 Uiso R . . . . .
H221 H 0.4616 0.4691 0.1094 0.1040 1.0000 Uiso R . . . . .
H222 H 0.5164 0.5360 0.1240 0.1038 1.0000 Uiso R . . . . .
H223 H 0.4741 0.5451 0.0390 0.1038 1.0000 Uiso R . . . . .
H251 H 0.2368 0.1513 0.0234 0.0501 1.0000 Uiso R . . . . .
H261 H 0.1750 0.0854 0.1280 0.0600 1.0000 Uiso R . . . . .
H271 H 0.1920 0.1172 0.2777 0.0562 1.0000 Uiso R . . . . .
H301 H 0.3415 0.1030 -0.1185 0.0961 1.0000 Uiso R . . . . .
H302 H 0.4141 0.1036 -0.1233 0.0961 1.0000 Uiso R . . . . .
H303 H 0.3805 0.1194 -0.0321 0.0961 1.0000 Uiso R . . . . .
H313 H 0.4361 0.3377 -0.0927 0.0980 1.0000 Uiso R . . . . .
H312 H 0.4706 0.2463 -0.1058 0.0980 1.0000 Uiso R . . . . .
H311 H 0.4384 0.2670 -0.0160 0.0980 1.0000 Uiso R . . . . .
H321 H 0.3730 0.3103 -0.2249 0.1210 1.0000 Uiso R . . . . .
H322 H 0.4057 0.2175 -0.2423 0.1209 1.0000 Uiso R . . . . .
H323 H 0.3342 0.2223 -0.2344 0.1209 1.0000 Uiso R . . . . .
H341 H 0.2150 0.3778 -0.0037 0.1179 1.0000 Uiso R . . . . .
H342 H 0.2334 0.4794 -0.0146 0.1179 1.0000 Uiso R . . . . .
H343 H 0.2701 0.4182 0.0505 0.1180 1.0000 Uiso R . . . . .
H353 H 0.3708 0.4425 -0.1327 0.1002 1.0000 Uiso R . . . . .
H352 H 0.3338 0.5153 -0.0789 0.0998 1.0000 Uiso R . . . . .
H351 H 0.3719 0.4423 -0.0280 0.0999 1.0000 Uiso R . . . . .
H361 H 0.2845 0.3817 -0.2142 0.1211 1.0000 Uiso R . . . . .
H362 H 0.2487 0.4655 -0.1769 0.1211 1.0000 Uiso R . . . . .
H363 H 0.2212 0.3682 -0.1671 0.1210 1.0000 Uiso R . . . . .
H383 H 0.2254 0.4347 0.3323 0.0839 1.0000 Uiso R . . . . .
H382 H 0.1605 0.4213 0.3745 0.0836 1.0000 Uiso R . . . . .
H381 H 0.1888 0.3455 0.3158 0.0842 1.0000 Uiso R . . . . .
H391 H 0.1966 0.2672 0.5401 0.0838 1.0000 Uiso R . . . . .
H392 H 0.1424 0.3115 0.4862 0.0840 1.0000 Uiso R . . . . .
H393 H 0.1802 0.2307 0.4455 0.0838 1.0000 Uiso R . . . . .
H401 H 0.2614 0.3984 0.5590 0.0902 1.0000 Uiso R . . . . .
H402 H 0.2731 0.4646 0.4788 0.0900 1.0000 Uiso R . . . . .
H403 H 0.2072 0.4580 0.5212 0.0901 1.0000 Uiso R . . . . .
H423 H 0.2786 0.1475 0.5246 0.0932 1.0000 Uiso R . . . . .
H422 H 0.3329 0.1555 0.5921 0.0931 1.0000 Uiso R . . . . .
H421 H 0.2823 0.2306 0.5881 0.0930 1.0000 Uiso R . . . . .
H431 H 0.4017 0.3446 0.4838 0.1291 1.0000 Uiso R . . . . .
H432 H 0.4157 0.2784 0.5612 0.1291 1.0000 Uiso R . . . . .
H433 H 0.3585 0.3441 0.5671 0.1290 1.0000 Uiso R . . . . .
H441 H 0.4001 0.1938 0.3856 0.1260 1.0000 Uiso R . . . . .
H442 H 0.4133 0.1460 0.4765 0.1258 1.0000 Uiso R . . . . .
H443 H 0.3551 0.1192 0.4212 0.1262 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.099(5)
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 . 1.398(8) yes
C1 . C6 . 1.399(8) yes
C1 . Li1 . 2.197(11) yes
C2 . C3 . 1.393(8) yes
C2 . O1 . 1.412(7) yes
C3 . C4 . 1.370(9) yes
C3 . H31 . 0.939 no
C4 . C5 . 1.373(9) yes
C4 . H41 . 0.930 no
C5 . C6 . 1.389(8) yes
C5 . H51 . 0.941 no
C6 . O2 . 1.426(7) yes
C7 . C8 . 1.529(10) yes
C7 . C9 . 1.520(10) yes
C7 . C10 . 1.535(10) yes
C7 . P1 . 1.883(7) yes
C8 . H81 . 0.967 no
C8 . H82 . 0.962 no
C8 . H83 . 0.966 no
C9 . H93 . 0.958 no
C9 . H92 . 0.962 no
C9 . H91 . 0.968 no
C10 . H101 . 0.966 no
C10 . H102 . 0.959 no
C10 . H103 . 0.964 no
C11 . C12 . 1.531(10) yes
C11 . C13 . 1.546(10) yes
C11 . C14 . 1.508(10) yes
C11 . P1 . 1.872(6) yes
C12 . H121 . 0.967 no
C12 . H122 . 0.967 no
C12 . H123 . 0.965 no
C13 . H133 . 0.965 no
C13 . H132 . 0.963 no
C13 . H131 . 0.961 no
C14 . H141 . 0.960 no
C14 . H142 . 0.958 no
C14 . H143 . 0.962 no
C15 . C16 . 1.544(11) yes
C15 . C17 . 1.536(9) yes
C15 . C18 . 1.510(9) yes
C15 . P2 . 1.873(6) yes
C16 . H163 . 0.969 no
C16 . H162 . 0.973 no
C16 . H161 . 0.971 no
C17 . H171 . 0.960 no
C17 . H172 . 0.971 no
C17 . H173 . 0.964 no
C18 . H181 . 0.967 no
C18 . H182 . 0.966 no
C18 . H183 . 0.966 no
C19 . C20 . 1.536(9) yes
C19 . C21 . 1.535(10) yes
C19 . C22 . 1.524(10) yes
C19 . P2 . 1.866(7) yes
C20 . H203 . 0.966 no
C20 . H202 . 0.967 no
C20 . H201 . 0.963 no
C21 . H211 . 0.968 no
C21 . H212 . 0.973 no
C21 . H213 . 0.967 no
C22 . H221 . 0.960 no
C22 . H222 . 0.974 no
C22 . H223 . 0.967 no
C23 . C24 . 1.403(8) yes
C23 . C28 . 1.410(8) yes
C23 . Li2 . 2.192(11) yes
C24 . C25 . 1.385(8) yes
C24 . O3 . 1.434(6) yes
C25 . C26 . 1.366(9) yes
C25 . H251 . 0.940 no
C26 . C27 . 1.392(10) yes
C26 . H261 . 0.931 no
C27 . C28 . 1.369(9) yes
C27 . H271 . 0.940 no
C28 . O4 . 1.413(7) yes
C29 . C30 . 1.534(10) yes
C29 . C31 . 1.530(10) yes
C29 . C32 . 1.539(10) yes
C29 . P3 . 1.859(7) yes
C30 . H301 . 0.971 no
C30 . H302 . 0.974 no
C30 . H303 . 0.972 no
C31 . H313 . 0.962 no
C31 . H312 . 0.961 no
C31 . H311 . 0.963 no
C32 . H321 . 0.958 no
C32 . H322 . 0.964 no
C32 . H323 . 0.962 no
C33 . C34 . 1.528(11) yes
C33 . C35 . 1.515(10) yes
C33 . C36 . 1.541(11) yes
C33 . P3 . 1.879(6) yes
C34 . H341 . 0.968 no
C34 . H342 . 0.958 no
C34 . H343 . 0.962 no
C35 . H353 . 0.967 no
C35 . H352 . 0.961 no
C35 . H351 . 0.967 no
C36 . H361 . 0.958 no
C36 . H362 . 0.961 no
C36 . H363 . 0.962 no
C37 . C38 . 1.542(10) yes
C37 . C39 . 1.532(9) yes
C37 . C40 . 1.542(9) yes
C37 . P4 . 1.872(6) yes
C38 . H383 . 0.967 no
C38 . H382 . 0.964 no
C38 . H381 . 0.959 no
C39 . H391 . 0.970 no
C39 . H392 . 0.971 no
C39 . H393 . 0.964 no
C40 . H401 . 0.970 no
C40 . H402 . 0.964 no
C40 . H403 . 0.970 no
C41 . C42 . 1.509(10) yes
C41 . C43 . 1.516(12) yes
C41 . C44 . 1.530(12) yes
C41 . P4 . 1.872(7) yes
C42 . H423 . 0.961 no
C42 . H422 . 0.961 no
C42 . H421 . 0.962 no
C43 . H431 . 0.955 no
C43 . H432 . 0.966 no
C43 . H433 . 0.969 no
C44 . H441 . 0.966 no
C44 . H442 . 0.967 no
C44 . H443 . 0.963 no
P2 . O2 . 1.689(4) yes
O2 . Li2 . 2.116(9) yes
O1 . P1 . 1.644(4) yes
P1 . Li1 . 2.614(9) yes
P3 . O3 . 1.684(4) yes
O3 . Li1 . 2.164(10) yes
O4 . P4 . 1.638(5) yes
P4 . Li2 . 2.544(10) 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 . C6 . 111.6(5) yes
C2 . C1 . Li1 . 111.2(5) yes
C6 . C1 . Li1 . 137.0(5) yes
C1 . C2 . C3 . 125.2(5) yes
C1 . C2 . O1 . 122.5(5) yes
C3 . C2 . O1 . 112.3(5) yes
C2 . C3 . C4 . 118.6(5) yes
C2 . C3 . H31 . 120.6 no
C4 . C3 . H31 . 120.8 no
C3 . C4 . C5 . 120.7(6) yes
C3 . C4 . H41 . 119.7 no
C5 . C4 . H41 . 119.5 no
C4 . C5 . C6 . 117.7(6) yes
C4 . C5 . H51 . 120.3 no
C6 . C5 . H51 . 122.0 no
C1 . C6 . C5 . 126.2(5) yes
C1 . C6 . O2 . 114.2(5) yes
C5 . C6 . O2 . 119.4(5) yes
C8 . C7 . C9 . 110.0(7) yes
C8 . C7 . C10 . 110.4(6) yes
C9 . C7 . C10 . 108.2(6) yes
C8 . C7 . P1 . 114.4(5) yes
C9 . C7 . P1 . 104.3(5) yes
C10 . C7 . P1 . 109.3(5) yes
C7 . C8 . H81 . 109.2 no
C7 . C8 . H82 . 109.2 no
H81 . C8 . H82 . 109.5 no
C7 . C8 . H83 . 108.7 no
H81 . C8 . H83 . 109.3 no
H82 . C8 . H83 . 110.8 no
C7 . C9 . H93 . 110.2 no
C7 . C9 . H92 . 110.1 no
H93 . C9 . H92 . 108.9 no
C7 . C9 . H91 . 109.1 no
H93 . C9 . H91 . 109.2 no
H92 . C9 . H91 . 109.4 no
C7 . C10 . H101 . 109.4 no
C7 . C10 . H102 . 108.7 no
H101 . C10 . H102 . 109.9 no
C7 . C10 . H103 . 109.4 no
H101 . C10 . H103 . 110.0 no
H102 . C10 . H103 . 109.4 no
C12 . C11 . C13 . 108.3(7) yes
C12 . C11 . C14 . 110.9(6) yes
C13 . C11 . C14 . 107.5(6) yes
C12 . C11 . P1 . 115.0(5) yes
C13 . C11 . P1 . 103.7(5) yes
C14 . C11 . P1 . 111.0(5) yes
C11 . C12 . H121 . 109.5 no
C11 . C12 . H122 . 108.4 no
H121 . C12 . H122 . 110.8 no
C11 . C12 . H123 . 109.1 no
H121 . C12 . H123 . 109.5 no
H122 . C12 . H123 . 109.4 no
C11 . C13 . H133 . 110.5 no
C11 . C13 . H132 . 108.6 no
H133 . C13 . H132 . 109.5 no
C11 . C13 . H131 . 110.3 no
H133 . C13 . H131 . 109.7 no
H132 . C13 . H131 . 108.3 no
C11 . C14 . H141 . 109.0 no
C11 . C14 . H142 . 109.7 no
H141 . C14 . H142 . 109.6 no
C11 . C14 . H143 . 110.3 no
H141 . C14 . H143 . 109.2 no
H142 . C14 . H143 . 109.0 no
C16 . C15 . C17 . 108.4(6) yes
C16 . C15 . C18 . 108.0(6) yes
C17 . C15 . C18 . 111.0(6) yes
C16 . C15 . P2 . 101.8(4) yes
C17 . C15 . P2 . 109.8(5) yes
C18 . C15 . P2 . 117.2(5) yes
C15 . C16 . H163 . 109.1 no
C15 . C16 . H162 . 110.3 no
H163 . C16 . H162 . 108.1 no
C15 . C16 . H161 . 110.7 no
H163 . C16 . H161 . 109.2 no
H162 . C16 . H161 . 109.4 no
C15 . C17 . H171 . 109.4 no
C15 . C17 . H172 . 110.1 no
H171 . C17 . H172 . 109.1 no
C15 . C17 . H173 . 109.9 no
H171 . C17 . H173 . 108.6 no
H172 . C17 . H173 . 109.7 no
C15 . C18 . H181 . 107.9 no
C15 . C18 . H182 . 110.0 no
H181 . C18 . H182 . 110.0 no
C15 . C18 . H183 . 109.0 no
H181 . C18 . H183 . 110.2 no
H182 . C18 . H183 . 109.7 no
C20 . C19 . C21 . 110.5(6) yes
C20 . C19 . C22 . 108.4(6) yes
C21 . C19 . C22 . 109.3(7) yes
C20 . C19 . P2 . 107.2(5) yes
C21 . C19 . P2 . 115.9(5) yes
C22 . C19 . P2 . 105.1(5) yes
C19 . C20 . H203 . 109.3 no
C19 . C20 . H202 . 109.3 no
H203 . C20 . H202 . 110.1 no
C19 . C20 . H201 . 109.8 no
H203 . C20 . H201 . 109.0 no
H202 . C20 . H201 . 109.3 no
C19 . C21 . H211 . 110.1 no
C19 . C21 . H212 . 111.8 no
H211 . C21 . H212 . 108.2 no
C19 . C21 . H213 . 109.5 no
H211 . C21 . H213 . 108.8 no
H212 . C21 . H213 . 108.5 no
C19 . C22 . H221 . 109.2 no
C19 . C22 . H222 . 108.3 no
H221 . C22 . H222 . 109.3 no
C19 . C22 . H223 . 109.6 no
H221 . C22 . H223 . 109.9 no
H222 . C22 . H223 . 110.5 no
C24 . C23 . C28 . 111.2(5) yes
C24 . C23 . Li2 . 135.3(5) yes
C28 . C23 . Li2 . 113.0(5) yes
C23 . C24 . C25 . 124.7(5) yes
C23 . C24 . O3 . 114.6(4) yes
C25 . C24 . O3 . 120.5(5) yes
C24 . C25 . C26 . 120.4(6) yes
C24 . C25 . H251 . 119.8 no
C26 . C25 . H251 . 119.8 no
C25 . C26 . C27 . 118.5(6) yes
C25 . C26 . H261 . 120.4 no
C27 . C26 . H261 . 121.1 no
C26 . C27 . C28 . 119.0(6) yes
C26 . C27 . H271 . 120.4 no
C28 . C27 . H271 . 120.6 no
C23 . C28 . C27 . 126.0(5) yes
C23 . C28 . O4 . 122.1(5) yes
C27 . C28 . O4 . 111.8(5) yes
C30 . C29 . C31 . 109.1(6) yes
C30 . C29 . C32 . 108.7(7) yes
C31 . C29 . C32 . 109.4(7) yes
C30 . C29 . P3 . 103.8(5) yes
C31 . C29 . P3 . 117.4(5) yes
C32 . C29 . P3 . 108.2(6) yes
C29 . C30 . H301 . 108.9 no
C29 . C30 . H302 . 109.7 no
H301 . C30 . H302 . 110.1 no
C29 . C30 . H303 . 109.8 no
H301 . C30 . H303 . 109.2 no
H302 . C30 . H303 . 109.1 no
C29 . C31 . H313 . 109.8 no
C29 . C31 . H312 . 110.5 no
H313 . C31 . H312 . 109.0 no
C29 . C31 . H311 . 109.9 no
H313 . C31 . H311 . 109.0 no
H312 . C31 . H311 . 108.7 no
C29 . C32 . H321 . 108.7 no
C29 . C32 . H322 . 109.4 no
H321 . C32 . H322 . 110.2 no
C29 . C32 . H323 . 109.3 no
H321 . C32 . H323 . 109.3 no
H322 . C32 . H323 . 109.8 no
C34 . C33 . C35 . 110.3(7) yes
C34 . C33 . C36 . 108.9(7) yes
C35 . C33 . C36 . 109.1(6) yes
C34 . C33 . P3 . 103.8(5) yes
C35 . C33 . P3 . 117.8(5) yes
C36 . C33 . P3 . 106.6(5) yes
C33 . C34 . H341 . 108.7 no
C33 . C34 . H342 . 110.0 no
H341 . C34 . H342 . 109.2 no
C33 . C34 . H343 . 109.7 no
H341 . C34 . H343 . 110.0 no
H342 . C34 . H343 . 109.2 no
C33 . C35 . H353 . 109.2 no
C33 . C35 . H352 . 108.4 no
H353 . C35 . H352 . 109.9 no
C33 . C35 . H351 . 109.9 no
H353 . C35 . H351 . 110.3 no
H352 . C35 . H351 . 109.1 no
C33 . C36 . H361 . 108.4 no
C33 . C36 . H362 . 108.4 no
H361 . C36 . H362 . 110.3 no
C33 . C36 . H363 . 109.9 no
H361 . C36 . H363 . 110.1 no
H362 . C36 . H363 . 109.8 no
C38 . C37 . C39 . 107.8(5) yes
C38 . C37 . C40 . 109.1(6) yes
C39 . C37 . C40 . 110.1(6) yes
C38 . C37 . P4 . 103.9(5) yes
C39 . C37 . P4 . 115.5(5) yes
C40 . C37 . P4 . 110.1(4) yes
C37 . C38 . H383 . 109.1 no
C37 . C38 . H382 . 110.2 no
H383 . C38 . H382 . 109.4 no
C37 . C38 . H381 . 110.2 no
H383 . C38 . H381 . 109.1 no
H382 . C38 . H381 . 108.8 no
C37 . C39 . H391 . 109.0 no
C37 . C39 . H392 . 110.7 no
H391 . C39 . H392 . 109.7 no
C37 . C39 . H393 . 108.7 no
H391 . C39 . H393 . 109.0 no
H392 . C39 . H393 . 109.8 no
C37 . C40 . H401 . 109.2 no
C37 . C40 . H402 . 108.2 no
H401 . C40 . H402 . 110.0 no
C37 . C40 . H403 . 109.3 no
H401 . C40 . H403 . 110.0 no
H402 . C40 . H403 . 110.2 no
C42 . C41 . C43 . 111.0(7) yes
C42 . C41 . C44 . 107.2(7) yes
C43 . C41 . C44 . 109.7(8) yes
C42 . C41 . P4 . 117.0(5) yes
C43 . C41 . P4 . 106.8(6) yes
C44 . C41 . P4 . 104.9(5) yes
C41 . C42 . H423 . 108.8 no
C41 . C42 . H422 . 109.1 no
H423 . C42 . H422 . 110.1 no
C41 . C42 . H421 . 109.7 no
H423 . C42 . H421 . 109.2 no
H422 . C42 . H421 . 109.9 no
C41 . C43 . H431 . 109.5 no
C41 . C43 . H432 . 110.0 no
H431 . C43 . H432 . 108.8 no
C41 . C43 . H433 . 107.5 no
H431 . C43 . H433 . 110.3 no
H432 . C43 . H433 . 110.8 no
C41 . C44 . H441 . 110.6 no
C41 . C44 . H442 . 109.9 no
H441 . C44 . H442 . 109.3 no
C41 . C44 . H443 . 107.2 no
H441 . C44 . H443 . 110.0 no
H442 . C44 . H443 . 109.9 no
C15 . P2 . C19 . 110.5(3) yes
C15 . P2 . O2 . 99.0(2) yes
C19 . P2 . O2 . 99.7(3) yes
C6 . O2 . P2 . 118.9(3) yes
C6 . O2 . Li2 . 86.1(4) yes
P2 . O2 . Li2 . 154.4(3) yes
C2 . O1 . P1 . 122.0(4) yes
C7 . P1 . C11 . 110.8(3) yes
C7 . P1 . O1 . 100.6(3) yes
C11 . P1 . O1 . 97.0(3) yes
C7 . P1 . Li1 . 130.0(3) yes
C11 . P1 . Li1 . 116.3(3) yes
O1 . P1 . Li1 . 89.7(3) yes
C33 . P3 . C29 . 110.8(3) yes
C33 . P3 . O3 . 101.9(3) yes
C29 . P3 . O3 . 98.3(3) yes
C24 . O3 . P3 . 119.5(3) yes
C24 . O3 . Li1 . 85.2(4) yes
P3 . O3 . Li1 . 150.4(3) yes
C28 . O4 . P4 . 123.0(4) yes
C41 . P4 . C37 . 111.1(3) yes
C41 . P4 . O4 . 98.7(3) yes
C37 . P4 . O4 . 98.8(3) yes
C41 . P4 . Li2 . 117.3(3) yes
C37 . P4 . Li2 . 126.6(3) yes
O4 . P4 . Li2 . 94.9(3) yes
C1 . Li1 . O3 . 152.2(5) yes
C1 . Li1 . P1 . 81.6(3) yes
O3 . Li1 . P1 . 125.1(4) yes
C23 . Li2 . O2 . 155.7(6) yes
C23 . Li2 . P4 . 81.9(3) yes
O2 . Li2 . P4 . 121.9(4) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 


# start Validation Reply Form
_vrf_PLAT340_LitBuPOCOP          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01003 Ang.  
RESPONSE: This is due to somewhat weakly diffracting
crystals and a drop off in high angle data
(reflected in an elevated wR2 value as well).
;
# end Validation Reply Form

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 2204757'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;


_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   14.0280(2)
_cell_length_b                   12.6260(3)
_cell_length_c                   15.6016(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.8481(16)
_cell_angle_gamma                90
_cell_volume                     2763.01(9)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_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
C 0.0181 0.0091 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 0.0492 0.0322 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'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ti 0.2191 1.8069 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            4

# Given Formula = C24 H45 O2 P2 Ti1 
# Dc =      1.14 Fooo =   1028.00 Mu =     38.30 M =    475.47
# Found Formula = C24 H45 O2 P2 Ti1 
# Dc =      1.14 FOOO =   1028.00 Mu =     38.30 M =    475.47

_chemical_formula_sum            'C24 H45 O2 P2 Ti1'
_chemical_formula_moiety         'C24 H45 O2 P2 Ti1'
_chemical_compound_source        .
_chemical_formula_weight         475.47


_cell_measurement_reflns_used    4014
_cell_measurement_theta_min      4
_cell_measurement_theta_max      73
_cell_measurement_temperature    173

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear intense blue'
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.300

_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1028
_exptl_absorpt_coefficient_mu    3.830

# Sheldrick geometric approximatio 0.46 0.68 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_T_max  0.68
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_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      173
_diffrn_reflns_number            8480
_diffrn_reflns_av_unetI/netI     0.059
_reflns_number_total             5250
_diffrn_reflns_av_R_equivalents  0.034
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 5250 
# Theoretical number of reflections is about 11180 


_diffrn_reflns_theta_min         4.207
_diffrn_reflns_theta_max         73.775
_diffrn_measured_fraction_theta_max 0.940

_diffrn_reflns_theta_full        73.775

_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -17
_reflns_limit_h_max              17
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   1.85
_oxford_diffrn_Wilson_scale      0.07

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

_refine_diff_density_min         -0.65
_refine_diff_density_max         0.58


# 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_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     425
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5248
_oxford_refine_ls_R_factor_ref   0.0534
_refine_ls_wR_factor_ref         0.0571
_refine_ls_goodness_of_fit_ref   1.0364
_refine_ls_shift/su_max          0.0099086
_refine_ls_shift/su_mean         0.0010220


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        5248
_refine_ls_R_factor_all          0.0534
_refine_ls_wR_factor_all         0.0571

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4260
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_gt          0.0451


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method = Chebychev polynomial, (Carruthers & Watkin, 1979) 
 W = 1.0/[A[0]*T[0]'(X)+A[1]*T[1]'(X) ... +A[NP-1]*T[NP-1]'(X)] 
 300. 386. 157. 
;

# 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 0.9229(3) 0.2430(3) 0.5811(3) 0.0446 1.0000 Uani . . . . . .
C2 C 0.8646(3) 0.1075(3) 0.4099(3) 0.0482 1.0000 Uani . . . . . .
C3 C 0.6532(2) 0.2334(2) 0.56021(17) 0.0202 1.0000 Uani . . . . . .
C4 C 0.6071(2) 0.1767(2) 0.62426(17) 0.0207 1.0000 Uani . . . . . .
C5 C 0.5269(2) 0.2106(3) 0.66737(19) 0.0253 1.0000 Uani . . . . . .
C6 C 0.4861(2) 0.3067(3) 0.64396(19) 0.0271 1.0000 Uani . . . . . .
C7 C 0.5256(2) 0.3668(3) 0.57947(18) 0.0255 1.0000 Uani . . . . . .
C8 C 0.6073(2) 0.3297(2) 0.54052(18) 0.0215 1.0000 Uani . . . . . .
C9 C 0.8045(2) -0.0151(3) 0.6991(2) 0.0301 1.0000 Uani . . . . . .
C10 C 0.8156(3) 0.0831(3) 0.7570(2) 0.0415 1.0000 Uani . . . . . .
C11 C 0.9031(2) -0.0503(3) 0.6692(2) 0.0423 1.0000 Uani . . . . . .
C12 C 0.7567(3) -0.1032(3) 0.7501(2) 0.0426 1.0000 Uani . . . . . .
C13 C 0.6820(2) -0.0820(3) 0.5412(2) 0.0329 1.0000 Uani . . . . . .
C14 C 0.6356(3) -0.0281(3) 0.4633(2) 0.0429 1.0000 Uani . . . . . .
C15 C 0.7590(3) -0.1580(3) 0.5111(3) 0.0508 1.0000 Uani . . . . . .
C16 C 0.6043(3) -0.1424(3) 0.5889(2) 0.0464 1.0000 Uani . . . . . .
C17 C 0.8118(2) 0.4770(3) 0.4281(2) 0.0291 1.0000 Uani . . . . . .
C18 C 0.8227(3) 0.5061(3) 0.5237(2) 0.0421 1.0000 Uani . . . . . .
C19 C 0.7689(3) 0.5727(3) 0.3812(2) 0.0402 1.0000 Uani . . . . . .
C20 C 0.9107(2) 0.4516(3) 0.3921(3) 0.0442 1.0000 Uani . . . . . .
C21 C 0.6835(2) 0.3307(3) 0.3169(2) 0.0302 1.0000 Uani . . . . . .
C22 C 0.6075(3) 0.4113(3) 0.2901(2) 0.0445 1.0000 Uani . . . . . .
C23 C 0.7613(3) 0.3245(3) 0.2497(2) 0.0420 1.0000 Uani . . . . . .
C24 C 0.6347(3) 0.2223(3) 0.3241(2) 0.0405 1.0000 Uani . . . . . .
Ti1 Ti 0.79821(4) 0.19040(4) 0.51295(3) 0.0231 1.0000 Uani . . . . . .
P1 P 0.73547(5) 0.03040(6) 0.60347(5) 0.0222 1.0000 Uani . . . . . .
O1 O 0.63978(15) 0.07714(17) 0.65010(14) 0.0285 1.0000 Uani . . . . . .
O2 O 0.64333(14) 0.39585(17) 0.47668(13) 0.0260 1.0000 Uani . . . . . .
P2 P 0.73772(5) 0.35476(6) 0.42549(5) 0.0226 1.0000 Uani . . . . . .
H51 H 0.5024 0.1703 0.7107 0.0299 1.0000 Uiso R . . . . .
H61 H 0.4310 0.3299 0.6725 0.0330 1.0000 Uiso R . . . . .
H71 H 0.4987 0.4309 0.5622 0.0308 1.0000 Uiso R . . . . .
H101 H 0.7541 0.1037 0.7780 0.0616 1.0000 Uiso R . . . . .
H102 H 0.8569 0.0655 0.8040 0.0618 1.0000 Uiso R . . . . .
H103 H 0.8430 0.1413 0.7261 0.0615 1.0000 Uiso R . . . . .
H113 H 0.8968 -0.1141 0.6349 0.0639 1.0000 Uiso R . . . . .
H112 H 0.9430 -0.0651 0.7187 0.0637 1.0000 Uiso R . . . . .
H111 H 0.9335 0.0040 0.6347 0.0640 1.0000 Uiso R . . . . .
H121 H 0.7557 -0.1670 0.7164 0.0636 1.0000 Uiso R . . . . .
H122 H 0.7922 -0.1155 0.8021 0.0637 1.0000 Uiso R . . . . .
H123 H 0.6926 -0.0835 0.7633 0.0635 1.0000 Uiso R . . . . .
H141 H 0.5889 0.0231 0.4819 0.0647 1.0000 Uiso R . . . . .
H142 H 0.6839 0.0053 0.4295 0.0650 1.0000 Uiso R . . . . .
H143 H 0.6049 -0.0819 0.4291 0.0648 1.0000 Uiso R . . . . .
H153 H 0.7855 -0.1946 0.5591 0.0761 1.0000 Uiso R . . . . .
H152 H 0.8086 -0.1190 0.4823 0.0757 1.0000 Uiso R . . . . .
H151 H 0.7315 -0.2089 0.4719 0.0759 1.0000 Uiso R . . . . .
H161 H 0.6313 -0.1851 0.6330 0.0686 1.0000 Uiso R . . . . .
H162 H 0.5598 -0.0940 0.6136 0.0685 1.0000 Uiso R . . . . .
H163 H 0.5701 -0.1865 0.5505 0.0689 1.0000 Uiso R . . . . .
H183 H 0.8496 0.4483 0.5558 0.0624 1.0000 Uiso R . . . . .
H182 H 0.8652 0.5659 0.5296 0.0628 1.0000 Uiso R . . . . .
H181 H 0.7628 0.5253 0.5484 0.0626 1.0000 Uiso R . . . . .
H191 H 0.7688 0.5610 0.3209 0.0608 1.0000 Uiso R . . . . .
H192 H 0.8057 0.6354 0.3926 0.0606 1.0000 Uiso R . . . . .
H193 H 0.7051 0.5848 0.3989 0.0607 1.0000 Uiso R . . . . .
H201 H 0.9041 0.4399 0.3323 0.0666 1.0000 Uiso R . . . . .
H202 H 0.9525 0.5102 0.4027 0.0665 1.0000 Uiso R . . . . .
H203 H 0.9352 0.3879 0.4189 0.0667 1.0000 Uiso R . . . . .
H223 H 0.5591 0.4141 0.3325 0.0665 1.0000 Uiso R . . . . .
H222 H 0.6362 0.4800 0.2827 0.0667 1.0000 Uiso R . . . . .
H221 H 0.5797 0.3897 0.2365 0.0671 1.0000 Uiso R . . . . .
H231 H 0.8119 0.2768 0.2692 0.0627 1.0000 Uiso R . . . . .
H232 H 0.7872 0.3940 0.2405 0.0626 1.0000 Uiso R . . . . .
H233 H 0.7337 0.2972 0.1959 0.0631 1.0000 Uiso R . . . . .
H241 H 0.6815 0.1686 0.3377 0.0608 1.0000 Uiso R . . . . .
H242 H 0.5862 0.2244 0.3675 0.0609 1.0000 Uiso R . . . . .
H243 H 0.6054 0.2049 0.2704 0.0608 1.0000 Uiso R . . . . .
H11 H 0.9780 0.2181 0.5527 0.0534 1.0000 Uiso R . . . . .
H12 H 0.9223 0.2160 0.6379 0.0534 1.0000 Uiso R . . . . .
H13 H 0.9237 0.3182 0.5827 0.0534 1.0000 Uiso R . . . . .
H21 H 0.9319 0.1102 0.4172 0.0580 1.0000 Uiso R . . . . .
H22 H 0.8443 0.0357 0.4098 0.0580 1.0000 Uiso R . . . . .
H23 H 0.8471 0.1397 0.3570 0.0580 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.793(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
C1 . Ti1 . 2.138(4) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . Ti1 . 2.143(4) yes
C2 . H21 . 0.950 no
C2 . H22 . 0.950 no
C2 . H23 . 0.950 no
C3 . C4 . 1.395(4) yes
C3 . C8 . 1.407(4) yes
C3 . Ti1 . 2.241(3) yes
C4 . C5 . 1.387(4) yes
C4 . O1 . 1.396(4) yes
C5 . C6 . 1.388(4) yes
C5 . H51 . 0.917 no
C6 . C7 . 1.383(4) yes
C6 . H61 . 0.944 no
C7 . C8 . 1.387(4) yes
C7 . H71 . 0.932 no
C8 . O2 . 1.400(3) yes
C9 . C10 . 1.541(5) yes
C9 . C11 . 1.533(5) yes
C9 . C12 . 1.528(5) yes
C9 . P1 . 1.858(3) yes
C10 . H101 . 0.964 no
C10 . H102 . 0.954 no
C10 . H103 . 0.961 no
C11 . H113 . 0.970 no
C11 . H112 . 0.965 no
C11 . H111 . 0.975 no
C12 . H121 . 0.962 no
C12 . H122 . 0.958 no
C12 . H123 . 0.958 no
C13 . C14 . 1.530(5) yes
C13 . C15 . 1.524(5) yes
C13 . C16 . 1.532(5) yes
C13 . P1 . 1.871(3) yes
C14 . H141 . 0.968 no
C14 . H142 . 0.962 no
C14 . H143 . 0.962 no
C15 . H153 . 0.952 no
C15 . H152 . 0.968 no
C15 . H151 . 0.964 no
C16 . H161 . 0.949 no
C16 . H162 . 0.959 no
C16 . H163 . 0.943 no
C17 . C18 . 1.542(5) yes
C17 . C19 . 1.530(5) yes
C17 . C20 . 1.539(4) yes
C17 . P2 . 1.861(3) yes
C18 . H183 . 0.959 no
C18 . H182 . 0.964 no
C18 . H181 . 0.961 no
C19 . H191 . 0.953 no
C19 . H192 . 0.961 no
C19 . H193 . 0.954 no
C20 . H201 . 0.948 no
C20 . H202 . 0.956 no
C20 . H203 . 0.967 no
C21 . C22 . 1.528(5) yes
C21 . C23 . 1.527(4) yes
C21 . C24 . 1.535(5) yes
C21 . P2 . 1.872(3) yes
C22 . H223 . 0.957 no
C22 . H222 . 0.964 no
C22 . H221 . 0.958 no
C23 . H231 . 0.976 no
C23 . H232 . 0.960 no
C23 . H233 . 0.982 no
C24 . H241 . 0.965 no
C24 . H242 . 0.968 no
C24 . H243 . 0.953 no
Ti1 . P1 . 2.6243(9) yes
Ti1 . P2 . 2.6180(9) yes
P1 . O1 . 1.646(2) yes
O2 . P2 . 1.641(2) 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
Ti1 . C1 . H11 . 109.4 no
Ti1 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.5 no
Ti1 . C1 . H13 . 109.5 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
Ti1 . C2 . H21 . 109.5 no
Ti1 . C2 . H22 . 109.4 no
H21 . C2 . H22 . 109.5 no
Ti1 . C2 . H23 . 109.4 no
H21 . C2 . H23 . 109.5 no
H22 . C2 . H23 . 109.5 no
C4 . C3 . C8 . 112.6(3) yes
C4 . C3 . Ti1 . 122.9(2) yes
C8 . C3 . Ti1 . 123.5(2) yes
C3 . C4 . C5 . 125.2(3) yes
C3 . C4 . O1 . 121.0(3) yes
C5 . C4 . O1 . 113.7(3) yes
C4 . C5 . C6 . 118.4(3) yes
C4 . C5 . H51 . 120.2 no
C6 . C5 . H51 . 121.4 no
C5 . C6 . C7 . 120.2(3) yes
C5 . C6 . H61 . 119.0 no
C7 . C6 . H61 . 120.8 no
C6 . C7 . C8 . 118.4(3) yes
C6 . C7 . H71 . 121.5 no
C8 . C7 . H71 . 120.1 no
C3 . C8 . C7 . 125.1(3) yes
C3 . C8 . O2 . 120.2(2) yes
C7 . C8 . O2 . 114.8(3) yes
C10 . C9 . C11 . 109.1(3) yes
C10 . C9 . C12 . 108.8(3) yes
C11 . C9 . C12 . 110.6(3) yes
C10 . C9 . P1 . 105.6(2) yes
C11 . C9 . P1 . 107.9(2) yes
C12 . C9 . P1 . 114.6(2) yes
C9 . C10 . H101 . 109.4 no
C9 . C10 . H102 . 108.5 no
H101 . C10 . H102 . 109.7 no
C9 . C10 . H103 . 111.0 no
H101 . C10 . H103 . 109.4 no
H102 . C10 . H103 . 108.8 no
C9 . C11 . H113 . 109.5 no
C9 . C11 . H112 . 109.2 no
H113 . C11 . H112 . 109.2 no
C9 . C11 . H111 . 111.6 no
H113 . C11 . H111 . 108.4 no
H112 . C11 . H111 . 108.9 no
C9 . C12 . H121 . 109.1 no
C9 . C12 . H122 . 109.4 no
H121 . C12 . H122 . 109.2 no
C9 . C12 . H123 . 110.1 no
H121 . C12 . H123 . 109.3 no
H122 . C12 . H123 . 109.7 no
C14 . C13 . C15 . 109.3(3) yes
C14 . C13 . C16 . 108.1(3) yes
C15 . C13 . C16 . 110.4(3) yes
C14 . C13 . P1 . 103.7(2) yes
C15 . C13 . P1 . 110.9(3) yes
C16 . C13 . P1 . 114.1(2) yes
C13 . C14 . H141 . 110.0 no
C13 . C14 . H142 . 109.6 no
H141 . C14 . H142 . 110.9 no
C13 . C14 . H143 . 108.0 no
H141 . C14 . H143 . 109.8 no
H142 . C14 . H143 . 108.5 no
C13 . C15 . H153 . 109.5 no
C13 . C15 . H152 . 110.0 no
H153 . C15 . H152 . 109.7 no
C13 . C15 . H151 . 109.7 no
H153 . C15 . H151 . 108.8 no
H152 . C15 . H151 . 109.2 no
C13 . C16 . H161 . 110.8 no
C13 . C16 . H162 . 110.5 no
H161 . C16 . H162 . 109.1 no
C13 . C16 . H163 . 110.1 no
H161 . C16 . H163 . 108.6 no
H162 . C16 . H163 . 107.7 no
C18 . C17 . C19 . 107.9(3) yes
C18 . C17 . C20 . 109.0(3) yes
C19 . C17 . C20 . 109.9(3) yes
C18 . C17 . P2 . 105.4(2) yes
C19 . C17 . P2 . 115.4(2) yes
C20 . C17 . P2 . 109.0(2) yes
C17 . C18 . H183 . 110.9 no
C17 . C18 . H182 . 109.3 no
H183 . C18 . H182 . 108.0 no
C17 . C18 . H181 . 111.9 no
H183 . C18 . H181 . 108.9 no
H182 . C18 . H181 . 107.9 no
C17 . C19 . H191 . 110.2 no
C17 . C19 . H192 . 110.8 no
H191 . C19 . H192 . 107.7 no
C17 . C19 . H193 . 110.7 no
H191 . C19 . H193 . 108.8 no
H192 . C19 . H193 . 108.6 no
C17 . C20 . H201 . 108.4 no
C17 . C20 . H202 . 109.2 no
H201 . C20 . H202 . 109.9 no
C17 . C20 . H203 . 109.4 no
H201 . C20 . H203 . 109.0 no
H202 . C20 . H203 . 110.9 no
C22 . C21 . C23 . 110.4(3) yes
C22 . C21 . C24 . 107.7(3) yes
C23 . C21 . C24 . 109.2(3) yes
C22 . C21 . P2 . 114.3(2) yes
C23 . C21 . P2 . 110.2(2) yes
C24 . C21 . P2 . 104.7(2) yes
C21 . C22 . H223 . 109.6 no
C21 . C22 . H222 . 110.0 no
H223 . C22 . H222 . 110.6 no
C21 . C22 . H221 . 108.9 no
H223 . C22 . H221 . 109.3 no
H222 . C22 . H221 . 108.5 no
C21 . C23 . H231 . 109.9 no
C21 . C23 . H232 . 109.4 no
H231 . C23 . H232 . 109.6 no
C21 . C23 . H233 . 109.1 no
H231 . C23 . H233 . 109.0 no
H232 . C23 . H233 . 109.9 no
C21 . C24 . H241 . 109.9 no
C21 . C24 . H242 . 110.2 no
H241 . C24 . H242 . 110.3 no
C21 . C24 . H243 . 109.2 no
H241 . C24 . H243 . 108.3 no
H242 . C24 . H243 . 108.8 no
C3 . Ti1 . C2 . 140.53(14) yes
C3 . Ti1 . C1 . 120.07(14) yes
C2 . Ti1 . C1 . 99.38(16) yes
C3 . Ti1 . P1 . 72.30(8) yes
C2 . Ti1 . P1 . 100.41(12) yes
C1 . Ti1 . P1 . 104.48(10) yes
C3 . Ti1 . P2 . 71.99(8) yes
C2 . Ti1 . P2 . 97.89(12) yes
C1 . Ti1 . P2 . 105.61(11) yes
P1 . Ti1 . P2 . 141.44(3) yes
C13 . P1 . C9 . 112.48(16) yes
C13 . P1 . Ti1 . 116.09(11) yes
C9 . P1 . Ti1 . 119.70(11) yes
C13 . P1 . O1 . 100.26(14) yes
C9 . P1 . O1 . 100.06(13) yes
Ti1 . P1 . O1 . 104.13(8) yes
C4 . O1 . P1 . 117.50(18) yes
C8 . O2 . P2 . 117.37(18) yes
C21 . P2 . C17 . 111.95(15) yes
C21 . P2 . Ti1 . 117.85(11) yes
C17 . P2 . Ti1 . 118.01(11) yes
C21 . P2 . O2 . 99.91(13) yes
C17 . P2 . O2 . 100.46(13) yes
Ti1 . P2 . O2 . 104.75(8) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 

# start Validation Reply Form
_vrf_PLAT230_5                   
;
PROBLEM: Hirshfeld Test Diff for    P1       --C9       .       14.6 s.u.  
RESPONSE: Failing Hirshfeld is not unusual for organometallic
compounds. Assignment of atoms is correct and applying
restraints on ADPs not necessary. 
;
_vrf_PLAT934_5                   
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          9 Check 
RESPONSE: This is not a significant number of outliers 
and is not indicative of a systematic issue.
;
# end Validation Reply Form

####################################################################### 
# 
# 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 2204756'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_cell_length_a                   11.9525(3)
_cell_length_b                   13.0318(2)
_cell_length_c                   15.1944(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.440(2)
_cell_angle_gamma                90
_cell_volume                     2319.70(9)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,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 0.2191 1.8069 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'
O 0.0492 0.0322 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'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0181 0.0091 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'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 '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            2

# Given Formula = C36 H62 Cl6 O4 P4 Ti2 
# Dc =      1.42 Fooo =   1032.00 Mu =     76.95 M =    991.30
# Found Formula = C36 H62 Cl6 O4 P4 Ti2 
# Dc =      1.42 FOOO =   1032.00 Mu =     76.95 M =    991.30

_chemical_formula_sum            'C36 H62 Cl6 O4 P4 Ti2'
_chemical_formula_moiety         'C36 H62 Cl6 O4 P4 Ti2'
_chemical_compound_source        .
_chemical_formula_weight         991.30


_cell_measurement_reflns_used    5213
_cell_measurement_theta_min      4
_cell_measurement_theta_max      73
_cell_measurement_temperature    173

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_max          0.050

_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    7.695

# Sheldrick geometric approximatio 0.68 0.68 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_T_max  0.68
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_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      173
_diffrn_reflns_number            13979
_diffrn_reflns_av_unetI/netI     0.058
_reflns_number_total             4544
_diffrn_reflns_av_R_equivalents  0.042
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 4544 
# Theoretical number of reflections is about 9334 


_diffrn_reflns_theta_min         3.773
_diffrn_reflns_theta_max         73.409
_diffrn_measured_fraction_theta_max 0.977

_diffrn_reflns_theta_full        68.271
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   2.54
_oxford_diffrn_Wilson_scale      0.08

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

_refine_diff_density_min         -0.87
_refine_diff_density_max         1.15


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4544
_oxford_refine_ls_R_factor_ref   0.0656
_refine_ls_wR_factor_ref         0.1729
_refine_ls_goodness_of_fit_ref   1.5275
_refine_ls_shift/su_max          0.0004878
_refine_ls_shift/su_mean         0.0000955


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4544
_refine_ls_R_factor_all          0.0656
_refine_ls_wR_factor_all         0.1729

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3840
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_gt          0.1576


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #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: 
 0.213E+04 0.354E+04 0.220E+04 931. 214. 
;

# 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 0.8272(3) 0.5283(3) 0.6784(3) 0.0322 1.0000 Uani . . . . . .
C2 C 0.8902(4) 0.6198(3) 0.6912(3) 0.0370 1.0000 Uani . . . . . .
C3 C 0.9918(4) 0.6326(4) 0.7512(4) 0.0441 1.0000 Uani . . . . . .
C4 C 1.0402(4) 0.5491(4) 0.8004(4) 0.0492 1.0000 Uani . . . . . .
C5 C 0.9842(4) 0.4552(4) 0.7907(3) 0.0440 1.0000 Uani . . . . . .
C6 C 0.8810(4) 0.4478(3) 0.7314(3) 0.0351 1.0000 Uani . . . . . .
C7 C 0.8766(5) 0.6489(5) 0.4744(4) 0.0600 1.0000 Uani . . . . . .
C8 C 0.8268(7) 0.6180(6) 0.3773(4) 0.0735 1.0000 Uani . . . . . .
C9 C 0.9655(6) 0.7359(6) 0.4834(5) 0.0769 1.0000 Uani . . . . . .
C10 C 0.6865(5) 0.7918(4) 0.5145(4) 0.0521 1.0000 Uani . . . . . .
C11 C 0.6694(6) 0.8193(5) 0.4152(4) 0.0652 1.0000 Uani . . . . . .
C12 C 0.7352(5) 0.8820(4) 0.5746(5) 0.0647 1.0000 Uani . . . . . .
C13 C 0.6553(4) 0.4201(3) 0.8131(3) 0.0397 1.0000 Uani . . . . . .
C14 C 0.7348(6) 0.3802(5) 0.8968(3) 0.0629 1.0000 Uani . . . . . .
C15 C 0.5299(5) 0.4088(5) 0.8152(4) 0.0603 1.0000 Uani . . . . . .
C16 C 0.6354(4) 0.2395(3) 0.6888(3) 0.0344 1.0000 Uani . . . . . .
C17 C 0.6505(5) 0.1971(4) 0.5986(3) 0.0472 1.0000 Uani . . . . . .
C18 C 0.6885(4) 0.1675(4) 0.7661(3) 0.0421 1.0000 Uani . . . . . .
Ti1 Ti 0.65769(6) 0.51292(6) 0.58327(5) 0.0301 1.0000 Uani . . . . . .
Cl3 Cl 0.46559(8) 0.41567(8) 0.56339(7) 0.0389 1.0000 Uani . . . . . .
Cl2 Cl 0.58529(8) 0.63246(7) 0.67202(7) 0.0316 1.0000 Uani . . . . . .
Cl1 Cl 0.74563(11) 0.40573(8) 0.49840(7) 0.0417 1.0000 Uani . . . . . .
P2 P 0.68730(9) 0.37219(8) 0.70577(7) 0.0298 1.0000 Uani . . . . . .
O2 O 0.8253(3) 0.3531(2) 0.7283(2) 0.0367 1.0000 Uani . . . . . .
O1 O 0.8494(3) 0.7045(2) 0.6392(2) 0.0406 1.0000 Uani . . . . . .
P1 P 0.76817(9) 0.67065(9) 0.54359(8) 0.0355 1.0000 Uani . . . . . .
H31 H 1.0298 0.6958 0.7574 0.0541 1.0000 Uiso R . . . . .
H41 H 1.1109 0.5573 0.8398 0.0600 1.0000 Uiso R . . . . .
H51 H 1.0155 0.3981 0.8247 0.0534 1.0000 Uiso R . . . . .
H71 H 0.9228 0.5905 0.5002 0.0718 1.0000 Uiso R . . . . .
H81 H 0.7707 0.5653 0.3737 0.1096 1.0000 Uiso R . . . . .
H83 H 0.8871 0.5947 0.3499 0.1100 1.0000 Uiso R . . . . .
H82 H 0.7934 0.6763 0.3443 0.1098 1.0000 Uiso R . . . . .
H91 H 0.9930 0.7479 0.5472 0.1180 1.0000 Uiso R . . . . .
H92 H 1.0264 0.7083 0.4567 0.1181 1.0000 Uiso R . . . . .
H93 H 0.9308 0.7960 0.4513 0.1182 1.0000 Uiso R . . . . .
H101 H 0.6101 0.7802 0.5264 0.0631 1.0000 Uiso R . . . . .
H111 H 0.6462 0.7603 0.3779 0.0980 1.0000 Uiso R . . . . .
H113 H 0.7406 0.8454 0.4024 0.0979 1.0000 Uiso R . . . . .
H112 H 0.6121 0.8721 0.4002 0.0981 1.0000 Uiso R . . . . .
H121 H 0.7491 0.8611 0.6378 0.0978 1.0000 Uiso R . . . . .
H122 H 0.8079 0.9013 0.5579 0.0980 1.0000 Uiso R . . . . .
H123 H 0.6804 0.9373 0.5638 0.0982 1.0000 Uiso R . . . . .
H131 H 0.6702 0.4940 0.8127 0.0483 1.0000 Uiso R . . . . .
H141 H 0.8130 0.3840 0.8908 0.0942 1.0000 Uiso R . . . . .
H142 H 0.7248 0.4187 0.9477 0.0938 1.0000 Uiso R . . . . .
H143 H 0.7155 0.3113 0.9068 0.0937 1.0000 Uiso R . . . . .
H151 H 0.4816 0.4395 0.7630 0.0906 1.0000 Uiso R . . . . .
H152 H 0.5144 0.4409 0.8689 0.0908 1.0000 Uiso R . . . . .
H153 H 0.5128 0.3377 0.8164 0.0909 1.0000 Uiso R . . . . .
H161 H 0.5536 0.2437 0.6875 0.0419 1.0000 Uiso R . . . . .
H171 H 0.6120 0.2406 0.5492 0.0709 1.0000 Uiso R . . . . .
H172 H 0.7312 0.1920 0.5975 0.0708 1.0000 Uiso R . . . . .
H173 H 0.6185 0.1284 0.5904 0.0710 1.0000 Uiso R . . . . .
H181 H 0.6703 0.1897 0.8216 0.0642 1.0000 Uiso R . . . . .
H182 H 0.7718 0.1666 0.7736 0.0638 1.0000 Uiso R . . . . .
H183 H 0.6601 0.0981 0.7540 0.0639 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.46(6)
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 . 1.404(6) yes
C1 . C6 . 1.399(6) yes
C1 . Ti1 . 2.252(4) yes
C2 . C3 . 1.376(6) yes
C2 . O1 . 1.388(5) yes
C3 . C4 . 1.380(7) yes
C3 . H31 . 0.936 no
C4 . C5 . 1.389(7) yes
C4 . H41 . 0.939 no
C5 . C6 . 1.379(6) yes
C5 . H51 . 0.940 no
C6 . O2 . 1.399(5) yes
C7 . C8 . 1.532(9) yes
C7 . C9 . 1.541(9) yes
C7 . P1 . 1.845(6) yes
C7 . H71 . 0.974 no
C8 . H81 . 0.954 no
C8 . H83 . 0.951 no
C8 . H82 . 0.952 no
C9 . H91 . 0.974 no
C9 . H92 . 0.970 no
C9 . H93 . 0.971 no
C10 . C11 . 1.526(8) yes
C10 . C12 . 1.530(8) yes
C10 . P1 . 1.863(5) yes
C10 . H101 . 0.977 no
C11 . H111 . 0.962 no
C11 . H113 . 0.970 no
C11 . H112 . 0.967 no
C12 . H121 . 0.981 no
C12 . H122 . 0.984 no
C12 . H123 . 0.967 no
C13 . C14 . 1.521(7) yes
C13 . C15 . 1.512(7) yes
C13 . P2 . 1.855(4) yes
C13 . H131 . 0.979 no
C14 . H141 . 0.958 no
C14 . H142 . 0.948 no
C14 . H143 . 0.946 no
C15 . H151 . 0.969 no
C15 . H152 . 0.968 no
C15 . H153 . 0.951 no
C16 . C17 . 1.521(6) yes
C16 . C18 . 1.538(6) yes
C16 . P2 . 1.837(4) yes
C16 . H161 . 0.976 no
C17 . H171 . 0.980 no
C17 . H172 . 0.970 no
C17 . H173 . 0.971 no
C18 . H181 . 0.958 no
C18 . H182 . 0.979 no
C18 . H183 . 0.972 no
Ti1 . Cl3 2_666 2.5886(12) yes
Ti1 . Cl3 . 2.5873(12) yes
Ti1 . Cl2 . 2.3360(12) yes
Ti1 . Cl1 . 2.2927(13) yes
Ti1 . P2 . 2.5869(12) yes
Ti1 . P1 . 2.5784(13) yes
P2 . O2 . 1.635(3) yes
O1 . P1 . 1.640(3) 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 . C6 . 112.6(4) yes
C2 . C1 . Ti1 . 123.7(3) yes
C6 . C1 . Ti1 . 123.7(3) yes
C1 . C2 . C3 . 125.0(4) yes
C1 . C2 . O1 . 118.5(4) yes
C3 . C2 . O1 . 116.5(4) yes
C2 . C3 . C4 . 118.9(4) yes
C2 . C3 . H31 . 121.3 no
C4 . C3 . H31 . 119.8 no
C3 . C4 . C5 . 119.7(4) yes
C3 . C4 . H41 . 118.8 no
C5 . C4 . H41 . 121.5 no
C4 . C5 . C6 . 118.8(4) yes
C4 . C5 . H51 . 120.6 no
C6 . C5 . H51 . 120.7 no
C1 . C6 . C5 . 124.9(4) yes
C1 . C6 . O2 . 118.8(4) yes
C5 . C6 . O2 . 116.2(4) yes
C8 . C7 . C9 . 114.0(5) yes
C8 . C7 . P1 . 114.0(5) yes
C9 . C7 . P1 . 112.7(5) yes
C8 . C7 . H71 . 105.2 no
C9 . C7 . H71 . 102.3 no
P1 . C7 . H71 . 107.3 no
C7 . C8 . H81 . 112.2 no
C7 . C8 . H83 . 108.7 no
H81 . C8 . H83 . 109.3 no
C7 . C8 . H82 . 109.9 no
H81 . C8 . H82 . 109.1 no
H83 . C8 . H82 . 107.5 no
C7 . C9 . H91 . 107.3 no
C7 . C9 . H92 . 104.6 no
H91 . C9 . H92 . 110.0 no
C7 . C9 . H93 . 109.3 no
H91 . C9 . H93 . 113.4 no
H92 . C9 . H93 . 111.7 no
C11 . C10 . C12 . 111.7(5) yes
C11 . C10 . P1 . 113.2(4) yes
C12 . C10 . P1 . 113.0(4) yes
C11 . C10 . H101 . 105.8 no
C12 . C10 . H101 . 105.5 no
P1 . C10 . H101 . 106.9 no
C10 . C11 . H111 . 111.1 no
C10 . C11 . H113 . 109.2 no
H111 . C11 . H113 . 109.0 no
C10 . C11 . H112 . 110.5 no
H111 . C11 . H112 . 108.8 no
H113 . C11 . H112 . 108.1 no
C10 . C12 . H121 . 110.0 no
C10 . C12 . H122 . 107.1 no
H121 . C12 . H122 . 109.7 no
C10 . C12 . H123 . 107.9 no
H121 . C12 . H123 . 110.4 no
H122 . C12 . H123 . 111.7 no
C14 . C13 . C15 . 114.0(5) yes
C14 . C13 . P2 . 114.6(4) yes
C15 . C13 . P2 . 111.3(4) yes
C14 . C13 . H131 . 104.9 no
C15 . C13 . H131 . 106.1 no
P2 . C13 . H131 . 104.8 no
C13 . C14 . H141 . 111.1 no
C13 . C14 . H142 . 110.0 no
H141 . C14 . H142 . 109.5 no
C13 . C14 . H143 . 109.0 no
H141 . C14 . H143 . 109.7 no
H142 . C14 . H143 . 107.3 no
C13 . C15 . H151 . 112.1 no
C13 . C15 . H152 . 109.4 no
H151 . C15 . H152 . 109.1 no
C13 . C15 . H153 . 108.3 no
H151 . C15 . H153 . 108.8 no
H152 . C15 . H153 . 109.0 no
C17 . C16 . C18 . 111.2(4) yes
C17 . C16 . P2 . 111.8(3) yes
C18 . C16 . P2 . 113.0(3) yes
C17 . C16 . H161 . 107.4 no
C18 . C16 . H161 . 108.0 no
P2 . C16 . H161 . 105.1 no
C16 . C17 . H171 . 111.0 no
C16 . C17 . H172 . 109.6 no
H171 . C17 . H172 . 110.1 no
C16 . C17 . H173 . 109.7 no
H171 . C17 . H173 . 108.8 no
H172 . C17 . H173 . 107.5 no
C16 . C18 . H181 . 110.9 no
C16 . C18 . H182 . 110.7 no
H181 . C18 . H182 . 107.7 no
C16 . C18 . H183 . 110.4 no
H181 . C18 . H183 . 108.4 no
H182 . C18 . H183 . 108.7 no
Cl3 2_666 Ti1 . C1 . 143.76(12) yes
Cl3 2_666 Ti1 . Cl3 . 74.64(4) yes
C1 . Ti1 . Cl3 . 141.54(12) yes
Cl3 2_666 Ti1 . Cl2 . 92.54(4) yes
C1 . Ti1 . Cl2 . 87.67(11) yes
Cl3 . Ti1 . Cl2 . 88.41(4) yes
Cl3 2_666 Ti1 . Cl1 . 88.91(5) yes
C1 . Ti1 . Cl1 . 87.74(11) yes
Cl3 . Ti1 . Cl1 . 97.54(5) yes
Cl2 . Ti1 . Cl1 . 174.05(5) yes
Cl3 2_666 Ti1 . P2 . 147.95(4) yes
C1 . Ti1 . P2 . 67.91(11) yes
Cl3 . Ti1 . P2 . 74.24(4) yes
Cl2 . Ti1 . P2 . 94.07(4) yes
Cl1 . Ti1 . P2 . 87.72(4) yes
Cl3 2_666 Ti1 . P1 . 75.08(4) yes
C1 . Ti1 . P1 . 69.02(11) yes
Cl3 . Ti1 . P1 . 147.89(4) yes
Cl2 . Ti1 . P1 . 82.46(4) yes
Cl1 . Ti1 . P1 . 92.35(5) yes
P2 . Ti1 . P1 . 136.89(4) yes
Ti1 2_666 Cl3 . Ti1 . 105.36(4) yes
C13 . P2 . C16 . 108.5(2) yes
C13 . P2 . Ti1 . 111.78(15) yes
C16 . P2 . Ti1 . 124.87(15) yes
C13 . P2 . O2 . 104.0(2) yes
C16 . P2 . O2 . 100.61(18) yes
Ti1 . P2 . O2 . 104.32(12) yes
C6 . O2 . P2 . 109.0(3) yes
C2 . O1 . P1 . 111.7(3) yes
C10 . P1 . C7 . 112.9(3) yes
C10 . P1 . Ti1 . 117.55(18) yes
C7 . P1 . Ti1 . 117.4(2) yes
C10 . P1 . O1 . 99.9(2) yes
C7 . P1 . O1 . 100.8(2) yes
Ti1 . P1 . O1 . 104.33(12) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 

# start Validation Reply Form
_vrf_PLAT934_4                   
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          4 Check 
RESPONSE: This is not a significant number of outliers and
not indicative of a systematic issue.
;
# end Validation Reply Form

####################################################################### 
# 
# 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 2204754'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;

_oxford_structure_analysis_title 'T-2\FMC2102_autored.cif_od At 15: 8 on 17/10'
_chemical_name_systematic        .
_chemical_melting_point          'not measured'


_cell_length_a                   9.8749(2)
_cell_length_b                   10.5591(3)
_cell_length_c                   13.2857(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.419(2)
_cell_angle_gamma                90
_cell_volume                     1366.62(6)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21 '
_symmetry_space_group_name_Hall  'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-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
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 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'
Ti 0.2191 1.8069 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'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0181 0.0091 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            2

# Given Formula = C22 H39 Cl3 O2 P2 Ti1 
# Dc =      1.34 Fooo =    580.00 Mu =     65.84 M =    551.76
# Found Formula = C22 H39 Cl3 O2 P2 Ti1 
# Dc =      1.34 FOOO =    580.00 Mu =     65.84 M =    551.76

_chemical_formula_sum            'C22 H39 Cl3 O2 P2 Ti'
_chemical_formula_moiety         'C22 H39 Cl3 O2 P2 Ti'
_chemical_compound_source        .
_chemical_formula_weight         551.76


_cell_measurement_reflns_used    2381
_cell_measurement_theta_min      5
_cell_measurement_theta_max      73
_cell_measurement_temperature    173

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_max          0.100

_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             580
_exptl_absorpt_coefficient_mu    6.584

# Sheldrick geometric approximatio 0.52 0.72 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_T_max  0.72
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_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      173
_diffrn_reflns_number            4812
_diffrn_reflns_av_unetI/netI     0.077
_reflns_number_total             3568
_diffrn_reflns_av_R_equivalents  0.049
# Number of reflections without Friedels Law is 3568 
# Number of reflections with Friedels Law is 2763 
# Theoretical number of reflections is about 2742 


_diffrn_reflns_theta_min         3.372
_diffrn_reflns_theta_max         73.245
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        73.245
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -8
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.41
_oxford_diffrn_Wilson_scale      0.13

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

_refine_diff_density_min         -0.41
_refine_diff_density_max         0.62


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     418
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3568
_oxford_refine_ls_R_factor_ref   0.0553
_refine_ls_wR_factor_ref         0.1360
_refine_ls_goodness_of_fit_ref   1.0055
_refine_ls_shift/su_max          0.0396075
_refine_ls_shift/su_mean         0.0058062


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3568
_refine_ls_R_factor_all          0.0553
_refine_ls_wR_factor_all         0.1360

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3251
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_gt          0.1278

# For an explanation, see Cooper & Watkin, Acta Cryst. (2016). B72, 661-683 
_oxford_Hooft_y                  0.003(16) # for 784 Friedel pairs 
_oxford_Bijvoet_difference       -0.033(14) # for 784 Friedel pairs 
# (Similar to the Parsons(q).) 
_oxford_refined_Flack_x          -0.028(13) # for 805 Friedel pairs 
_refine_ls_abs_structure_Flack   -0.033(14)
_refine_ls_abs_structure_details 
; 
 Parsons, Flack & Wagner (2013), 
 784 Friedel Pairs 
;

# 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 ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² + 0.09P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.41244(9) 0.32098(9) 0.27552(9) 0.0280 1.0000 Uani . . . . . .
C2 C 0.48942(9) 0.34259(9) 0.19725(9) 0.0283 1.0000 Uani . . . . . .
C3 C 0.62988(7) 0.31409(7) 0.20702(7) 0.0378 1.0000 Uani . . . . . .
C4 C 0.69441(7) 0.26328(7) 0.29702(7) 0.0404 1.0000 Uani . . . . . .
C5 C 0.62492(7) 0.23588(7) 0.37599(7) 0.0346 1.0000 Uani . . . . . .
C6 C 0.48632(9) 0.26452(9) 0.36275(9) 0.0292 1.0000 Uani . . . . . .
C7 C 0.34676(9) 0.63299(9) 0.09851(9) 0.0355 1.0000 Uani . . . . . .
C8 C 0.46671(5) 0.63990(5) 0.03793(5) 0.0484 1.0000 Uani . . . . . .
C9 C 0.40413(5) 0.67534(5) 0.20886(5) 0.0457 1.0000 Uani . . . . . .
C10 C 0.23299(5) 0.72415(5) 0.05262(5) 0.0451 1.0000 Uani . . . . . .
C11 C 0.18249(9) 0.41158(9) -0.01814(9) 0.0291 1.0000 Uani . . . . . .
C12 C 0.24816(5) 0.44903(5) -0.11139(5) 0.0430 1.0000 Uani . . . . . .
C13 C 0.18159(5) 0.26618(5) -0.01324(5) 0.0360 1.0000 Uani . . . . . .
C14 C 0.03653(5) 0.46231(5) -0.02901(5) 0.0382 1.0000 Uani . . . . . .
C15 C 0.18264(9) 0.19675(9) 0.52290(9) 0.0368 1.0000 Uani . . . . . .
C16 C 0.23276(5) 0.31125(5) 0.58886(5) 0.0534 1.0000 Uani . . . . . .
C17 C 0.22095(5) 0.07668(5) 0.58676(5) 0.0526 1.0000 Uani . . . . . .
C18 C 0.02380(5) 0.20657(5) 0.49326(5) 0.0492 1.0000 Uani . . . . . .
C19 C 0.25531(9) 0.03754(9) 0.34360(9) 0.0357 1.0000 Uani . . . . . .
C20 C 0.29149(5) 0.04527(5) 0.23365(5) 0.0382 1.0000 Uani . . . . . .
C21 C 0.36916(5) -0.04372(5) 0.40535(5) 0.0499 1.0000 Uani . . . . . .
C22 C 0.11572(5) -0.02671(5) 0.33498(5) 0.0461 1.0000 Uani . . . . . .
Ti1 Ti 0.20415(6) 0.39730(7) 0.27508(5) 0.0273 1.0000 Uani . . . . . .
Cl3 Cl 0.02304(7) 0.26858(8) 0.20964(7) 0.0378 1.0000 Uani . . . . . .
Cl2 Cl 0.05331(8) 0.57085(8) 0.22649(7) 0.0424 1.0000 Uani . . . . . .
Cl1 Cl 0.29238(8) 0.51410(8) 0.41327(7) 0.0455 1.0000 Uani . . . . . .
P1 P 0.28495(7) 0.46591(8) 0.10545(6) 0.0262 1.0000 Uani . . . . . .
O1 O 0.42945(9) 0.39012(9) 0.10478(9) 0.0310 1.0000 Uani . . . . . .
O2 O 0.41744(9) 0.22792(9) 0.44330(9) 0.0329 1.0000 Uani . . . . . .
P2 P 0.25427(7) 0.20333(8) 0.40017(6) 0.0291 1.0000 Uani . . . . . .
H31 H 0.6771 0.3297 0.1538 0.0452 1.0000 Uiso R . . . . .
H41 H 0.7882 0.2469 0.3048 0.0482 1.0000 Uiso R . . . . .
H51 H 0.6685 0.1991 0.4364 0.0417 1.0000 Uiso R . . . . .
H81 H 0.4368 0.6116 -0.0311 0.0727 1.0000 Uiso R . . . . .
H82 H 0.4977 0.7265 0.0374 0.0730 1.0000 Uiso R . . . . .
H83 H 0.5400 0.5864 0.0708 0.0729 1.0000 Uiso R . . . . .
H93 H 0.3314 0.6752 0.2481 0.0688 1.0000 Uiso R . . . . .
H92 H 0.4415 0.7594 0.2080 0.0690 1.0000 Uiso R . . . . .
H91 H 0.4759 0.6185 0.2390 0.0689 1.0000 Uiso R . . . . .
H101 H 0.1589 0.7194 0.0911 0.0677 1.0000 Uiso R . . . . .
H102 H 0.2693 0.8083 0.0551 0.0679 1.0000 Uiso R . . . . .
H103 H 0.2016 0.7013 -0.0170 0.0675 1.0000 Uiso R . . . . .
H121 H 0.2470 0.5391 -0.1190 0.0641 1.0000 Uiso R . . . . .
H122 H 0.3412 0.4197 -0.1029 0.0638 1.0000 Uiso R . . . . .
H123 H 0.1985 0.4115 -0.1719 0.0637 1.0000 Uiso R . . . . .
H133 H 0.1312 0.2403 0.0390 0.0540 1.0000 Uiso R . . . . .
H132 H 0.2734 0.2354 0.0028 0.0538 1.0000 Uiso R . . . . .
H131 H 0.1397 0.2330 -0.0774 0.0542 1.0000 Uiso R . . . . .
H141 H -0.0059 0.4355 0.0266 0.0571 1.0000 Uiso R . . . . .
H142 H 0.0355 0.5537 -0.0317 0.0569 1.0000 Uiso R . . . . .
H143 H -0.0150 0.4304 -0.0917 0.0569 1.0000 Uiso R . . . . .
H163 H 0.1975 0.3877 0.5546 0.0797 1.0000 Uiso R . . . . .
H162 H 0.2004 0.3053 0.6533 0.0800 1.0000 Uiso R . . . . .
H161 H 0.3311 0.3147 0.6005 0.0800 1.0000 Uiso R . . . . .
H171 H 0.1810 0.0041 0.5501 0.0788 1.0000 Uiso R . . . . .
H172 H 0.1874 0.0820 0.6499 0.0791 1.0000 Uiso R . . . . .
H173 H 0.3191 0.0667 0.5997 0.0789 1.0000 Uiso R . . . . .
H181 H -0.0111 0.1362 0.4510 0.0738 1.0000 Uiso R . . . . .
H182 H -0.0160 0.2080 0.5543 0.0741 1.0000 Uiso R . . . . .
H183 H 0.0017 0.2831 0.4557 0.0738 1.0000 Uiso R . . . . .
H203 H 0.2284 0.1000 0.1922 0.0568 1.0000 Uiso R . . . . .
H202 H 0.3827 0.0772 0.2356 0.0567 1.0000 Uiso R . . . . .
H201 H 0.2851 -0.0377 0.2034 0.0569 1.0000 Uiso R . . . . .
H211 H 0.3572 -0.0488 0.4753 0.0749 1.0000 Uiso R . . . . .
H212 H 0.4569 -0.0072 0.4020 0.0750 1.0000 Uiso R . . . . .
H213 H 0.3655 -0.1274 0.3767 0.0751 1.0000 Uiso R . . . . .
H221 H 0.0965 -0.0435 0.4022 0.0689 1.0000 Uiso R . . . . .
H222 H 0.1162 -0.1050 0.2982 0.0689 1.0000 Uiso R . . . . .
H223 H 0.0455 0.0274 0.3003 0.0688 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.754(18)
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 . 1.4035(17) yes
C1 . C6 . 1.3978(15) yes
C1 . Ti1 . 2.2081(11) yes
C2 . C3 . 1.4044(11) yes
C2 . O1 . 1.3689(15) yes
C3 . C4 . 1.3691(11) yes
C3 . H31 . 0.923 no
C4 . C5 . 1.3751(12) yes
C4 . H41 . 0.932 no
C5 . C6 . 1.3844(11) yes
C5 . H51 . 0.931 no
C6 . O2 . 1.4127(16) yes
C7 . C8 . 1.5388(12) yes
C7 . C9 . 1.5487(13) yes
C7 . C10 . 1.5284(10) yes
C7 . P1 . 1.8740(13) yes
C8 . H81 . 0.964 no
C8 . H82 . 0.964 no
C8 . H83 . 0.964 no
C9 . H93 . 0.954 no
C9 . H92 . 0.962 no
C9 . H91 . 0.965 no
C10 . H101 . 0.960 no
C10 . H102 . 0.957 no
C10 . H103 . 0.957 no
C11 . C12 . 1.5411(13) yes
C11 . C13 . 1.5368(11) yes
C11 . C14 . 1.5221(10) yes
C11 . P1 . 1.8722(13) yes
C12 . H121 . 0.956 no
C12 . H122 . 0.958 no
C12 . H123 . 0.956 no
C13 . H133 . 0.957 no
C13 . H132 . 0.954 no
C13 . H131 . 0.952 no
C14 . H141 . 0.950 no
C14 . H142 . 0.966 no
C14 . H143 . 0.964 no
C15 . C16 . 1.5273(12) yes
C15 . C17 . 1.5380(12) yes
C15 . C18 . 1.5569(10) yes
C15 . P2 . 1.8818(15) yes
C16 . H163 . 0.964 no
C16 . H162 . 0.963 no
C16 . H161 . 0.959 no
C17 . H171 . 0.958 no
C17 . H172 . 0.952 no
C17 . H173 . 0.962 no
C18 . H181 . 0.960 no
C18 . H182 . 0.957 no
C18 . H183 . 0.956 no
C19 . C20 . 1.5617(14) yes
C19 . C21 . 1.5399(11) yes
C19 . C22 . 1.5238(10) yes
C19 . P2 . 1.9058(13) yes
C20 . H203 . 0.956 no
C20 . H202 . 0.958 no
C20 . H201 . 0.962 no
C21 . H211 . 0.958 no
C21 . H212 . 0.956 no
C21 . H213 . 0.960 no
C22 . H221 . 0.960 no
C22 . H222 . 0.961 no
C22 . H223 . 0.956 no
Ti1 . Cl3 . 2.3006(10) yes
Ti1 . Cl2 . 2.3831(10) yes
Ti1 . Cl1 . 2.2643(11) yes
Ti1 . P1 . 2.6133(11) yes
Ti1 . P2 . 2.6330(11) yes
P1 . O1 . 1.6374(12) yes
O2 . P2 . 1.6401(11) 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 . C6 . 114.27(9) yes
C2 . C1 . Ti1 . 123.77(7) yes
C6 . C1 . Ti1 . 121.16(8) yes
C1 . C2 . C3 . 122.90(9) yes
C1 . C2 . O1 . 121.16(9) yes
C3 . C2 . O1 . 115.92(10) yes
C2 . C3 . C4 . 118.44(8) yes
C2 . C3 . H31 . 120.4 no
C4 . C3 . H31 . 121.2 no
C3 . C4 . C5 . 121.99(6) yes
C3 . C4 . H41 . 118.8 no
C5 . C4 . H41 . 119.2 no
C4 . C5 . C6 . 117.61(8) yes
C4 . C5 . H51 . 121.8 no
C6 . C5 . H51 . 120.6 no
C1 . C6 . C5 . 124.72(10) yes
C1 . C6 . O2 . 119.61(9) yes
C5 . C6 . O2 . 115.63(9) yes
C8 . C7 . C9 . 106.72(6) yes
C8 . C7 . C10 . 109.88(8) yes
C9 . C7 . C10 . 109.08(7) yes
C8 . C7 . P1 . 110.80(7) yes
C9 . C7 . P1 . 107.27(7) yes
C10 . C7 . P1 . 112.86(6) yes
C7 . C8 . H81 . 109.9 no
C7 . C8 . H82 . 108.7 no
H81 . C8 . H82 . 109.6 no
C7 . C8 . H83 . 108.7 no
H81 . C8 . H83 . 109.8 no
H82 . C8 . H83 . 110.1 no
C7 . C9 . H93 . 109.0 no
C7 . C9 . H92 . 109.7 no
H93 . C9 . H92 . 109.4 no
C7 . C9 . H91 . 110.1 no
H93 . C9 . H91 . 109.9 no
H92 . C9 . H91 . 108.8 no
C7 . C10 . H101 . 109.2 no
C7 . C10 . H102 . 108.9 no
H101 . C10 . H102 . 110.1 no
C7 . C10 . H103 . 109.1 no
H101 . C10 . H103 . 110.3 no
H102 . C10 . H103 . 109.1 no
C12 . C11 . C13 . 107.25(7) yes
C12 . C11 . C14 . 110.48(7) yes
C13 . C11 . C14 . 110.10(6) yes
C12 . C11 . P1 . 112.85(6) yes
C13 . C11 . P1 . 105.96(7) yes
C14 . C11 . P1 . 110.05(7) yes
C11 . C12 . H121 . 109.9 no
C11 . C12 . H122 . 110.1 no
H121 . C12 . H122 . 109.2 no
C11 . C12 . H123 . 110.1 no
H121 . C12 . H123 . 109.1 no
H122 . C12 . H123 . 108.4 no
C11 . C13 . H133 . 108.9 no
C11 . C13 . H132 . 109.8 no
H133 . C13 . H132 . 109.2 no
C11 . C13 . H131 . 109.5 no
H133 . C13 . H131 . 110.1 no
H132 . C13 . H131 . 109.4 no
C11 . C14 . H141 . 110.7 no
C11 . C14 . H142 . 111.1 no
H141 . C14 . H142 . 108.9 no
C11 . C14 . H143 . 108.5 no
H141 . C14 . H143 . 109.3 no
H142 . C14 . H143 . 108.5 no
C16 . C15 . C17 . 107.98(7) yes
C16 . C15 . C18 . 108.11(7) yes
C17 . C15 . C18 . 109.94(7) yes
C16 . C15 . P2 . 109.60(7) yes
C17 . C15 . P2 . 114.52(7) yes
C18 . C15 . P2 . 106.52(7) yes
C15 . C16 . H163 . 109.5 no
C15 . C16 . H162 . 109.6 no
H163 . C16 . H162 . 109.1 no
C15 . C16 . H161 . 110.3 no
H163 . C16 . H161 . 108.8 no
H162 . C16 . H161 . 109.5 no
C15 . C17 . H171 . 109.6 no
C15 . C17 . H172 . 110.3 no
H171 . C17 . H172 . 108.8 no
C15 . C17 . H173 . 109.8 no
H171 . C17 . H173 . 108.8 no
H172 . C17 . H173 . 109.6 no
C15 . C18 . H181 . 110.3 no
C15 . C18 . H182 . 108.9 no
H181 . C18 . H182 . 110.5 no
C15 . C18 . H183 . 108.8 no
H181 . C18 . H183 . 108.6 no
H182 . C18 . H183 . 109.8 no
C20 . C19 . C21 . 105.58(7) yes
C20 . C19 . C22 . 107.19(7) yes
C21 . C19 . C22 . 111.38(7) yes
C20 . C19 . P2 . 109.74(7) yes
C21 . C19 . P2 . 110.63(6) yes
C22 . C19 . P2 . 112.05(7) yes
C19 . C20 . H203 . 110.1 no
C19 . C20 . H202 . 110.5 no
H203 . C20 . H202 . 108.9 no
C19 . C20 . H201 . 109.5 no
H203 . C20 . H201 . 108.6 no
H202 . C20 . H201 . 109.2 no
C19 . C21 . H211 . 110.7 no
C19 . C21 . H212 . 109.8 no
H211 . C21 . H212 . 108.9 no
C19 . C21 . H213 . 109.0 no
H211 . C21 . H213 . 109.3 no
H212 . C21 . H213 . 109.2 no
C19 . C22 . H221 . 109.1 no
C19 . C22 . H222 . 110.0 no
H221 . C22 . H222 . 109.5 no
C19 . C22 . H223 . 110.2 no
H221 . C22 . H223 . 108.7 no
H222 . C22 . H223 . 109.4 no
C1 . Ti1 . Cl3 . 116.84(5) yes
C1 . Ti1 . Cl2 . 145.28(5) yes
Cl3 . Ti1 . Cl2 . 86.51(3) yes
C1 . Ti1 . Cl1 . 87.82(4) yes
Cl3 . Ti1 . Cl1 . 143.16(4) yes
Cl2 . Ti1 . Cl1 . 86.64(4) yes
C1 . Ti1 . P1 . 71.80(4) yes
Cl3 . Ti1 . P1 . 99.56(4) yes
Cl2 . Ti1 . P1 . 79.55(3) yes
Cl1 . Ti1 . P1 . 114.64(4) yes
C1 . Ti1 . P2 . 68.64(4) yes
Cl3 . Ti1 . P2 . 80.40(3) yes
Cl2 . Ti1 . P2 . 144.47(4) yes
Cl1 . Ti1 . P2 . 84.51(4) yes
P1 . Ti1 . P2 . 135.04(4) yes
C7 . P1 . C11 . 112.27(6) yes
C7 . P1 . Ti1 . 116.83(6) yes
C11 . P1 . Ti1 . 118.29(5) yes
C7 . P1 . O1 . 99.71(6) yes
C11 . P1 . O1 . 101.06(6) yes
Ti1 . P1 . O1 . 104.98(6) yes
C2 . O1 . P1 . 115.07(9) yes
C6 . O2 . P2 . 110.24(8) yes
C19 . P2 . C15 . 109.57(6) yes
C19 . P2 . Ti1 . 118.57(5) yes
C15 . P2 . Ti1 . 121.14(5) yes
C19 . P2 . O2 . 102.40(6) yes
C15 . P2 . O2 . 100.97(6) yes
Ti1 . P2 . O2 . 99.78(5) 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 . C17 . 134 0.96 2.53 3.2745(10) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 

# start Validation Reply Form
_vrf_PLAT230_2                   
;
PROBLEM: Hirshfeld Test Diff for    P1       --O1       .       52.3 s.u.  
RESPONSE: There was a drop off in high angle data, which has resulted
in somewhat higher S.U.. Atomic assignments are correct and restrainst not
necessary.
;
_vrf_PLAT915_2                   
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         31 %     
RESPONSE: Absolute structure not required so full Friedel
Pair coverage not undertaken.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_6B
_database_code_depnum_ccdc_archive 'CCDC 2204759'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;


_chemical_name_systematic        .
_chemical_melting_point          'not measured'
_cell_length_a                   15.4564(2)
_cell_length_b                   12.7270(2)
_cell_length_c                   15.5888(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.7926(14)
_cell_angle_gamma                90
_cell_volume                     3038.21(7)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_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 0.2191 1.8069 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'
O 0.0492 0.0322 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'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.6763 1.2805 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0181 0.0091 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 = C28 H43 Br1 O2 P2 Ti1 
# Dc =      1.31 Fooo =   1256.00 Mu =     50.84 M =    601.40
# Found Formula = C28 H44 Br1 O2 P2 Ti1 
# Dc =      1.32 FOOO =   1260.00 Mu =     50.84 M =    602.41

_chemical_formula_sum            'C28 H44 Br1 O2 P2 Ti1'
_chemical_formula_moiety         'C28 H44 Br1 O2 P2 Ti1'
_chemical_compound_source        .
_chemical_formula_weight         602.41


_cell_measurement_reflns_used    4024
_cell_measurement_theta_min      3.76
_cell_measurement_theta_max      73.07
_cell_measurement_temperature    173

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_max          0.300

_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1260
_exptl_absorpt_coefficient_mu    5.084

# Sheldrick geometric approximatio 0.22 0.60 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_T_max  0.60
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_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      173
_diffrn_reflns_number            10033
_diffrn_reflns_av_unetI/netI     0.077
_reflns_number_total             5799
_diffrn_reflns_av_R_equivalents  0.042
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 5799 
# Theoretical number of reflections is about 12249 


_diffrn_reflns_theta_min         3.779
_diffrn_reflns_theta_max         73.525
_diffrn_measured_fraction_theta_max 0.948

_diffrn_reflns_theta_full        73.525


_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       10
_reflns_limit_h_min              -19
_reflns_limit_h_max              18
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   2.41
_oxford_diffrn_Wilson_scale      0.38

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

_refine_diff_density_min         -0.90
_refine_diff_density_max         0.67


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

# Explicitly named reflections are ALWAYS excluded from R&wR 

# The values actually used during refinement 
# These are labelled "all" for compatibility with PLATON 
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_number_restraints     799
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5799
_oxford_refine_ls_R_factor_ref   0.0629
_refine_ls_R_factor_all          0.0629
_refine_ls_wR_factor_ref         0.1124
_refine_ls_wR_factor_all         0.1124
_refine_ls_goodness_of_fit_ref   0.9051
_refine_ls_shift/su_max          0.0046890
_refine_ls_shift/su_mean         0.0006436


# Computed with I/sigma = -10 
_oxford_reflns_number_all        5799
_oxford_refine_ls_R_factor_all   0.0629
_oxford_refine_ls_wR_factor_all  0.1124

# Computed with no filters except I/sigma = +2 a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4303
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_gt          0.0707


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method = Chebychev polynomial, (Carruthers & Watkin, 1979) 
 W = 1.0/[A[0]*T[0]'(X)+A[1]*T[1]'(X) ... +A[NP-1]*T[NP-1]'(X)] 
 146. 177. 44.8 
;

# 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 0.58168(9) 0.17672(9) 0.85665(9) 0.0252 1.0000 Uani . U . . . .
C2 C 0.58395(9) 0.26088(9) 0.91442(9) 0.0298 1.0000 Uani . U . . . .
C3 C 0.64602(7) 0.27447(7) 0.98742(7) 0.0353 1.0000 Uani . U . . . .
C4 C 0.70978(7) 0.19908(7) 1.00472(7) 0.0369 1.0000 Uani . U . . . .
C5 C 0.71140(7) 0.11277(7) 0.95218(7) 0.0352 1.0000 Uani . U . . . .
C6 C 0.64822(9) 0.10343(9) 0.88012(9) 0.0266 1.0000 Uani . U . . . .
C7 C 0.34985(9) 0.28647(9) 0.89389(9) 0.0447 1.0000 Uani . U . . . .
C8 C 0.26028(5) 0.29426(5) 0.83884(5) 0.0630 1.0000 Uani . U . . . .
C9 C 0.36725(5) 0.17151(5) 0.92000(5) 0.0493 1.0000 Uani . U . . . .
C10 C 0.35243(5) 0.35351(5) 0.97641(5) 0.0719 1.0000 Uani . U . . . .
C11 C 0.42384(9) 0.45750(9) 0.78150(9) 0.0376 1.0000 Uani . U . . . .
C12 C 0.35578(5) 0.45497(5) 0.70129(5) 0.0517 1.0000 Uani . U . . . .
C13 C 0.51232(5) 0.48954(5) 0.75507(5) 0.0588 1.0000 Uani . U . . . .
C14 C 0.39897(5) 0.53898(5) 0.84643(5) 0.0447 1.0000 Uani . U . . . .
C15 C 0.52364(9) -0.12315(9) 0.77807(9) 0.0483 1.0000 Uani . U . . . .
C16 C 0.46545(5) -0.16921(5) 0.69888(5) 0.0677 1.0000 Uani . U . . . .
C17 C 0.58425(5) -0.20820(5) 0.82428(5) 0.0693 1.0000 Uani . U . . . .
C18 C 0.46498(5) -0.08310(5) 0.84352(5) 0.0599 1.0000 Uani . U . . . .
C19 C 0.65364(9) -0.03421(9) 0.66162(9) 0.0496 1.0000 Uani . U . . . .
C20 C 0.59708(5) -0.01942(5) 0.57302(5) 0.0739 1.0000 Uani . U . . . .
C21 C 0.69259(5) -0.14520(5) 0.66650(5) 0.0713 1.0000 Uani . U . . . .
C22 C 0.72684(5) 0.04598(5) 0.67254(5) 0.0665 1.0000 Uani . U . . . .
C23 C 0.53128(9) 0.25371(9) 0.63192(9) 0.0302 1.0000 Uani . U . . . .
C24 C 0.61710(7) 0.29516(7) 0.64677(7) 0.0394 1.0000 Uani . U . . . .
C25 C 0.64951(7) 0.35991(7) 0.58735(7) 0.0518 1.0000 Uani . U . . . .
C26 C 0.59823(7) 0.38625(7) 0.51195(7) 0.0579 1.0000 Uani . U . . . .
C27 C 0.51376(7) 0.34682(7) 0.49444(7) 0.0522 1.0000 Uani . U . . . .
C28 C 0.48177(7) 0.28079(7) 0.55298(7) 0.0378 1.0000 Uani . U . . . .
P2 P 0.58190(6) -0.00439(7) 0.74574(6) 0.0283 1.0000 Uani . U . . . .
P1 P 0.43793(6) 0.32203(7) 0.82703(6) 0.0286 1.0000 Uani . U . . . .
Br1 Br 0.34689(4) 0.10435(5) 0.66667(4) 0.0436 1.0000 Uani . U . . . .
Ti1 Ti 0.49025(5) 0.16919(5) 0.73497(5) 0.0229 1.0000 Uani . U . . . .
O2 O 0.65359(9) 0.01193(9) 0.83205(9) 0.0334 1.0000 Uani . U . . . .
O1 O 0.52105(9) 0.34150(9) 0.90208(9) 0.0442 1.0000 Uani . U . . . .
H31 H 0.6439 0.3331 1.0229 0.0422 1.0000 Uiso R . . . . .
H41 H 0.7521 0.2068 1.0524 0.0440 1.0000 Uiso R . . . . .
H51 H 0.7534 0.0615 0.9640 0.0424 1.0000 Uiso R . . . . .
H82 H 0.2434 0.3663 0.8312 0.0950 1.0000 Uiso R . . . . .
H81 H 0.2179 0.2578 0.8670 0.0950 1.0000 Uiso R . . . . .
H83 H 0.2626 0.2633 0.7830 0.0952 1.0000 Uiso R . . . . .
H93 H 0.4224 0.1642 0.9550 0.0758 1.0000 Uiso R . . . . .
H91 H 0.3225 0.1484 0.9519 0.0760 1.0000 Uiso R . . . . .
H92 H 0.3660 0.1286 0.8699 0.0761 1.0000 Uiso R . . . . .
H101 H 0.4118 0.3660 1.0005 0.1051 1.0000 Uiso R . . . . .
H102 H 0.3231 0.3168 1.0174 0.1050 1.0000 Uiso R . . . . .
H103 H 0.3232 0.4190 0.9626 0.1048 1.0000 Uiso R . . . . .
H123 H 0.2997 0.4349 0.7166 0.0801 1.0000 Uiso R . . . . .
H121 H 0.3520 0.5236 0.6758 0.0802 1.0000 Uiso R . . . . .
H122 H 0.3730 0.4054 0.6606 0.0799 1.0000 Uiso R . . . . .
H131 H 0.5553 0.4947 0.8057 0.0896 1.0000 Uiso R . . . . .
H132 H 0.5069 0.5565 0.7265 0.0899 1.0000 Uiso R . . . . .
H133 H 0.5301 0.4379 0.7163 0.0900 1.0000 Uiso R . . . . .
H142 H 0.4360 0.5309 0.9005 0.0678 1.0000 Uiso R . . . . .
H143 H 0.4067 0.6084 0.8244 0.0680 1.0000 Uiso R . . . . .
H141 H 0.3390 0.5294 0.8550 0.0679 1.0000 Uiso R . . . . .
H161 H 0.4303 -0.1147 0.6698 0.1059 1.0000 Uiso R . . . . .
H162 H 0.4284 -0.2226 0.7171 0.1061 1.0000 Uiso R . . . . .
H163 H 0.5014 -0.1993 0.6598 0.1058 1.0000 Uiso R . . . . .
H172 H 0.6269 -0.1750 0.8662 0.1060 1.0000 Uiso R . . . . .
H173 H 0.5505 -0.2577 0.8523 0.1059 1.0000 Uiso R . . . . .
H171 H 0.6132 -0.2437 0.7821 0.1059 1.0000 Uiso R . . . . .
H181 H 0.5004 -0.0454 0.8891 0.0878 1.0000 Uiso R . . . . .
H183 H 0.4380 -0.1419 0.8677 0.0879 1.0000 Uiso R . . . . .
H182 H 0.4207 -0.0383 0.8143 0.0878 1.0000 Uiso R . . . . .
H202 H 0.5755 0.0519 0.5681 0.1119 1.0000 Uiso R . . . . .
H201 H 0.6316 -0.0336 0.5275 0.1120 1.0000 Uiso R . . . . .
H203 H 0.5485 -0.0678 0.5680 0.1120 1.0000 Uiso R . . . . .
H211 H 0.7217 -0.1582 0.7235 0.1059 1.0000 Uiso R . . . . .
H213 H 0.7339 -0.1510 0.6262 0.1059 1.0000 Uiso R . . . . .
H212 H 0.6468 -0.1956 0.6528 0.1060 1.0000 Uiso R . . . . .
H222 H 0.7599 0.0378 0.7288 0.1020 1.0000 Uiso R . . . . .
H221 H 0.7644 0.0362 0.6292 0.1020 1.0000 Uiso R . . . . .
H223 H 0.7027 0.1150 0.6670 0.1020 1.0000 Uiso R . . . . .
H241 H 0.6529 0.2789 0.6979 0.0459 1.0000 Uiso R . . . . .
H251 H 0.7068 0.3853 0.5991 0.0602 1.0000 Uiso R . . . . .
H261 H 0.6192 0.4308 0.4722 0.0721 1.0000 Uiso R . . . . .
H271 H 0.4783 0.3651 0.4431 0.0631 1.0000 Uiso R . . . . .
H281 H 0.4255 0.2540 0.5400 0.0471 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.3013(19)
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 . 1.3967(18) yes
C1 . C6 . 1.3999(18) yes
C1 . Ti1 . 2.2086(15) yes
C2 . C3 . 1.3962(16) yes
C2 . O1 . 1.4087(18) yes
C3 . C4 . 1.3757(13) yes
C3 . H31 . 0.932 no
C4 . C5 . 1.3724(13) yes
C4 . H41 . 0.926 no
C5 . C6 . 1.3899(16) yes
C5 . H51 . 0.922 no
C6 . O2 . 1.3934(17) yes
C7 . C8 . 1.5299(15) yes
C7 . C9 . 1.5326(13) yes
C7 . C10 . 1.5396(15) yes
C7 . P1 . 1.8787(18) yes
C8 . H82 . 0.957 no
C8 . H81 . 0.956 no
C8 . H83 . 0.961 no
C9 . H93 . 0.953 no
C9 . H91 . 0.951 no
C9 . H92 . 0.951 no
C10 . H101 . 0.956 no
C10 . H102 . 0.955 no
C10 . H103 . 0.959 no
C11 . C12 . 1.5213(15) yes
C11 . C13 . 1.5360(16) yes
C11 . C14 . 1.5340(15) yes
C11 . P1 . 1.8660(15) yes
C12 . H123 . 0.965 no
C12 . H121 . 0.958 no
C12 . H122 . 0.958 no
C13 . H131 . 0.962 no
C13 . H132 . 0.960 no
C13 . H133 . 0.958 no
C14 . H142 . 0.958 no
C14 . H143 . 0.961 no
C14 . H141 . 0.962 no
C15 . C16 . 1.5412(15) yes
C15 . C17 . 1.5444(14) yes
C15 . C18 . 1.5408(17) yes
C15 . P2 . 1.8633(16) yes
C16 . H161 . 0.957 no
C16 . H162 . 0.956 no
C16 . H163 . 0.958 no
C17 . H172 . 0.961 no
C17 . H173 . 0.959 no
C17 . H171 . 0.957 no
C18 . H181 . 0.964 no
C18 . H183 . 0.958 no
C18 . H182 . 0.957 no
C19 . C20 . 1.5427(15) yes
C19 . C21 . 1.5334(14) yes
C19 . C22 . 1.5160(15) yes
C19 . P2 . 1.8676(18) yes
C20 . H202 . 0.967 no
C20 . H201 . 0.961 no
C20 . H203 . 0.965 no
C21 . H211 . 0.955 no
C21 . H213 . 0.957 no
C21 . H212 . 0.958 no
C22 . H222 . 0.959 no
C22 . H221 . 0.957 no
C22 . H223 . 0.954 no
C23 . C24 . 1.4170(17) yes
C23 . C28 . 1.4011(16) yes
C23 . Ti1 . 2.1014(16) yes
C24 . C25 . 1.3836(14) yes
C24 . H241 . 0.930 no
C25 . C26 . 1.3673(13) yes
C25 . H251 . 0.937 no
C26 . C27 . 1.3907(14) yes
C26 . H261 . 0.930 no
C27 . C28 . 1.3805(14) yes
C27 . H271 . 0.936 no
C28 . H281 . 0.931 no
P2 . Ti1 . 2.6174(11) yes
P2 . O2 . 1.6361(15) yes
P1 . Ti1 . 2.6100(11) yes
P1 . O1 . 1.6350(16) yes
Br1 . Ti1 . 2.4667(9) 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 . C6 . 112.90(12) yes
C2 . C1 . Ti1 . 122.97(9) yes
C6 . C1 . Ti1 . 123.88(10) yes
C1 . C2 . C3 . 125.10(11) yes
C1 . C2 . O1 . 120.94(12) yes
C3 . C2 . O1 . 113.97(11) yes
C2 . C3 . C4 . 117.91(9) yes
C2 . C3 . H31 . 120.5 no
C4 . C3 . H31 . 121.6 no
C3 . C4 . C5 . 120.78(9) yes
C3 . C4 . H41 . 119.6 no
C5 . C4 . H41 . 119.7 no
C4 . C5 . C6 . 118.89(9) yes
C4 . C5 . H51 . 121.1 no
C6 . C5 . H51 . 120.0 no
C1 . C6 . C5 . 124.40(11) yes
C1 . C6 . O2 . 120.76(12) yes
C5 . C6 . O2 . 114.81(11) yes
C8 . C7 . C9 . 108.89(8) yes
C8 . C7 . C10 . 110.59(9) yes
C9 . C7 . C10 . 108.88(9) yes
C8 . C7 . P1 . 109.99(9) yes
C9 . C7 . P1 . 105.25(8) yes
C10 . C7 . P1 . 113.04(8) yes
C7 . C8 . H82 . 110.0 no
C7 . C8 . H81 . 109.6 no
H82 . C8 . H81 . 109.2 no
C7 . C8 . H83 . 109.9 no
H82 . C8 . H83 . 108.9 no
H81 . C8 . H83 . 109.2 no
C7 . C9 . H93 . 110.9 no
C7 . C9 . H91 . 108.7 no
H93 . C9 . H91 . 109.1 no
C7 . C9 . H92 . 110.3 no
H93 . C9 . H92 . 109.4 no
H91 . C9 . H92 . 108.4 no
C7 . C10 . H101 . 109.6 no
C7 . C10 . H102 . 109.1 no
H101 . C10 . H102 . 109.7 no
C7 . C10 . H103 . 109.7 no
H101 . C10 . H103 . 110.0 no
H102 . C10 . H103 . 108.9 no
C12 . C11 . C13 . 109.08(10) yes
C12 . C11 . C14 . 110.45(9) yes
C13 . C11 . C14 . 108.03(8) yes
C12 . C11 . P1 . 108.97(8) yes
C13 . C11 . P1 . 106.56(8) yes
C14 . C11 . P1 . 113.60(9) yes
C11 . C12 . H123 . 110.3 no
C11 . C12 . H121 . 108.6 no
H123 . C12 . H121 . 109.7 no
C11 . C12 . H122 . 109.5 no
H123 . C12 . H122 . 109.2 no
H121 . C12 . H122 . 109.4 no
C11 . C13 . H131 . 109.8 no
C11 . C13 . H132 . 109.6 no
H131 . C13 . H132 . 109.1 no
C11 . C13 . H133 . 109.3 no
H131 . C13 . H133 . 109.8 no
H132 . C13 . H133 . 109.3 no
C11 . C14 . H142 . 109.5 no
C11 . C14 . H143 . 109.3 no
H142 . C14 . H143 . 108.9 no
C11 . C14 . H141 . 109.8 no
H142 . C14 . H141 . 109.6 no
H143 . C14 . H141 . 109.6 no
C16 . C15 . C17 . 110.99(8) yes
C16 . C15 . C18 . 108.92(9) yes
C17 . C15 . C18 . 107.29(9) yes
C16 . C15 . P2 . 110.05(9) yes
C17 . C15 . P2 . 114.20(9) yes
C18 . C15 . P2 . 105.07(7) yes
C15 . C16 . H161 . 109.6 no
C15 . C16 . H162 . 109.9 no
H161 . C16 . H162 . 109.4 no
C15 . C16 . H163 . 109.6 no
H161 . C16 . H163 . 109.2 no
H162 . C16 . H163 . 109.1 no
C15 . C17 . H172 . 109.0 no
C15 . C17 . H173 . 109.9 no
H172 . C17 . H173 . 110.1 no
C15 . C17 . H171 . 108.7 no
H172 . C17 . H171 . 109.5 no
H173 . C17 . H171 . 109.7 no
C15 . C18 . H181 . 109.0 no
C15 . C18 . H183 . 109.2 no
H181 . C18 . H183 . 109.4 no
C15 . C18 . H182 . 109.2 no
H181 . C18 . H182 . 110.6 no
H183 . C18 . H182 . 109.4 no
C20 . C19 . C21 . 109.14(9) yes
C20 . C19 . C22 . 110.01(9) yes
C21 . C19 . C22 . 109.42(9) yes
C20 . C19 . P2 . 106.59(9) yes
C21 . C19 . P2 . 114.76(9) yes
C22 . C19 . P2 . 106.83(8) yes
C19 . C20 . H202 . 109.4 no
C19 . C20 . H201 . 109.5 no
H202 . C20 . H201 . 109.8 no
C19 . C20 . H203 . 109.6 no
H202 . C20 . H203 . 109.7 no
H201 . C20 . H203 . 108.9 no
C19 . C21 . H211 . 109.8 no
C19 . C21 . H213 . 109.3 no
H211 . C21 . H213 . 109.1 no
C19 . C21 . H212 . 109.4 no
H211 . C21 . H212 . 109.4 no
H213 . C21 . H212 . 110.0 no
C19 . C22 . H222 . 109.0 no
C19 . C22 . H221 . 110.4 no
H222 . C22 . H221 . 109.5 no
C19 . C22 . H223 . 109.5 no
H222 . C22 . H223 . 109.6 no
H221 . C22 . H223 . 108.9 no
C24 . C23 . C28 . 116.08(11) yes
C24 . C23 . Ti1 . 116.00(9) yes
C28 . C23 . Ti1 . 127.72(10) yes
C23 . C24 . C25 . 121.89(10) yes
C23 . C24 . H241 . 119.5 no
C25 . C24 . H241 . 118.6 no
C24 . C25 . C26 . 120.08(9) yes
C24 . C25 . H251 . 119.6 no
C26 . C25 . H251 . 120.4 no
C25 . C26 . C27 . 119.98(9) yes
C25 . C26 . H261 . 120.6 no
C27 . C26 . H261 . 119.5 no
C26 . C27 . C28 . 120.05(9) yes
C26 . C27 . H271 . 120.2 no
C28 . C27 . H271 . 119.8 no
C23 . C28 . C27 . 121.90(10) yes
C23 . C28 . H281 . 119.0 no
C27 . C28 . H281 . 119.1 no
C19 . P2 . C15 . 112.32(7) yes
C19 . P2 . Ti1 . 119.61(6) yes
C15 . P2 . Ti1 . 115.14(6) yes
C19 . P2 . O2 . 101.70(8) yes
C15 . P2 . O2 . 100.30(8) yes
Ti1 . P2 . O2 . 104.24(6) yes
C7 . P1 . C11 . 112.19(7) yes
C7 . P1 . Ti1 . 115.30(6) yes
C11 . P1 . Ti1 . 120.55(7) yes
C7 . P1 . O1 . 101.40(8) yes
C11 . P1 . O1 . 99.90(7) yes
Ti1 . P1 . O1 . 103.56(6) yes
P2 . Ti1 . P1 . 143.04(4) yes
P2 . Ti1 . C1 . 72.77(4) yes
P1 . Ti1 . C1 . 72.86(4) yes
P2 . Ti1 . Br1 . 101.07(3) yes
P1 . Ti1 . Br1 . 99.18(4) yes
C1 . Ti1 . Br1 . 144.88(5) yes
P2 . Ti1 . C23 . 105.33(5) yes
P1 . Ti1 . C23 . 100.78(5) yes
C1 . Ti1 . C23 . 114.21(6) yes
Br1 . Ti1 . C23 . 100.83(5) yes
C6 . O2 . P2 . 117.73(10) yes
C2 . O1 . P1 . 116.62(10) 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
C13 . H133 . C24 . 163 0.96 2.58 3.5120(13) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 

# start Validation Reply Form

_vrf_PLAT230_6B                  
;
PROBLEM: Hirshfeld Test Diff for    P2       --C15      .       12.8 s.u.  
RESPONSE: Failing Hirshfeld is not unusual for organometallic
compounds. Assignment of atoms is correct and applying
restraints on ADPs not necessary. 
;
_vrf_PLAT934_6B                  
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          5 Check 
RESPONSE: This is not a significant number of outliers
and not indicative of a systematic issue.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 2204760'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;

_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   17.1600(3)
_cell_length_b                   17.1600(3)
_cell_length_c                   21.1327(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6222.9(3)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P -4 21 c '
_symmetry_space_group_name_Hall  'P -4 2n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y+1/2,-x+1/2,z+1/2
-y,x,-z
-x,-y,z
y+1/2,x+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2
y,-x,-z
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 0.2191 1.8069 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'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 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'
C 0.0181 0.0091 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'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C27 H50 Cl1 O2 P2 Ti1 
# Dc =      1.18 Fooo =   2376.00 Mu =     42.38 M =    551.99
# Found Formula = C27 H50 Cl1 O2 P2 Ti1 
# Dc =      1.18 FOOO =   2376.00 Mu =     42.38 M =    551.99

_chemical_formula_sum            'C27 H50 Cl1 O2 P2 Ti1'
_chemical_formula_moiety         'C27 H50 Cl1 O2 P2 Ti1'
_chemical_compound_source        .
_chemical_formula_weight         551.99


_cell_measurement_reflns_used    4633
_cell_measurement_theta_min      5
_cell_measurement_theta_max      72
_cell_measurement_temperature    173

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.200
_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             2376
_exptl_absorpt_coefficient_mu    4.238

# Sheldrick geometric approximatio 0.43 0.43 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_T_max  0.43
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_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      173
_diffrn_reflns_number            11746
_diffrn_reflns_av_unetI/netI     0.054
_reflns_number_total             3386
_diffrn_reflns_av_R_equivalents  0.036
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 3386 
# Theoretical number of reflections is about 6257 


_diffrn_reflns_theta_min         3.318
_diffrn_reflns_theta_max         73.380
_diffrn_measured_fraction_theta_max 0.984

_diffrn_reflns_theta_full        69.711
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              0
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              21
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   2.91
_oxford_diffrn_Wilson_scale      0.34

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

_refine_diff_density_min         -0.36
_refine_diff_density_max         1.42


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3386
_oxford_refine_ls_R_factor_ref   0.0626
_refine_ls_wR_factor_ref         0.1585
_refine_ls_goodness_of_fit_ref   0.9087
_refine_ls_shift/su_max          0.0003845
_refine_ls_shift/su_mean         0.0000206


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3386
_refine_ls_R_factor_all          0.0626
_refine_ls_wR_factor_all         0.1585

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3092
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_gt          0.1539

# For an explanation, see Cooper & Watkin, Acta Cryst. (2016). B72, 661-683 
_oxford_Hooft_y                  0. # for 0 Friedel pairs 
_oxford_Bijvoet_difference       0. # for 0 Friedel pairs 
# (Similar to the Parsons(q).) 
_oxford_refined_Flack_x          . # for 0 Friedel pairs 
# NOTE: The Flack parameter was determined before Friedel pairs were merged 
_refine_ls_abs_structure_Flack   0.
_refine_ls_abs_structure_details 
; 
 Parsons, Flack & Wagner (2013), 
 0 Friedel Pairs 
;

# 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 ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.10P)² +10.48P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.2614(5) 0.6076(3) 0.6458(3) 0.0480 1.0000 Uani . . . . . .
C2 C 0.2618(5) 0.5355(3) 0.6891(3) 0.0508 1.0000 Uani . . . . . .
C3 C 0.3318(5) 0.4833(5) 0.6737(5) 0.0726 1.0000 Uani . . . . . .
C4 C 0.2648(8) 0.5628(5) 0.7576(4) 0.0866 1.0000 Uani . . . . . .
C5 C 0.1882(5) 0.4870(4) 0.6784(4) 0.0632 1.0000 Uani . . . . . .
C6 C 0.2314(3) 0.7442(3) 0.5208(2) 0.0345 1.0000 Uani . . . . . .
C7 C 0.2938(3) 0.7468(4) 0.4778(3) 0.0380 1.0000 Uani . . . . . .
C8 C 0.2852(3) 0.7475(4) 0.4116(3) 0.0413 1.0000 Uani . . . . . .
C9 C 0.2118(4) 0.7469(4) 0.3872(3) 0.0451 1.0000 Uani . . . . . .
C10 C 0.1469(3) 0.7467(4) 0.4261(3) 0.0439 1.0000 Uani . . . . . .
C11 C 0.1592(3) 0.7454(4) 0.4911(2) 0.0385 1.0000 Uani . . . . . .
C12 C 0.4707(4) 0.6912(4) 0.5851(3) 0.0505 1.0000 Uani . . . . . .
C13 C 0.4479(5) 0.6127(4) 0.5542(4) 0.0582 1.0000 Uani . . . . . .
C14 C 0.5451(4) 0.7199(5) 0.5538(4) 0.0692 1.0000 Uani . . . . . .
C15 C 0.4847(5) 0.6781(5) 0.6562(4) 0.0678 1.0000 Uani . . . . . .
C16 C 0.4150(4) 0.8631(4) 0.5821(3) 0.0500 1.0000 Uani . . . . . .
C17 C 0.4662(5) 0.8883(6) 0.5276(4) 0.0746 1.0000 Uani . . . . . .
C18 C 0.4551(5) 0.8774(5) 0.6461(4) 0.0680 1.0000 Uani . . . . . .
C19 C 0.3394(5) 0.9094(4) 0.5802(4) 0.0607 1.0000 Uani . . . . . .
C20 C 0.0297(4) 0.6787(4) 0.6303(4) 0.0509 1.0000 Uani . . . . . .
C21 C 0.0427(6) 0.6613(5) 0.6999(4) 0.0686 1.0000 Uani . . . . . .
C22 C -0.0565(4) 0.6982(6) 0.6168(5) 0.0728 1.0000 Uani . . . . . .
C23 C 0.0500(5) 0.6059(4) 0.5909(4) 0.0612 1.0000 Uani . . . . . .
C24 C 0.0630(4) 0.8553(4) 0.6189(4) 0.0519 1.0000 Uani . . . . . .
C25 C 0.1324(5) 0.9085(4) 0.6026(4) 0.0645 1.0000 Uani . . . . . .
C26 C 0.0424(5) 0.8649(5) 0.6875(4) 0.0662 1.0000 Uani . . . . . .
C27 C -0.0048(6) 0.8769(5) 0.5758(5) 0.0774 1.0000 Uani . . . . . .
Ti1 Ti 0.24802(6) 0.72203(5) 0.62346(4) 0.0330 1.0000 Uani . . . . . .
Cl1 Cl 0.26105(10) 0.79078(7) 0.72070(6) 0.0440 1.0000 Uani . . . . . .
P2 P 0.10044(8) 0.75411(9) 0.60429(7) 0.0371 1.0000 Uani . . . . . .
O2 O 0.0906(2) 0.7486(3) 0.52735(18) 0.0483 1.0000 Uani . . . . . .
O1 O 0.3703(2) 0.7490(3) 0.49884(18) 0.0496 1.0000 Uani . . . . . .
P1 P 0.38460(8) 0.75724(9) 0.57570(7) 0.0393 1.0000 Uani . . . . . .
H11 H 0.3179 0.6134 0.6482 0.0604 1.0000 Uiso R . . . . .
H12 H 0.2476 0.5844 0.6053 0.0603 1.0000 Uiso R . . . . .
H31 H 0.3365 0.4420 0.7042 0.1100 1.0000 Uiso R . . . . .
H32 H 0.3788 0.5143 0.6741 0.1100 1.0000 Uiso R . . . . .
H33 H 0.3253 0.4609 0.6319 0.1100 1.0000 Uiso R . . . . .
H41 H 0.2624 0.5187 0.7859 0.1330 1.0000 Uiso R . . . . .
H42 H 0.3124 0.5906 0.7643 0.1330 1.0000 Uiso R . . . . .
H43 H 0.2218 0.5971 0.7652 0.1331 1.0000 Uiso R . . . . .
H51 H 0.1921 0.4386 0.7009 0.0940 1.0000 Uiso R . . . . .
H52 H 0.1430 0.5153 0.6931 0.0937 1.0000 Uiso R . . . . .
H53 H 0.1828 0.4766 0.6338 0.0940 1.0000 Uiso R . . . . .
H81 H 0.3282 0.7486 0.3849 0.0512 1.0000 Uiso R . . . . .
H91 H 0.2048 0.7460 0.3439 0.0530 1.0000 Uiso R . . . . .
H101 H 0.0962 0.7484 0.4094 0.0551 1.0000 Uiso R . . . . .
H131 H 0.3977 0.5970 0.5705 0.0849 1.0000 Uiso R . . . . .
H132 H 0.4862 0.5736 0.5650 0.0851 1.0000 Uiso R . . . . .
H133 H 0.4452 0.6176 0.5089 0.0851 1.0000 Uiso R . . . . .
H141 H 0.5621 0.7675 0.5731 0.0991 1.0000 Uiso R . . . . .
H142 H 0.5857 0.6818 0.5595 0.0991 1.0000 Uiso R . . . . .
H143 H 0.5371 0.7281 0.5091 0.0991 1.0000 Uiso R . . . . .
H151 H 0.5027 0.7263 0.6749 0.1011 1.0000 Uiso R . . . . .
H152 H 0.5230 0.6375 0.6620 0.1009 1.0000 Uiso R . . . . .
H153 H 0.4362 0.6624 0.6761 0.1011 1.0000 Uiso R . . . . .
H171 H 0.4453 0.8694 0.4880 0.1070 1.0000 Uiso R . . . . .
H172 H 0.4688 0.9441 0.5265 0.1070 1.0000 Uiso R . . . . .
H173 H 0.5178 0.8673 0.5343 0.1070 1.0000 Uiso R . . . . .
H182 H 0.4265 0.8518 0.6794 0.1110 1.0000 Uiso R . . . . .
H181 H 0.4568 0.9326 0.6544 0.1108 1.0000 Uiso R . . . . .
H183 H 0.5072 0.8575 0.6440 0.1110 1.0000 Uiso R . . . . .
H192 H 0.3074 0.8906 0.6141 0.0889 1.0000 Uiso R . . . . .
H191 H 0.3515 0.9638 0.5862 0.0890 1.0000 Uiso R . . . . .
H193 H 0.3143 0.9012 0.5399 0.0890 1.0000 Uiso R . . . . .
H212 H 0.0978 0.6602 0.7080 0.1040 1.0000 Uiso R . . . . .
H211 H 0.0192 0.7015 0.7252 0.1041 1.0000 Uiso R . . . . .
H213 H 0.0210 0.6116 0.7105 0.1040 1.0000 Uiso R . . . . .
H222 H -0.0641 0.7066 0.5723 0.1172 1.0000 Uiso R . . . . .
H221 H -0.0709 0.7451 0.6388 0.1170 1.0000 Uiso R . . . . .
H223 H -0.0890 0.6561 0.6306 0.1170 1.0000 Uiso R . . . . .
H232 H 0.0446 0.6166 0.5461 0.0989 1.0000 Uiso R . . . . .
H231 H 0.1020 0.5885 0.5995 0.0990 1.0000 Uiso R . . . . .
H233 H 0.0144 0.5650 0.6022 0.0991 1.0000 Uiso R . . . . .
H252 H 0.1490 0.8996 0.5595 0.0940 1.0000 Uiso R . . . . .
H251 H 0.1178 0.9623 0.6077 0.0938 1.0000 Uiso R . . . . .
H253 H 0.1745 0.8966 0.6312 0.0938 1.0000 Uiso R . . . . .
H262 H -0.0021 0.8333 0.6966 0.0971 1.0000 Uiso R . . . . .
H261 H 0.0302 0.9189 0.6952 0.0971 1.0000 Uiso R . . . . .
H263 H 0.0859 0.8487 0.7132 0.0970 1.0000 Uiso R . . . . .
H272 H -0.0495 0.8461 0.5873 0.1110 1.0000 Uiso R . . . . .
H271 H -0.0166 0.9315 0.5822 0.1110 1.0000 Uiso R . . . . .
H273 H 0.0098 0.8679 0.5324 0.1111 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.756(19)
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 . 1.539(8) yes
C1 . Ti1 . 2.033(6) yes
C1 . H11 . 0.976 no
C1 . H12 . 0.973 no
C2 . C3 . 1.533(11) yes
C2 . C4 . 1.522(10) yes
C2 . C5 . 1.530(11) yes
C3 . H31 . 0.962 no
C3 . H32 . 0.966 no
C3 . H33 . 0.969 no
C4 . H41 . 0.965 no
C4 . H42 . 0.956 no
C4 . H43 . 0.958 no
C5 . H51 . 0.958 no
C5 . H52 . 0.967 no
C5 . H53 . 0.962 no
C6 . C7 . 1.404(8) yes
C6 . C11 . 1.389(8) yes
C6 . Ti1 . 2.222(5) yes
C7 . C8 . 1.407(8) yes
C7 . O1 . 1.386(7) yes
C8 . C9 . 1.362(8) yes
C8 . H81 . 0.928 no
C9 . C10 . 1.384(8) yes
C9 . H91 . 0.923 no
C10 . C11 . 1.390(7) yes
C10 . H101 . 0.940 no
C11 . O2 . 1.406(7) yes
C12 . C13 . 1.546(10) yes
C12 . C14 . 1.519(10) yes
C12 . C15 . 1.539(10) yes
C12 . P1 . 1.872(7) yes
C13 . H131 . 0.967 no
C13 . H132 . 0.967 no
C13 . H133 . 0.963 no
C14 . H141 . 0.959 no
C14 . H142 . 0.962 no
C14 . H143 . 0.965 no
C15 . H151 . 0.967 no
C15 . H152 . 0.965 no
C15 . H153 . 0.970 no
C16 . C17 . 1.512(10) yes
C16 . C18 . 1.537(10) yes
C16 . C19 . 1.522(10) yes
C16 . P1 . 1.894(7) yes
C17 . H171 . 0.967 no
C17 . H172 . 0.959 no
C17 . H173 . 0.966 no
C18 . H182 . 0.964 no
C18 . H181 . 0.962 no
C18 . H183 . 0.958 no
C19 . H192 . 0.958 no
C19 . H191 . 0.965 no
C19 . H193 . 0.964 no
C20 . C21 . 1.518(10) yes
C20 . C22 . 1.543(10) yes
C20 . C23 . 1.543(10) yes
C20 . P2 . 1.857(7) yes
C21 . H212 . 0.962 no
C21 . H211 . 0.960 no
C21 . H213 . 0.957 no
C22 . H222 . 0.962 no
C22 . H221 . 0.961 no
C22 . H223 . 0.958 no
C23 . H232 . 0.969 no
C23 . H231 . 0.958 no
C23 . H233 . 0.960 no
C24 . C25 . 1.539(11) yes
C24 . C26 . 1.500(11) yes
C24 . C27 . 1.524(11) yes
C24 . P2 . 1.878(7) yes
C25 . H252 . 0.966 no
C25 . H251 . 0.962 no
C25 . H253 . 0.964 no
C26 . H262 . 0.957 no
C26 . H261 . 0.964 no
C26 . H263 . 0.963 no
C27 . H272 . 0.963 no
C27 . H271 . 0.968 no
C27 . H273 . 0.964 no
Ti1 . Cl1 . 2.3799(14) yes
Ti1 . P2 . 2.6232(17) yes
Ti1 . P1 . 2.6223(17) yes
P2 . O2 . 1.638(4) yes
O1 . P1 . 1.649(4) 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 . Ti1 . 156.3(5) yes
C2 . C1 . H11 . 92.7 no
Ti1 . C1 . H11 . 91.4 no
C2 . C1 . H12 . 101.3 no
Ti1 . C1 . H12 . 99.4 no
H11 . C1 . H12 . 109.1 no
C1 . C2 . C3 . 110.3(6) yes
C1 . C2 . C4 . 108.5(5) yes
C3 . C2 . C4 . 110.8(8) yes
C1 . C2 . C5 . 110.2(6) yes
C3 . C2 . C5 . 107.3(6) yes
C4 . C2 . C5 . 109.7(8) yes
C2 . C3 . H31 . 110.7 no
C2 . C3 . H32 . 109.2 no
H31 . C3 . H32 . 109.2 no
C2 . C3 . H33 . 109.7 no
H31 . C3 . H33 . 109.2 no
H32 . C3 . H33 . 108.8 no
C2 . C4 . H41 . 110.3 no
C2 . C4 . H42 . 108.9 no
H41 . C4 . H42 . 109.6 no
C2 . C4 . H43 . 108.8 no
H41 . C4 . H43 . 110.2 no
H42 . C4 . H43 . 109.0 no
C2 . C5 . H51 . 109.9 no
C2 . C5 . H52 . 109.9 no
H51 . C5 . H52 . 109.3 no
C2 . C5 . H53 . 109.0 no
H51 . C5 . H53 . 109.5 no
H52 . C5 . H53 . 109.2 no
C7 . C6 . C11 . 112.9(5) yes
C7 . C6 . Ti1 . 122.6(4) yes
C11 . C6 . Ti1 . 123.9(4) yes
C6 . C7 . C8 . 124.3(5) yes
C6 . C7 . O1 . 121.0(5) yes
C8 . C7 . O1 . 114.7(5) yes
C7 . C8 . C9 . 118.2(5) yes
C7 . C8 . H81 . 121.4 no
C9 . C8 . H81 . 120.3 no
C8 . C9 . C10 . 121.3(5) yes
C8 . C9 . H91 . 119.7 no
C10 . C9 . H91 . 118.9 no
C9 . C10 . C11 . 117.7(5) yes
C9 . C10 . H101 . 121.4 no
C11 . C10 . H101 . 120.9 no
C10 . C11 . C6 . 125.6(5) yes
C10 . C11 . O2 . 114.2(5) yes
C6 . C11 . O2 . 120.2(5) yes
C13 . C12 . C14 . 108.1(6) yes
C13 . C12 . C15 . 108.9(7) yes
C14 . C12 . C15 . 109.9(7) yes
C13 . C12 . P1 . 106.5(5) yes
C14 . C12 . P1 . 114.9(5) yes
C15 . C12 . P1 . 108.4(5) yes
C12 . C13 . H131 . 108.6 no
C12 . C13 . H132 . 109.5 no
H131 . C13 . H132 . 109.1 no
C12 . C13 . H133 . 110.9 no
H131 . C13 . H133 . 109.7 no
H132 . C13 . H133 . 109.1 no
C12 . C14 . H141 . 110.2 no
C12 . C14 . H142 . 109.6 no
H141 . C14 . H142 . 107.8 no
C12 . C14 . H143 . 110.7 no
H141 . C14 . H143 . 109.6 no
H142 . C14 . H143 . 109.0 no
C12 . C15 . H151 . 108.9 no
C12 . C15 . H152 . 109.6 no
H151 . C15 . H152 . 110.3 no
C12 . C15 . H153 . 109.3 no
H151 . C15 . H153 . 109.6 no
H152 . C15 . H153 . 109.2 no
C17 . C16 . C18 . 111.3(7) yes
C17 . C16 . C19 . 109.0(6) yes
C18 . C16 . C19 . 108.8(7) yes
C17 . C16 . P1 . 112.3(6) yes
C18 . C16 . P1 . 109.9(5) yes
C19 . C16 . P1 . 105.3(5) yes
C16 . C17 . H171 . 110.4 no
C16 . C17 . H172 . 109.4 no
H171 . C17 . H172 . 109.3 no
C16 . C17 . H173 . 108.3 no
H171 . C17 . H173 . 110.0 no
H172 . C17 . H173 . 109.4 no
C16 . C18 . H182 . 110.0 no
C16 . C18 . H181 . 109.3 no
H182 . C18 . H181 . 109.3 no
C16 . C18 . H183 . 108.7 no
H182 . C18 . H183 . 110.3 no
H181 . C18 . H183 . 109.3 no
C16 . C19 . H192 . 107.0 no
C16 . C19 . H191 . 108.6 no
H192 . C19 . H191 . 110.5 no
C16 . C19 . H193 . 109.1 no
H192 . C19 . H193 . 110.8 no
H191 . C19 . H193 . 110.7 no
C21 . C20 . C22 . 111.2(7) yes
C21 . C20 . C23 . 109.3(6) yes
C22 . C20 . C23 . 107.0(6) yes
C21 . C20 . P2 . 109.2(6) yes
C22 . C20 . P2 . 114.9(6) yes
C23 . C20 . P2 . 104.9(5) yes
C20 . C21 . H212 . 108.7 no
C20 . C21 . H211 . 109.6 no
H212 . C21 . H211 . 109.2 no
C20 . C21 . H213 . 110.2 no
H212 . C21 . H213 . 109.0 no
H211 . C21 . H213 . 110.2 no
C20 . C22 . H222 . 110.1 no
C20 . C22 . H221 . 109.8 no
H222 . C22 . H221 . 108.2 no
C20 . C22 . H223 . 109.8 no
H222 . C22 . H223 . 109.4 no
H221 . C22 . H223 . 109.6 no
C20 . C23 . H232 . 110.6 no
C20 . C23 . H231 . 111.1 no
H232 . C23 . H231 . 109.6 no
C20 . C23 . H233 . 108.3 no
H232 . C23 . H233 . 108.7 no
H231 . C23 . H233 . 108.6 no
C25 . C24 . C26 . 109.5(7) yes
C25 . C24 . C27 . 108.2(7) yes
C26 . C24 . C27 . 111.8(7) yes
C25 . C24 . P2 . 104.3(5) yes
C26 . C24 . P2 . 109.9(5) yes
C27 . C24 . P2 . 112.8(5) yes
C24 . C25 . H252 . 110.1 no
C24 . C25 . H251 . 110.0 no
H252 . C25 . H251 . 109.5 no
C24 . C25 . H253 . 108.3 no
H252 . C25 . H253 . 109.6 no
H251 . C25 . H253 . 109.2 no
C24 . C26 . H262 . 108.7 no
C24 . C26 . H261 . 108.7 no
H262 . C26 . H261 . 109.6 no
C24 . C26 . H263 . 109.3 no
H262 . C26 . H263 . 110.0 no
H261 . C26 . H263 . 110.5 no
C24 . C27 . H272 . 108.9 no
C24 . C27 . H271 . 108.1 no
H272 . C27 . H271 . 109.3 no
C24 . C27 . H273 . 109.4 no
H272 . C27 . H273 . 110.9 no
H271 . C27 . H273 . 110.2 no
C6 . Ti1 . C1 . 114.0(2) yes
C6 . Ti1 . Cl1 . 140.40(15) yes
C1 . Ti1 . Cl1 . 105.52(17) yes
C6 . Ti1 . P2 . 71.91(14) yes
C1 . Ti1 . P2 . 110.3(2) yes
Cl1 . Ti1 . P2 . 96.89(6) yes
C6 . Ti1 . P1 . 72.48(14) yes
C1 . Ti1 . P1 . 102.2(2) yes
Cl1 . Ti1 . P1 . 97.71(6) yes
P2 . Ti1 . P1 . 139.03(6) yes
C24 . P2 . C20 . 111.8(3) yes
C24 . P2 . Ti1 . 119.9(2) yes
C20 . P2 . Ti1 . 116.0(2) yes
C24 . P2 . O2 . 100.5(3) yes
C20 . P2 . O2 . 100.7(3) yes
Ti1 . P2 . O2 . 103.94(16) yes
C11 . O2 . P2 . 117.2(3) yes
C7 . O1 . P1 . 117.3(3) yes
C16 . P1 . C12 . 110.8(3) yes
C16 . P1 . Ti1 . 116.1(2) yes
C12 . P1 . Ti1 . 121.7(2) yes
C16 . P1 . O1 . 101.2(3) yes
C12 . P1 . O1 . 99.8(3) yes
Ti1 . P1 . O1 . 103.07(16) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 

####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 2204761'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_cell_length_a                   10.79430(10)
_cell_length_b                   22.1846(3)
_cell_length_c                   27.3239(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.8675(10)
_cell_angle_gamma                90
_cell_volume                     6539.70(13)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,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
C 0.0181 0.0091 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'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 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'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ti 0.2191 1.8069 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'
Si 0.2541 0.3302 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C52 H104 Cl2 O4 P4 Si2 Ti2 
# Dc =      1.16 Fooo =   2456.00 Mu =     43.85 M =   1140.17
# Found Formula = C52 H104 Cl2 O4 P4 Si2 Ti2 
# Dc =      1.16 FOOO =   2456.00 Mu =     43.85 M =   1140.17

_chemical_formula_sum            'C52 H104 Cl2 O4 P4 Si2 Ti2'
_chemical_formula_moiety         'C44 H80 Cl2 O4 P4 Ti2, 2(C4 H12 Si)'
_chemical_compound_source        .
_chemical_formula_weight         1140.17


_cell_measurement_reflns_used    8619
_cell_measurement_theta_min      4
_cell_measurement_theta_max      73
_cell_measurement_temperature    173

_exptl_crystal_description       block
_exptl_crystal_colour            'clear dark purple'
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.300

_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2456
_exptl_absorpt_coefficient_mu    4.385

# Sheldrick geometric approximatio 0.42 0.64 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_T_max  0.64
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_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      173
_diffrn_reflns_number            21714
_diffrn_reflns_av_unetI/netI     0.075
_reflns_number_total             12534
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 12534 
# Theoretical number of reflections is about 26371 


_diffrn_reflns_theta_min         3.801
_diffrn_reflns_theta_max         73.549
_diffrn_measured_fraction_theta_max 0.950

_diffrn_reflns_theta_full        73.549



_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       33
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              27
_reflns_limit_l_min              0
_reflns_limit_l_max              33

_oxford_diffrn_Wilson_B_factor   3.35
_oxford_diffrn_Wilson_scale      0.25

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

_refine_diff_density_min         -0.74
_refine_diff_density_max         3.23


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     596
_refine_ls_number_reflns         12534
_oxford_refine_ls_R_factor_ref   0.0898
_refine_ls_wR_factor_ref         0.1945
_refine_ls_goodness_of_fit_ref   0.9828
_refine_ls_shift/su_max          0.0007370
_refine_ls_shift/su_mean         0.0000339


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        12534
_refine_ls_R_factor_all          0.0898
_refine_ls_wR_factor_all         0.1945

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9694
_refine_ls_R_factor_gt           0.0725
_refine_ls_wR_factor_gt          0.1755


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² +13.38P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.1664(4) 0.6562(2) 0.70443(16) 0.0441 1.0000 Uani . . . . . .
C2 C 0.1727(4) 0.6892(2) 0.74823(16) 0.0459 1.0000 Uani . . . . . .
C3 C 0.2805(4) 0.6980(2) 0.77689(17) 0.0488 1.0000 Uani . . . . . .
C4 C 0.3890(4) 0.6716(3) 0.76198(18) 0.0516 1.0000 Uani . . . . . .
C5 C 0.3900(4) 0.6358(2) 0.72022(17) 0.0489 1.0000 Uani . . . . . .
C6 C 0.2793(4) 0.6295(2) 0.69336(16) 0.0426 1.0000 Uani . . . . . .
C7 C -0.1607(4) 0.7650(3) 0.75010(16) 0.0509 1.0000 Uani . . . . . .
C8 C -0.0845(5) 0.8164(3) 0.72933(19) 0.0617 1.0000 Uani . . . . . .
C9 C -0.1935(6) 0.7832(3) 0.80216(19) 0.0667 1.0000 Uani . . . . . .
C10 C -0.2808(5) 0.7563(3) 0.71851(19) 0.0589 1.0000 Uani . . . . . .
C11 C -0.1126(5) 0.6384(3) 0.79158(17) 0.0589 1.0000 Uani . . . . . .
C12 C -0.0404(6) 0.5808(3) 0.7813(2) 0.0674 1.0000 Uani . . . . . .
C13 C -0.0769(7) 0.6583(3) 0.84410(19) 0.0785 1.0000 Uani . . . . . .
C14 C -0.2517(6) 0.6240(3) 0.7866(2) 0.0735 1.0000 Uani . . . . . .
C15 C 0.2205(4) 0.5802(2) 0.55656(16) 0.0445 1.0000 Uani . . . . . .
C16 C 0.2697(5) 0.6443(2) 0.5514(2) 0.0583 1.0000 Uani . . . . . .
C17 C 0.1115(5) 0.5729(3) 0.5203(2) 0.0688 1.0000 Uani . . . . . .
C18 C 0.3250(5) 0.5368(2) 0.5447(2) 0.0564 1.0000 Uani . . . . . .
C19 C 0.1489(5) 0.4929(2) 0.6383(2) 0.0565 1.0000 Uani . . . . . .
C20 C 0.0531(7) 0.4618(3) 0.6053(2) 0.0736 1.0000 Uani . . . . . .
C21 C 0.2701(7) 0.4594(3) 0.6399(3) 0.0887 1.0000 Uani . . . . . .
C22 C 0.1027(6) 0.4934(3) 0.6910(2) 0.0650 1.0000 Uani . . . . . .
C23 C 0.0504(4) 0.7568(2) 0.51213(15) 0.0425 1.0000 Uani . . . . . .
C24 C 0.1687(4) 0.7793(2) 0.50383(15) 0.0400 1.0000 Uani . . . . . .
C25 C 0.2337(4) 0.7698(2) 0.46135(16) 0.0463 1.0000 Uani . . . . . .
C26 C 0.1781(5) 0.7370(2) 0.42405(16) 0.0504 1.0000 Uani . . . . . .
C27 C 0.0599(4) 0.7139(2) 0.42867(16) 0.0461 1.0000 Uani . . . . . .
C28 C -0.0001(4) 0.7245(2) 0.47211(16) 0.0438 1.0000 Uani . . . . . .
C29 C 0.1347(6) 0.9171(3) 0.5736(3) 0.0684 1.0000 Uani . . . . . .
C30 C 0.2468(7) 0.9476(3) 0.5516(3) 0.0902 1.0000 Uani . . . . . .
C31 C 0.0951(8) 0.9497(3) 0.6197(3) 0.0943 1.0000 Uani . . . . . .
C32 C 0.0277(7) 0.9184(3) 0.5356(3) 0.0865 1.0000 Uani . . . . . .
C33 C 0.2865(4) 0.8262(2) 0.63574(16) 0.0471 1.0000 Uani . . . . . .
C34 C 0.3990(5) 0.8667(3) 0.6303(2) 0.0670 1.0000 Uani . . . . . .
C35 C 0.3343(5) 0.7610(3) 0.6307(2) 0.0622 1.0000 Uani . . . . . .
C36 C 0.2336(6) 0.8320(3) 0.68620(19) 0.0650 1.0000 Uani . . . . . .
C37 C -0.3044(5) 0.7837(3) 0.48150(17) 0.0562 1.0000 Uani . . . . . .
C38 C -0.3445(6) 0.7641(3) 0.42912(19) 0.0716 1.0000 Uani . . . . . .
C39 C -0.2206(6) 0.8392(3) 0.4763(2) 0.0641 1.0000 Uani . . . . . .
C40 C -0.4174(5) 0.8020(3) 0.51081(19) 0.0613 1.0000 Uani . . . . . .
C41 C -0.3065(4) 0.6578(2) 0.52683(16) 0.0475 1.0000 Uani . . . . . .
C42 C -0.4020(5) 0.6409(3) 0.48666(19) 0.0578 1.0000 Uani . . . . . .
C43 C -0.2171(5) 0.6043(3) 0.53237(19) 0.0604 1.0000 Uani . . . . . .
C44 C -0.3715(4) 0.6679(3) 0.57556(17) 0.0548 1.0000 Uani . . . . . .
C45 C -0.3656(6) 0.9724(3) 0.5658(2) 0.0722 1.0000 Uani . . . . . .
C46 C -0.3138(11) 0.9846(5) 0.6752(3) 0.1301 1.0000 Uani . . . . . .
C47 C -0.2266(10) 1.0798(5) 0.6076(4) 0.1251 1.0000 Uani . . . . . .
C48 C -0.4981(10) 1.0660(6) 0.6238(5) 0.1849 1.0000 Uani . . . . . .
C49 C -0.3995(8) 0.4610(4) 0.7175(3) 0.0956 1.0000 Uani . . . . . .
C50 C -0.1945(5) 0.3798(3) 0.6846(2) 0.0700 1.0000 Uani . . . . . .
C51 C -0.3616(7) 0.4414(4) 0.6085(2) 0.0866 1.0000 Uani . . . . . .
C52 C -0.4622(6) 0.3404(3) 0.6698(3) 0.0796 1.0000 Uani . . . . . .
Ti1 Ti -0.00210(7) 0.65254(4) 0.65626(3) 0.0399 1.0000 Uani . . . . . .
Ti2 Ti -0.04112(7) 0.76283(4) 0.58357(3) 0.0413 1.0000 Uani . . . . . .
Cl2 Cl -0.18317(12) 0.83225(7) 0.61059(4) 0.0579 1.0000 Uani . . . . . .
P4 P -0.20962(10) 0.72547(6) 0.51603(4) 0.0463 1.0000 Uani . . . . . .
O4 O -0.1205(3) 0.7007(2) 0.47286(12) 0.0593 1.0000 Uani . . . . . .
O3 O 0.2321(3) 0.81294(17) 0.53948(11) 0.0517 1.0000 Uani . . . . . .
P3 P 0.15903(11) 0.83516(5) 0.58786(4) 0.0425 1.0000 Uani . . . . . .
Cl1 Cl -0.16791(11) 0.58632(7) 0.65650(4) 0.0575 1.0000 Uani . . . . . .
P2 P 0.16285(10) 0.57446(5) 0.62056(4) 0.0405 1.0000 Uani . . . . . .
O2 O 0.2897(3) 0.59357(17) 0.65143(12) 0.0506 1.0000 Uani . . . . . .
O1 O 0.0677(3) 0.71801(19) 0.76621(12) 0.0587 1.0000 Uani . . . . . .
P1 P -0.06720(10) 0.69479(7) 0.74388(4) 0.0472 1.0000 Uani . . . . . .
Si1 Si -0.35097(15) 1.02553(8) 0.61804(7) 0.0656 1.0000 Uani . . . . . .
Si2 Si -0.35535(13) 0.40646(8) 0.67010(5) 0.0552 1.0000 Uani . . . . . .
H2 H 0.0079 0.7378 0.6514 0.1051 1.0000 Uiso R . . . . .
H1 H -0.0347 0.6762 0.5864 0.1051 1.0000 Uiso R . . . . .
H31 H 0.2793 0.7214 0.8060 0.0588 1.0000 Uiso R . . . . .
H41 H 0.4639 0.6782 0.7804 0.0623 1.0000 Uiso R . . . . .
H51 H 0.4636 0.6162 0.7105 0.0592 1.0000 Uiso R . . . . .
H81 H -0.0624 0.8067 0.6969 0.0748 1.0000 Uiso R . . . . .
H82 H -0.1324 0.8523 0.7290 0.0748 1.0000 Uiso R . . . . .
H83 H -0.0116 0.8222 0.7492 0.0748 1.0000 Uiso R . . . . .
H91 H -0.2410 0.7521 0.8163 0.0811 1.0000 Uiso R . . . . .
H92 H -0.2404 0.8195 0.8011 0.0811 1.0000 Uiso R . . . . .
H93 H -0.1196 0.7893 0.8213 0.0811 1.0000 Uiso R . . . . .
H101 H -0.3278 0.7242 0.7316 0.0718 1.0000 Uiso R . . . . .
H102 H -0.3282 0.7923 0.7188 0.0718 1.0000 Uiso R . . . . .
H103 H -0.2604 0.7469 0.6858 0.0718 1.0000 Uiso R . . . . .
H121 H -0.0605 0.5671 0.7491 0.0808 1.0000 Uiso R . . . . .
H122 H -0.0615 0.5506 0.8042 0.0808 1.0000 Uiso R . . . . .
H123 H 0.0459 0.5889 0.7843 0.0808 1.0000 Uiso R . . . . .
H131 H -0.1206 0.6941 0.8517 0.0952 1.0000 Uiso R . . . . .
H132 H -0.0977 0.6274 0.8665 0.0952 1.0000 Uiso R . . . . .
H133 H 0.0097 0.6657 0.8465 0.0952 1.0000 Uiso R . . . . .
H141 H -0.2981 0.6594 0.7929 0.0884 1.0000 Uiso R . . . . .
H142 H -0.2719 0.5936 0.8096 0.0884 1.0000 Uiso R . . . . .
H143 H -0.2710 0.6101 0.7544 0.0884 1.0000 Uiso R . . . . .
H161 H 0.3381 0.6502 0.5737 0.0709 1.0000 Uiso R . . . . .
H162 H 0.2061 0.6724 0.5584 0.0709 1.0000 Uiso R . . . . .
H163 H 0.2957 0.6503 0.5189 0.0709 1.0000 Uiso R . . . . .
H171 H 0.0789 0.5332 0.5228 0.0835 1.0000 Uiso R . . . . .
H172 H 0.0490 0.6014 0.5275 0.0835 1.0000 Uiso R . . . . .
H173 H 0.1385 0.5793 0.4880 0.0835 1.0000 Uiso R . . . . .
H181 H 0.2964 0.4965 0.5477 0.0684 1.0000 Uiso R . . . . .
H182 H 0.3934 0.5432 0.5668 0.0684 1.0000 Uiso R . . . . .
H183 H 0.3501 0.5436 0.5121 0.0684 1.0000 Uiso R . . . . .
H201 H -0.0223 0.4838 0.6052 0.0890 1.0000 Uiso R . . . . .
H202 H 0.0393 0.4222 0.6172 0.0890 1.0000 Uiso R . . . . .
H203 H 0.0825 0.4596 0.5730 0.0890 1.0000 Uiso R . . . . .
H211 H 0.3278 0.4802 0.6608 0.1075 1.0000 Uiso R . . . . .
H212 H 0.2581 0.4198 0.6521 0.1075 1.0000 Uiso R . . . . .
H213 H 0.3013 0.4572 0.6078 0.1075 1.0000 Uiso R . . . . .
H221 H 0.1622 0.5131 0.7118 0.0784 1.0000 Uiso R . . . . .
H222 H 0.0262 0.5145 0.6917 0.0784 1.0000 Uiso R . . . . .
H223 H 0.0912 0.4533 0.7020 0.0784 1.0000 Uiso R . . . . .
H251 H 0.3149 0.7855 0.4582 0.0557 1.0000 Uiso R . . . . .
H261 H 0.2211 0.7302 0.3948 0.0609 1.0000 Uiso R . . . . .
H271 H 0.0209 0.6914 0.4029 0.0555 1.0000 Uiso R . . . . .
H301 H 0.2689 0.9265 0.5229 0.1099 1.0000 Uiso R . . . . .
H302 H 0.2268 0.9882 0.5434 0.1099 1.0000 Uiso R . . . . .
H303 H 0.3145 0.9471 0.5747 0.1099 1.0000 Uiso R . . . . .
H311 H 0.0254 0.9300 0.6327 0.1117 1.0000 Uiso R . . . . .
H312 H 0.0742 0.9902 0.6119 0.1117 1.0000 Uiso R . . . . .
H313 H 0.1619 0.9491 0.6432 0.1117 1.0000 Uiso R . . . . .
H321 H -0.0430 0.8997 0.5487 0.1055 1.0000 Uiso R . . . . .
H322 H 0.0086 0.9590 0.5272 0.1055 1.0000 Uiso R . . . . .
H323 H 0.0512 0.8973 0.5071 0.1055 1.0000 Uiso R . . . . .
H341 H 0.3744 0.9076 0.6332 0.0808 1.0000 Uiso R . . . . .
H342 H 0.4594 0.8574 0.6552 0.0808 1.0000 Uiso R . . . . .
H343 H 0.4331 0.8603 0.5991 0.0808 1.0000 Uiso R . . . . .
H351 H 0.2674 0.7336 0.6338 0.0750 1.0000 Uiso R . . . . .
H352 H 0.3956 0.7532 0.6556 0.0750 1.0000 Uiso R . . . . .
H353 H 0.3693 0.7561 0.5995 0.0750 1.0000 Uiso R . . . . .
H361 H 0.1638 0.8062 0.6886 0.0784 1.0000 Uiso R . . . . .
H362 H 0.2090 0.8725 0.6914 0.0784 1.0000 Uiso R . . . . .
H363 H 0.2949 0.8209 0.7103 0.0784 1.0000 Uiso R . . . . .
H381 H -0.3967 0.7297 0.4307 0.0867 1.0000 Uiso R . . . . .
H382 H -0.3885 0.7960 0.4132 0.0867 1.0000 Uiso R . . . . .
H383 H -0.2733 0.7544 0.4112 0.0867 1.0000 Uiso R . . . . .
H391 H -0.1936 0.8529 0.5078 0.0774 1.0000 Uiso R . . . . .
H392 H -0.2658 0.8704 0.4599 0.0774 1.0000 Uiso R . . . . .
H393 H -0.1507 0.8287 0.4579 0.0774 1.0000 Uiso R . . . . .
H401 H -0.3908 0.8139 0.5428 0.0742 1.0000 Uiso R . . . . .
H402 H -0.4591 0.8346 0.4949 0.0742 1.0000 Uiso R . . . . .
H403 H -0.4722 0.7686 0.5128 0.0742 1.0000 Uiso R . . . . .
H421 H -0.4593 0.6731 0.4821 0.0703 1.0000 Uiso R . . . . .
H422 H -0.4450 0.6055 0.4960 0.0703 1.0000 Uiso R . . . . .
H423 H -0.3611 0.6336 0.4570 0.0703 1.0000 Uiso R . . . . .
H431 H -0.1559 0.6131 0.5571 0.0730 1.0000 Uiso R . . . . .
H432 H -0.2620 0.5694 0.5412 0.0730 1.0000 Uiso R . . . . .
H433 H -0.1781 0.5974 0.5022 0.0730 1.0000 Uiso R . . . . .
H441 H -0.3117 0.6784 0.6004 0.0663 1.0000 Uiso R . . . . .
H442 H -0.4302 0.6997 0.5717 0.0663 1.0000 Uiso R . . . . .
H443 H -0.4128 0.6320 0.5845 0.0663 1.0000 Uiso R . . . . .
H451 H -0.2894 0.9517 0.5622 0.0883 1.0000 Uiso R . . . . .
H452 H -0.3855 0.9942 0.5367 0.0883 1.0000 Uiso R . . . . .
H453 H -0.4295 0.9441 0.5717 0.0883 1.0000 Uiso R . . . . .
H461 H -0.3066 1.0125 0.7015 0.1627 1.0000 Uiso R . . . . .
H462 H -0.3785 0.9568 0.6813 0.1627 1.0000 Uiso R . . . . .
H463 H -0.2379 0.9633 0.6725 0.1627 1.0000 Uiso R . . . . .
H471 H -0.2198 1.1067 0.6346 0.1541 1.0000 Uiso R . . . . .
H472 H -0.2450 1.1019 0.5785 0.1541 1.0000 Uiso R . . . . .
H473 H -0.1505 1.0588 0.6044 0.1541 1.0000 Uiso R . . . . .
H481 H -0.4918 1.0933 0.6505 0.2309 1.0000 Uiso R . . . . .
H482 H -0.5176 1.0876 0.5946 0.2309 1.0000 Uiso R . . . . .
H483 H -0.5616 1.0374 0.6296 0.2309 1.0000 Uiso R . . . . .
H491 H -0.3446 0.4944 0.7174 0.1158 1.0000 Uiso R . . . . .
H492 H -0.3947 0.4421 0.7488 0.1158 1.0000 Uiso R . . . . .
H493 H -0.4819 0.4745 0.7109 0.1158 1.0000 Uiso R . . . . .
H501 H -0.1395 0.4132 0.6848 0.0845 1.0000 Uiso R . . . . .
H502 H -0.1915 0.3610 0.7158 0.0845 1.0000 Uiso R . . . . .
H503 H -0.1706 0.3517 0.6604 0.0845 1.0000 Uiso R . . . . .
H511 H -0.3075 0.4752 0.6082 0.1078 1.0000 Uiso R . . . . .
H512 H -0.4439 0.4542 0.6007 0.1078 1.0000 Uiso R . . . . .
H513 H -0.3365 0.4128 0.5849 0.1078 1.0000 Uiso R . . . . .
H521 H -0.5445 0.3535 0.6625 0.0970 1.0000 Uiso R . . . . .
H522 H -0.4587 0.3217 0.7011 0.0970 1.0000 Uiso R . . . . .
H523 H -0.4377 0.3124 0.6457 0.0970 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.086(16)

loop_
_oxford_twin_element_scale_factors
0.9983(3)
0.0017(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
C1 . C2 . 1.402(6) yes
C1 . C6 . 1.397(6) yes
C1 . Ti1 . 2.212(4) yes
C2 . C3 . 1.395(6) yes
C2 . O1 . 1.404(6) yes
C3 . C4 . 1.383(7) yes
C3 . H31 . 0.950 no
C4 . C5 . 1.390(7) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.388(6) yes
C5 . H51 . 0.950 no
C6 . O2 . 1.404(5) yes
C7 . C8 . 1.526(8) yes
C7 . C9 . 1.532(6) yes
C7 . C10 . 1.546(7) yes
C7 . P1 . 1.867(6) yes
C8 . H81 . 0.950 no
C8 . H82 . 0.950 no
C8 . H83 . 0.950 no
C9 . H91 . 0.950 no
C9 . H92 . 0.950 no
C9 . H93 . 0.950 no
C10 . H101 . 0.950 no
C10 . H102 . 0.950 no
C10 . H103 . 0.950 no
C11 . C12 . 1.528(8) yes
C11 . C13 . 1.538(7) yes
C11 . C14 . 1.536(8) yes
C11 . P1 . 1.883(6) yes
C12 . H121 . 0.950 no
C12 . H122 . 0.950 no
C12 . H123 . 0.950 no
C13 . H131 . 0.950 no
C13 . H132 . 0.950 no
C13 . H133 . 0.950 no
C14 . H141 . 0.950 no
C14 . H142 . 0.950 no
C14 . H143 . 0.950 no
C15 . C16 . 1.527(7) yes
C15 . C17 . 1.522(7) yes
C15 . C18 . 1.526(6) yes
C15 . P2 . 1.880(4) yes
C16 . H161 . 0.950 no
C16 . H162 . 0.950 no
C16 . H163 . 0.950 no
C17 . H171 . 0.950 no
C17 . H172 . 0.950 no
C17 . H173 . 0.950 no
C18 . H181 . 0.950 no
C18 . H182 . 0.950 no
C18 . H183 . 0.950 no
C19 . C20 . 1.516(8) yes
C19 . C21 . 1.505(8) yes
C19 . C22 . 1.540(7) yes
C19 . P2 . 1.880(6) yes
C20 . H201 . 0.950 no
C20 . H202 . 0.950 no
C20 . H203 . 0.950 no
C21 . H211 . 0.950 no
C21 . H212 . 0.950 no
C21 . H213 . 0.950 no
C22 . H221 . 0.950 no
C22 . H222 . 0.950 no
C22 . H223 . 0.950 no
C23 . C24 . 1.397(6) yes
C23 . C28 . 1.402(6) yes
C23 . Ti2 . 2.221(4) yes
C24 . C25 . 1.392(6) yes
C24 . O3 . 1.389(5) yes
C25 . C26 . 1.374(7) yes
C25 . H251 . 0.950 no
C26 . C27 . 1.385(7) yes
C26 . H261 . 0.950 no
C27 . C28 . 1.391(6) yes
C27 . H271 . 0.950 no
C28 . O4 . 1.404(6) yes
C29 . C30 . 1.527(9) yes
C29 . C31 . 1.525(10) yes
C29 . C32 . 1.528(9) yes
C29 . P3 . 1.875(6) yes
C30 . H301 . 0.950 no
C30 . H302 . 0.950 no
C30 . H303 . 0.950 no
C31 . H311 . 0.950 no
C31 . H312 . 0.950 no
C31 . H313 . 0.950 no
C32 . H321 . 0.950 no
C32 . H322 . 0.950 no
C32 . H323 . 0.950 no
C33 . C34 . 1.522(7) yes
C33 . C35 . 1.543(8) yes
C33 . C36 . 1.515(7) yes
C33 . P3 . 1.878(5) yes
C34 . H341 . 0.950 no
C34 . H342 . 0.950 no
C34 . H343 . 0.950 no
C35 . H351 . 0.950 no
C35 . H352 . 0.950 no
C35 . H353 . 0.950 no
C36 . H361 . 0.950 no
C36 . H362 . 0.950 no
C36 . H363 . 0.950 no
C37 . C38 . 1.544(7) yes
C37 . C39 . 1.539(8) yes
C37 . C40 . 1.535(7) yes
C37 . P4 . 1.882(6) yes
C38 . H381 . 0.950 no
C38 . H382 . 0.950 no
C38 . H383 . 0.950 no
C39 . H391 . 0.950 no
C39 . H392 . 0.950 no
C39 . H393 . 0.950 no
C40 . H401 . 0.950 no
C40 . H402 . 0.950 no
C40 . H403 . 0.950 no
C41 . C42 . 1.528(6) yes
C41 . C43 . 1.534(7) yes
C41 . C44 . 1.542(6) yes
C41 . P4 . 1.858(5) yes
C42 . H421 . 0.950 no
C42 . H422 . 0.950 no
C42 . H423 . 0.950 no
C43 . H431 . 0.950 no
C43 . H432 . 0.950 no
C43 . H433 . 0.950 no
C44 . H441 . 0.950 no
C44 . H442 . 0.950 no
C44 . H443 . 0.950 no
C45 . Si1 . 1.854(7) yes
C45 . H451 . 0.950 no
C45 . H452 . 0.950 no
C45 . H453 . 0.950 no
C46 . Si1 . 1.841(9) yes
C46 . H461 . 0.950 no
C46 . H462 . 0.950 no
C46 . H463 . 0.950 no
C47 . Si1 . 1.832(8) yes
C47 . H471 . 0.950 no
C47 . H472 . 0.950 no
C47 . H473 . 0.950 no
C48 . Si1 . 1.835(9) yes
C48 . H481 . 0.950 no
C48 . H482 . 0.950 no
C48 . H483 . 0.950 no
C49 . Si2 . 1.847(8) yes
C49 . H491 . 0.950 no
C49 . H492 . 0.950 no
C49 . H493 . 0.950 no
C50 . Si2 . 1.864(6) yes
C50 . H501 . 0.950 no
C50 . H502 . 0.950 no
C50 . H503 . 0.950 no
C51 . Si2 . 1.853(6) yes
C51 . H511 . 0.950 no
C51 . H512 . 0.950 no
C51 . H513 . 0.950 no
C52 . Si2 . 1.864(7) yes
C52 . H521 . 0.950 no
C52 . H522 . 0.950 no
C52 . H523 . 0.950 no
Ti1 . Ti2 . 3.1708(12) yes
Ti1 . Cl1 . 2.3157(14) yes
Ti1 . P2 . 2.6898(13) yes
Ti1 . P1 . 2.6858(13) yes
Ti1 . H2 . 1.899 no
Ti1 . H1 . 2.000 no
Ti2 . Cl2 . 2.3113(14) yes
Ti2 . P4 . 2.6799(13) yes
Ti2 . P3 . 2.6906(13) yes
Ti2 . H2 . 1.990 no
Ti2 . H1 . 1.925 no
P4 . O4 . 1.641(3) yes
O3 . P3 . 1.637(3) yes
P2 . O2 . 1.640(3) yes
O1 . P1 . 1.644(3) 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 . C6 . 112.8(4) yes
C2 . C1 . Ti1 . 122.9(3) yes
C6 . C1 . Ti1 . 124.2(3) yes
C1 . C2 . C3 . 124.6(4) yes
C1 . C2 . O1 . 121.3(4) yes
C3 . C2 . O1 . 114.1(4) yes
C2 . C3 . C4 . 118.3(4) yes
C2 . C3 . H31 . 120.9 no
C4 . C3 . H31 . 120.8 no
C3 . C4 . C5 . 120.9(4) yes
C3 . C4 . H41 . 119.5 no
C5 . C4 . H41 . 119.6 no
C4 . C5 . C6 . 117.5(4) yes
C4 . C5 . H51 . 121.2 no
C6 . C5 . H51 . 121.3 no
C1 . C6 . C5 . 125.8(4) yes
C1 . C6 . O2 . 120.7(4) yes
C5 . C6 . O2 . 113.5(4) yes
C8 . C7 . C9 . 107.0(5) yes
C8 . C7 . C10 . 109.8(4) yes
C9 . C7 . C10 . 109.6(4) yes
C8 . C7 . P1 . 106.9(4) yes
C9 . C7 . P1 . 116.6(4) yes
C10 . C7 . P1 . 106.9(4) yes
C7 . C8 . H81 . 109.5 no
C7 . C8 . H82 . 109.3 no
H81 . C8 . H82 . 109.5 no
C7 . C8 . H83 . 109.6 no
H81 . C8 . H83 . 109.5 no
H82 . C8 . H83 . 109.5 no
C7 . C9 . H91 . 109.3 no
C7 . C9 . H92 . 109.6 no
H91 . C9 . H92 . 109.5 no
C7 . C9 . H93 . 109.5 no
H91 . C9 . H93 . 109.5 no
H92 . C9 . H93 . 109.5 no
C7 . C10 . H101 . 109.4 no
C7 . C10 . H102 . 109.3 no
H101 . C10 . H102 . 109.5 no
C7 . C10 . H103 . 109.6 no
H101 . C10 . H103 . 109.5 no
H102 . C10 . H103 . 109.5 no
C12 . C11 . C13 . 107.3(5) yes
C12 . C11 . C14 . 108.2(6) yes
C13 . C11 . C14 . 110.9(5) yes
C12 . C11 . P1 . 106.4(3) yes
C13 . C11 . P1 . 113.1(5) yes
C14 . C11 . P1 . 110.7(4) yes
C11 . C12 . H121 . 109.6 no
C11 . C12 . H122 . 109.5 no
H121 . C12 . H122 . 109.5 no
C11 . C12 . H123 . 109.2 no
H121 . C12 . H123 . 109.5 no
H122 . C12 . H123 . 109.5 no
C11 . C13 . H131 . 109.5 no
C11 . C13 . H132 . 109.6 no
H131 . C13 . H132 . 109.5 no
C11 . C13 . H133 . 109.3 no
H131 . C13 . H133 . 109.5 no
H132 . C13 . H133 . 109.5 no
C11 . C14 . H141 . 109.4 no
C11 . C14 . H142 . 109.6 no
H141 . C14 . H142 . 109.5 no
C11 . C14 . H143 . 109.5 no
H141 . C14 . H143 . 109.5 no
H142 . C14 . H143 . 109.5 no
C16 . C15 . C17 . 107.7(5) yes
C16 . C15 . C18 . 107.8(4) yes
C17 . C15 . C18 . 110.8(5) yes
C16 . C15 . P2 . 105.9(3) yes
C17 . C15 . P2 . 109.1(3) yes
C18 . C15 . P2 . 115.1(3) yes
C15 . C16 . H161 . 109.5 no
C15 . C16 . H162 . 109.6 no
H161 . C16 . H162 . 109.5 no
C15 . C16 . H163 . 109.3 no
H161 . C16 . H163 . 109.5 no
H162 . C16 . H163 . 109.5 no
C15 . C17 . H171 . 109.3 no
C15 . C17 . H172 . 109.5 no
H171 . C17 . H172 . 109.5 no
C15 . C17 . H173 . 109.6 no
H171 . C17 . H173 . 109.5 no
H172 . C17 . H173 . 109.5 no
C15 . C18 . H181 . 109.3 no
C15 . C18 . H182 . 109.6 no
H181 . C18 . H182 . 109.5 no
C15 . C18 . H183 . 109.6 no
H181 . C18 . H183 . 109.5 no
H182 . C18 . H183 . 109.5 no
C20 . C19 . C21 . 111.5(6) yes
C20 . C19 . C22 . 108.9(5) yes
C21 . C19 . C22 . 106.5(5) yes
C20 . C19 . P2 . 110.2(4) yes
C21 . C19 . P2 . 114.0(4) yes
C22 . C19 . P2 . 105.4(4) yes
C19 . C20 . H201 . 109.6 no
C19 . C20 . H202 . 109.3 no
H201 . C20 . H202 . 109.5 no
C19 . C20 . H203 . 109.5 no
H201 . C20 . H203 . 109.5 no
H202 . C20 . H203 . 109.5 no
C19 . C21 . H211 . 109.2 no
C19 . C21 . H212 . 109.8 no
H211 . C21 . H212 . 109.5 no
C19 . C21 . H213 . 109.4 no
H211 . C21 . H213 . 109.5 no
H212 . C21 . H213 . 109.5 no
C19 . C22 . H221 . 109.3 no
C19 . C22 . H222 . 109.4 no
H221 . C22 . H222 . 109.5 no
C19 . C22 . H223 . 109.7 no
H221 . C22 . H223 . 109.5 no
H222 . C22 . H223 . 109.5 no
C24 . C23 . C28 . 113.0(4) yes
C24 . C23 . Ti2 . 123.8(3) yes
C28 . C23 . Ti2 . 122.9(3) yes
C23 . C24 . C25 . 124.7(4) yes
C23 . C24 . O3 . 120.7(4) yes
C25 . C24 . O3 . 114.6(4) yes
C24 . C25 . C26 . 118.7(4) yes
C24 . C25 . H251 . 120.7 no
C26 . C25 . H251 . 120.6 no
C25 . C26 . C27 . 120.6(4) yes
C25 . C26 . H261 . 119.7 no
C27 . C26 . H261 . 119.7 no
C26 . C27 . C28 . 118.1(4) yes
C26 . C27 . H271 . 120.9 no
C28 . C27 . H271 . 121.0 no
C23 . C28 . C27 . 124.9(4) yes
C23 . C28 . O4 . 121.2(4) yes
C27 . C28 . O4 . 113.9(4) yes
C30 . C29 . C31 . 111.1(6) yes
C30 . C29 . C32 . 108.3(6) yes
C31 . C29 . C32 . 109.0(6) yes
C30 . C29 . P3 . 113.9(5) yes
C31 . C29 . P3 . 109.2(5) yes
C32 . C29 . P3 . 105.0(4) yes
C29 . C30 . H301 . 109.2 no
C29 . C30 . H302 . 109.6 no
H301 . C30 . H302 . 109.5 no
C29 . C30 . H303 . 109.6 no
H301 . C30 . H303 . 109.5 no
H302 . C30 . H303 . 109.5 no
C29 . C31 . H311 . 109.7 no
C29 . C31 . H312 . 109.6 no
H311 . C31 . H312 . 109.5 no
C29 . C31 . H313 . 109.0 no
H311 . C31 . H313 . 109.5 no
H312 . C31 . H313 . 109.5 no
C29 . C32 . H321 . 109.4 no
C29 . C32 . H322 . 109.6 no
H321 . C32 . H322 . 109.5 no
C29 . C32 . H323 . 109.4 no
H321 . C32 . H323 . 109.5 no
H322 . C32 . H323 . 109.5 no
C34 . C33 . C35 . 105.9(4) yes
C34 . C33 . C36 . 111.3(4) yes
C35 . C33 . C36 . 107.3(5) yes
C34 . C33 . P3 . 116.0(4) yes
C35 . C33 . P3 . 106.1(3) yes
C36 . C33 . P3 . 109.6(4) yes
C33 . C34 . H341 . 109.3 no
C33 . C34 . H342 . 109.5 no
H341 . C34 . H342 . 109.5 no
C33 . C34 . H343 . 109.5 no
H341 . C34 . H343 . 109.5 no
H342 . C34 . H343 . 109.5 no
C33 . C35 . H351 . 109.5 no
C33 . C35 . H352 . 109.5 no
H351 . C35 . H352 . 109.5 no
C33 . C35 . H353 . 109.3 no
H351 . C35 . H353 . 109.5 no
H352 . C35 . H353 . 109.5 no
C33 . C36 . H361 . 109.5 no
C33 . C36 . H362 . 109.4 no
H361 . C36 . H362 . 109.5 no
C33 . C36 . H363 . 109.5 no
H361 . C36 . H363 . 109.5 no
H362 . C36 . H363 . 109.5 no
C38 . C37 . C39 . 106.7(5) yes
C38 . C37 . C40 . 110.7(5) yes
C39 . C37 . C40 . 108.4(5) yes
C38 . C37 . P4 . 113.8(4) yes
C39 . C37 . P4 . 106.5(4) yes
C40 . C37 . P4 . 110.4(4) yes
C37 . C38 . H381 . 109.3 no
C37 . C38 . H382 . 109.5 no
H381 . C38 . H382 . 109.5 no
C37 . C38 . H383 . 109.5 no
H381 . C38 . H383 . 109.5 no
H382 . C38 . H383 . 109.5 no
C37 . C39 . H391 . 109.6 no
C37 . C39 . H392 . 109.4 no
H391 . C39 . H392 . 109.5 no
C37 . C39 . H393 . 109.4 no
H391 . C39 . H393 . 109.5 no
H392 . C39 . H393 . 109.5 no
C37 . C40 . H401 . 109.5 no
C37 . C40 . H402 . 109.6 no
H401 . C40 . H402 . 109.5 no
C37 . C40 . H403 . 109.3 no
H401 . C40 . H403 . 109.5 no
H402 . C40 . H403 . 109.5 no
C42 . C41 . C43 . 106.8(4) yes
C42 . C41 . C44 . 109.9(4) yes
C43 . C41 . C44 . 109.3(4) yes
C42 . C41 . P4 . 117.0(4) yes
C43 . C41 . P4 . 106.6(3) yes
C44 . C41 . P4 . 107.1(4) yes
C41 . C42 . H421 . 109.3 no
C41 . C42 . H422 . 109.5 no
H421 . C42 . H422 . 109.5 no
C41 . C42 . H423 . 109.5 no
H421 . C42 . H423 . 109.5 no
H422 . C42 . H423 . 109.5 no
C41 . C43 . H431 . 109.4 no
C41 . C43 . H432 . 109.4 no
H431 . C43 . H432 . 109.5 no
C41 . C43 . H433 . 109.5 no
H431 . C43 . H433 . 109.5 no
H432 . C43 . H433 . 109.5 no
C41 . C44 . H441 . 109.5 no
C41 . C44 . H442 . 109.5 no
H441 . C44 . H442 . 109.5 no
C41 . C44 . H443 . 109.4 no
H441 . C44 . H443 . 109.5 no
H442 . C44 . H443 . 109.5 no
Si1 . C45 . H451 . 109.5 no
Si1 . C45 . H452 . 109.3 no
H451 . C45 . H452 . 109.5 no
Si1 . C45 . H453 . 109.5 no
H451 . C45 . H453 . 109.5 no
H452 . C45 . H453 . 109.5 no
Si1 . C46 . H461 . 109.3 no
Si1 . C46 . H462 . 109.0 no
H461 . C46 . H462 . 109.5 no
Si1 . C46 . H463 . 110.0 no
H461 . C46 . H463 . 109.5 no
H462 . C46 . H463 . 109.5 no
Si1 . C47 . H471 . 109.4 no
Si1 . C47 . H472 . 109.6 no
H471 . C47 . H472 . 109.5 no
Si1 . C47 . H473 . 109.5 no
H471 . C47 . H473 . 109.5 no
H472 . C47 . H473 . 109.5 no
Si1 . C48 . H481 . 109.7 no
Si1 . C48 . H482 . 110.1 no
H481 . C48 . H482 . 109.5 no
Si1 . C48 . H483 . 108.6 no
H481 . C48 . H483 . 109.5 no
H482 . C48 . H483 . 109.5 no
Si2 . C49 . H491 . 109.4 no
Si2 . C49 . H492 . 109.5 no
H491 . C49 . H492 . 109.5 no
Si2 . C49 . H493 . 109.6 no
H491 . C49 . H493 . 109.5 no
H492 . C49 . H493 . 109.5 no
Si2 . C50 . H501 . 109.4 no
Si2 . C50 . H502 . 109.5 no
H501 . C50 . H502 . 109.5 no
Si2 . C50 . H503 . 109.5 no
H501 . C50 . H503 . 109.5 no
H502 . C50 . H503 . 109.5 no
Si2 . C51 . H511 . 109.4 no
Si2 . C51 . H512 . 109.5 no
H511 . C51 . H512 . 109.5 no
Si2 . C51 . H513 . 109.5 no
H511 . C51 . H513 . 109.5 no
H512 . C51 . H513 . 109.5 no
Si2 . C52 . H521 . 109.5 no
Si2 . C52 . H522 . 109.5 no
H521 . C52 . H522 . 109.5 no
Si2 . C52 . H523 . 109.4 no
H521 . C52 . H523 . 109.5 no
H522 . C52 . H523 . 109.5 no
C1 . Ti1 . Ti2 . 115.72(13) yes
C1 . Ti1 . Cl1 . 129.99(14) yes
Ti2 . Ti1 . Cl1 . 113.85(4) yes
C1 . Ti1 . P2 . 72.44(13) yes
Ti2 . Ti1 . P2 . 110.22(4) yes
Cl1 . Ti1 . P2 . 96.50(5) yes
C1 . Ti1 . P1 . 71.98(12) yes
Ti2 . Ti1 . P1 . 104.82(4) yes
Cl1 . Ti1 . P1 . 89.67(5) yes
P2 . Ti1 . P1 . 138.03(5) yes
C1 . Ti1 . H2 . 87.5 no
Ti2 . Ti1 . H2 . 36.3 no
Cl1 . Ti1 . H2 . 132.7 no
P2 . Ti1 . H2 . 125.2 no
P1 . Ti1 . H2 . 74.5 no
C1 . Ti1 . H1 . 132.4 no
Ti2 . Ti1 . H1 . 35.3 no
Cl1 . Ti1 . H1 . 93.3 no
P2 . Ti1 . H1 . 85.5 no
P1 . Ti1 . H1 . 135.8 no
H2 . Ti1 . H1 . 71.4 no
Ti1 . Ti2 . C23 . 116.75(13) yes
Ti1 . Ti2 . Cl2 . 112.96(4) yes
C23 . Ti2 . Cl2 . 129.79(13) yes
Ti1 . Ti2 . P4 . 105.43(4) yes
C23 . Ti2 . P4 . 71.78(12) yes
Cl2 . Ti2 . P4 . 89.06(5) yes
Ti1 . Ti2 . P3 . 110.05(4) yes
C23 . Ti2 . P3 . 72.23(12) yes
Cl2 . Ti2 . P3 . 97.40(5) yes
P4 . Ti2 . P3 . 137.77(5) yes
Ti1 . Ti2 . H2 . 34.4 no
C23 . Ti2 . H2 . 133.6 no
Cl2 . Ti2 . H2 . 92.8 no
P4 . Ti2 . H2 . 135.1 no
P3 . Ti2 . H2 . 86.4 no
Ti1 . Ti2 . H1 . 36.9 no
C23 . Ti2 . H1 . 87.6 no
Cl2 . Ti2 . H1 . 132.5 no
P4 . Ti2 . H1 . 75.0 no
P3 . Ti2 . H1 . 124.5 no
H2 . Ti2 . H1 . 71.1 no
Ti2 . P4 . C37 . 118.61(18) yes
Ti2 . P4 . C41 . 120.87(15) yes
C37 . P4 . C41 . 109.5(2) yes
Ti2 . P4 . O4 . 101.43(12) yes
C37 . P4 . O4 . 101.0(2) yes
C41 . P4 . O4 . 100.9(2) yes
C28 . O4 . P4 . 116.7(3) yes
C24 . O3 . P3 . 119.2(3) yes
Ti2 . P3 . C33 . 122.40(15) yes
Ti2 . P3 . C29 . 117.5(2) yes
C33 . P3 . C29 . 110.0(2) yes
Ti2 . P3 . O3 . 101.11(12) yes
C33 . P3 . O3 . 99.7(2) yes
C29 . P3 . O3 . 101.1(3) yes
Ti1 . P2 . C19 . 117.81(17) yes
Ti1 . P2 . C15 . 122.48(15) yes
C19 . P2 . C15 . 109.7(2) yes
Ti1 . P2 . O2 . 101.45(12) yes
C19 . P2 . O2 . 100.9(2) yes
C15 . P2 . O2 . 99.50(19) yes
C6 . O2 . P2 . 118.6(3) yes
C2 . O1 . P1 . 116.3(3) yes
Ti1 . P1 . C11 . 117.82(18) yes
Ti1 . P1 . C7 . 122.02(15) yes
C11 . P1 . C7 . 109.7(2) yes
Ti1 . P1 . O1 . 100.71(12) yes
C11 . P1 . O1 . 101.5(2) yes
C7 . P1 . O1 . 100.4(2) yes
C45 . Si1 . C46 . 110.5(4) yes
C45 . Si1 . C48 . 109.0(4) yes
C46 . Si1 . C48 . 109.5(7) yes
C45 . Si1 . C47 . 110.0(4) yes
C46 . Si1 . C47 . 108.4(5) yes
C48 . Si1 . C47 . 109.4(7) yes
C52 . Si2 . C50 . 108.9(3) yes
C52 . Si2 . C51 . 108.7(3) yes
C50 . Si2 . C51 . 109.3(3) yes
C52 . Si2 . C49 . 110.1(4) yes
C50 . Si2 . C49 . 108.6(3) yes
C51 . Si2 . C49 . 111.2(4) yes
Ti1 . H2 . Ti2 . 109.3 no
Ti2 . H1 . Ti1 . 107.8 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
C13 . H131 . C9 . 134 0.95 2.51 3.238(9) yes
C21 . H213 . C18 . 131 0.95 2.49 3.189(9) yes
C30 . H303 . C34 . 132 0.95 2.50 3.212(9) yes
C38 . H381 . C42 . 134 0.95 2.49 3.223(9) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 


# start Validation reply Form

_vrf_PLAT094_8                   
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.36 Report
RESPONSE: Thie electron density is positioned in the 
centre of the M-H-M unit and likely corresponds
to the hydride electron density.
;
_vrf_PLAT097_8                   
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       3.23 eA-3  
RESPONSE: Thie electron density is positioned in the 
centre of the M-H-M unit and likely corresponds
to the hydride electron density.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 2204758'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_oxford_structure_analysis_title 'T-2\FMC2113_autored.cif_od At 14:41 on 17/10'
_chemical_name_systematic        .
_chemical_melting_point          'not measured'

_cell_length_a                   15.3936(3)
_cell_length_b                   12.7200(3)
_cell_length_c                   15.5084(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.601(2)
_cell_angle_gamma                90
_cell_volume                     3002.50(12)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_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
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'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 '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'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 '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            4

# Given Formula = C28 H44 Cl1 O2 P2 Ti1 
# Dc =      1.23 Fooo =   1188.00 Mu =      5.03 M =    557.96
# Found Formula = C28 H44 Cl1 O2 P2 Ti1 
# Dc =      1.23 FOOO =   1188.00 Mu =      5.03 M =    557.96

_chemical_formula_sum            'C28 H44 Cl O2 P2 Ti'
_chemical_formula_moiety         'C28 H44 Cl O2 P2 Ti'
_chemical_compound_source        .
_chemical_formula_weight         557.96


_cell_measurement_reflns_used    13487
_cell_measurement_theta_min      3
_cell_measurement_theta_max      28
_cell_measurement_temperature    173

_exptl_crystal_description       shard
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.500

_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1188
_exptl_absorpt_coefficient_mu    0.503

# Sheldrick geometric approximatio 0.90 0.98 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_T_max  0.98
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_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       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_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      173
_diffrn_reflns_number            41186
_diffrn_reflns_av_unetI/netI     0.060
_reflns_number_total             6774
_diffrn_reflns_av_R_equivalents  0.050
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6774 
# Theoretical number of reflections is about 15059 


_diffrn_reflns_theta_min         2.579
_diffrn_reflns_theta_max         28.388
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        28.388
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -20
_reflns_limit_h_max              20
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      0.05

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

_refine_diff_density_min         -0.55
_refine_diff_density_max         0.55


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6768
_oxford_refine_ls_R_factor_ref   0.0627
_refine_ls_wR_factor_ref         0.0951
_refine_ls_goodness_of_fit_ref   1.0251
_refine_ls_shift/su_max          0.0007251
_refine_ls_shift/su_mean         0.0000500


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6774
_refine_ls_R_factor_all          0.0636
_refine_ls_wR_factor_all         0.1009

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5162
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_gt          0.0909


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 1.85P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# 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 0.58065(12) 0.17597(15) 0.85717(12) 0.0222 1.0000 Uani . . . . . .
C2 C 0.58203(13) 0.26043(17) 0.91541(13) 0.0279 1.0000 Uani . . . . . .
C3 C 0.64404(14) 0.27481(18) 0.98889(14) 0.0333 1.0000 Uani . . . . . .
C4 C 0.70967(14) 0.20133(18) 1.00758(14) 0.0339 1.0000 Uani . . . . . .
C5 C 0.71276(14) 0.11534(18) 0.95435(14) 0.0328 1.0000 Uani . . . . . .
C6 C 0.64911(13) 0.10496(15) 0.88159(13) 0.0240 1.0000 Uani . . . . . .
C7 C 0.41946(15) 0.45569(17) 0.78087(15) 0.0338 1.0000 Uani . . . . . .
C8 C 0.39393(18) 0.53640(19) 0.84540(17) 0.0446 1.0000 Uani . . . . . .
C9 C 0.35063(19) 0.4529(2) 0.69860(16) 0.0503 1.0000 Uani . . . . . .
C10 C 0.50809(19) 0.4884(2) 0.7547(2) 0.0585 1.0000 Uani . . . . . .
C11 C 0.34564(17) 0.2825(2) 0.88925(17) 0.0448 1.0000 Uani . . . . . .
C12 C 0.3445(3) 0.3492(3) 0.9720(2) 0.0809 1.0000 Uani . . . . . .
C13 C 0.25652(17) 0.2855(3) 0.8322(2) 0.0719 1.0000 Uani . . . . . .
C14 C 0.36609(19) 0.1682(2) 0.91749(18) 0.0511 1.0000 Uani . . . . . .
C15 C 0.65799(16) -0.0293(2) 0.66092(15) 0.0424 1.0000 Uani . . . . . .
C16 C 0.73104(18) 0.0530(3) 0.6753(2) 0.0620 1.0000 Uani . . . . . .
C17 C 0.7003(2) -0.1387(3) 0.6654(2) 0.0681 1.0000 Uani . . . . . .
C18 C 0.6028(2) -0.0129(3) 0.57110(17) 0.0642 1.0000 Uani . . . . . .
C19 C 0.52850(17) -0.12314(19) 0.77449(18) 0.0456 1.0000 Uani . . . . . .
C20 C 0.46973(19) -0.0862(2) 0.8399(2) 0.0593 1.0000 Uani . . . . . .
C21 C 0.47173(19) -0.1683(2) 0.6932(2) 0.0661 1.0000 Uani . . . . . .
C22 C 0.5907(2) -0.2084(2) 0.8193(2) 0.0657 1.0000 Uani . . . . . .
C23 C 0.52667(14) 0.25234(16) 0.63055(13) 0.0271 1.0000 Uani . . . . . .
C24 C 0.47462(16) 0.27895(17) 0.55182(14) 0.0339 1.0000 Uani . . . . . .
C25 C 0.5050(2) 0.3465(2) 0.49220(16) 0.0501 1.0000 Uani . . . . . .
C26 C 0.5888(2) 0.3874(2) 0.50935(19) 0.0580 1.0000 Uani . . . . . .
C27 C 0.64206(19) 0.3622(2) 0.58494(19) 0.0510 1.0000 Uani . . . . . .
C28 C 0.61131(15) 0.29678(19) 0.64440(16) 0.0381 1.0000 Uani . . . . . .
Ti1 Ti 0.48772(2) 0.16649(3) 0.73391(2) 0.0203 1.0000 Uani . . . . . .
Cl1 Cl 0.35312(3) 0.10106(5) 0.66963(4) 0.0384 1.0000 Uani . . . . . .
P2 P 0.58512(3) -0.00270(4) 0.74400(4) 0.0257 1.0000 Uani . . . . . .
O2 O 0.65655(10) 0.01456(11) 0.83247(9) 0.0309 1.0000 Uani . . . . . .
O1 O 0.51702(11) 0.33830(13) 0.90303(10) 0.0440 1.0000 Uani . . . . . .
P1 P 0.43410(3) 0.31948(4) 0.82510(4) 0.0265 1.0000 Uani . . . . . .
H31 H 0.6409 0.3343 1.0251 0.0406 1.0000 Uiso R . . . . .
H41 H 0.7515 0.2100 1.0577 0.0389 1.0000 Uiso R . . . . .
H51 H 0.7575 0.0630 0.9659 0.0387 1.0000 Uiso R . . . . .
H82 H 0.4351 0.5322 0.8987 0.0702 1.0000 Uiso R . . . . .
H81 H 0.3971 0.6035 0.8204 0.0691 1.0000 Uiso R . . . . .
H83 H 0.3336 0.5240 0.8552 0.0696 1.0000 Uiso R . . . . .
H93 H 0.3687 0.4054 0.6559 0.0725 1.0000 Uiso R . . . . .
H91 H 0.3458 0.5228 0.6745 0.0732 1.0000 Uiso R . . . . .
H92 H 0.2918 0.4330 0.7136 0.0735 1.0000 Uiso R . . . . .
H101 H 0.5244 0.4390 0.7136 0.0880 1.0000 Uiso R . . . . .
H102 H 0.5511 0.4916 0.8081 0.0882 1.0000 Uiso R . . . . .
H103 H 0.5001 0.5567 0.7282 0.0879 1.0000 Uiso R . . . . .
H123 H 0.4045 0.3553 1.0022 0.1231 1.0000 Uiso R . . . . .
H121 H 0.3085 0.3140 1.0060 0.1213 1.0000 Uiso R . . . . .
H122 H 0.3187 0.4162 0.9545 0.1220 1.0000 Uiso R . . . . .
H131 H 0.2553 0.2489 0.7762 0.1070 1.0000 Uiso R . . . . .
H132 H 0.2127 0.2541 0.8628 0.1068 1.0000 Uiso R . . . . .
H133 H 0.2393 0.3576 0.8192 0.1067 1.0000 Uiso R . . . . .
H142 H 0.3627 0.1216 0.8679 0.0757 1.0000 Uiso R . . . . .
H143 H 0.4231 0.1619 0.9522 0.0763 1.0000 Uiso R . . . . .
H141 H 0.3240 0.1446 0.9524 0.0755 1.0000 Uiso R . . . . .
H161 H 0.7078 0.1237 0.6722 0.0868 1.0000 Uiso R . . . . .
H162 H 0.7670 0.0427 0.7319 0.0868 1.0000 Uiso R . . . . .
H163 H 0.7671 0.0450 0.6310 0.0868 1.0000 Uiso R . . . . .
H172 H 0.6546 -0.1899 0.6488 0.0972 1.0000 Uiso R . . . . .
H173 H 0.7296 -0.1530 0.7243 0.0968 1.0000 Uiso R . . . . .
H171 H 0.7428 -0.1386 0.6261 0.0968 1.0000 Uiso R . . . . .
H181 H 0.5535 -0.0601 0.5632 0.0981 1.0000 Uiso R . . . . .
H183 H 0.6382 -0.0249 0.5266 0.0973 1.0000 Uiso R . . . . .
H182 H 0.5805 0.0586 0.5657 0.0975 1.0000 Uiso R . . . . .
H202 H 0.5050 -0.0543 0.8905 0.0864 1.0000 Uiso R . . . . .
H201 H 0.4391 -0.1466 0.8587 0.0869 1.0000 Uiso R . . . . .
H203 H 0.4272 -0.0352 0.8125 0.0868 1.0000 Uiso R . . . . .
H211 H 0.5101 -0.1962 0.6554 0.0995 1.0000 Uiso R . . . . .
H213 H 0.4362 -0.2235 0.7110 0.0988 1.0000 Uiso R . . . . .
H212 H 0.4346 -0.1133 0.6644 0.0984 1.0000 Uiso R . . . . .
H222 H 0.6190 -0.2382 0.7744 0.0988 1.0000 Uiso R . . . . .
H221 H 0.6333 -0.1759 0.8654 0.0990 1.0000 Uiso R . . . . .
H223 H 0.5565 -0.2622 0.8419 0.0990 1.0000 Uiso R . . . . .
H241 H 0.4160 0.2493 0.5392 0.0417 1.0000 Uiso R . . . . .
H251 H 0.4676 0.3639 0.4397 0.0574 1.0000 Uiso R . . . . .
H261 H 0.6084 0.4322 0.4706 0.0735 1.0000 Uiso R . . . . .
H271 H 0.7007 0.3908 0.5974 0.0607 1.0000 Uiso R . . . . .
H281 H 0.6502 0.2821 0.6986 0.0457 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.83(5)
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 . 1.402(3) yes
C1 . C6 . 1.397(3) yes
C1 . Ti1 . 2.2129(19) yes
C2 . C3 . 1.385(3) yes
C2 . O1 . 1.401(2) yes
C3 . C4 . 1.375(3) yes
C3 . H31 . 0.948 no
C4 . C5 . 1.375(3) yes
C4 . H41 . 0.939 no
C5 . C6 . 1.386(3) yes
C5 . H51 . 0.955 no
C6 . O2 . 1.394(2) yes
C7 . C8 . 1.526(3) yes
C7 . C9 . 1.532(3) yes
C7 . C10 . 1.538(3) yes
C7 . P1 . 1.865(2) yes
C8 . H82 . 0.965 no
C8 . H81 . 0.942 no
C8 . H83 . 0.975 no
C9 . H93 . 0.968 no
C9 . H91 . 0.963 no
C9 . H92 . 1.000 no
C10 . H101 . 0.955 no
C10 . H102 . 0.981 no
C10 . H103 . 0.961 no
C11 . C12 . 1.542(4) yes
C11 . C13 . 1.518(4) yes
C11 . C14 . 1.537(3) yes
C11 . P1 . 1.863(2) yes
C12 . H123 . 0.973 no
C12 . H121 . 0.936 no
C12 . H122 . 0.962 no
C13 . H131 . 0.983 no
C13 . H132 . 0.967 no
C13 . H133 . 0.968 no
C14 . H142 . 0.965 no
C14 . H143 . 0.961 no
C14 . H141 . 0.952 no
C15 . C16 . 1.528(4) yes
C15 . C17 . 1.534(4) yes
C15 . C18 . 1.533(3) yes
C15 . P2 . 1.862(2) yes
C16 . H161 . 0.967 no
C16 . H162 . 0.973 no
C16 . H163 . 0.952 no
C17 . H172 . 0.965 no
C17 . H173 . 0.973 no
C17 . H171 . 0.959 no
C18 . H181 . 0.962 no
C18 . H183 . 0.953 no
C18 . H182 . 0.971 no
C19 . C20 . 1.530(4) yes
C19 . C21 . 1.534(4) yes
C19 . C22 . 1.542(4) yes
C19 . P2 . 1.858(3) yes
C20 . H202 . 0.974 no
C20 . H201 . 0.969 no
C20 . H203 . 0.972 no
C21 . H211 . 0.961 no
C21 . H213 . 0.955 no
C21 . H212 . 0.969 no
C22 . H222 . 0.954 no
C22 . H221 . 0.986 no
C22 . H223 . 0.962 no
C23 . C24 . 1.398(3) yes
C23 . C28 . 1.407(3) yes
C23 . Ti1 . 2.100(2) yes
C24 . C25 . 1.393(3) yes
C24 . H241 . 0.970 no
C25 . C26 . 1.380(4) yes
C25 . H251 . 0.950 no
C26 . C27 . 1.364(4) yes
C26 . H261 . 0.913 no
C27 . C28 . 1.377(3) yes
C27 . H271 . 0.966 no
C28 . H281 . 0.974 no
Ti1 . Cl1 . 2.3156(6) yes
Ti1 . P2 . 2.6141(6) yes
Ti1 . P1 . 2.6109(6) yes
P2 . O2 . 1.6396(14) yes
O1 . P1 . 1.6388(16) 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 . C6 . 112.51(17) yes
C2 . C1 . Ti1 . 122.95(14) yes
C6 . C1 . Ti1 . 124.27(14) yes
C1 . C2 . C3 . 125.00(19) yes
C1 . C2 . O1 . 120.80(18) yes
C3 . C2 . O1 . 114.19(18) yes
C2 . C3 . C4 . 118.6(2) yes
C2 . C3 . H31 . 120.2 no
C4 . C3 . H31 . 121.2 no
C3 . C4 . C5 . 120.28(19) yes
C3 . C4 . H41 . 119.1 no
C5 . C4 . H41 . 120.6 no
C4 . C5 . C6 . 118.74(19) yes
C4 . C5 . H51 . 122.0 no
C6 . C5 . H51 . 119.3 no
C1 . C6 . C5 . 124.91(18) yes
C1 . C6 . O2 . 120.38(17) yes
C5 . C6 . O2 . 114.70(17) yes
C8 . C7 . C9 . 110.4(2) yes
C8 . C7 . C10 . 108.5(2) yes
C9 . C7 . C10 . 108.5(2) yes
C8 . C7 . P1 . 114.38(17) yes
C9 . C7 . P1 . 108.36(16) yes
C10 . C7 . P1 . 106.58(16) yes
C7 . C8 . H82 . 109.0 no
C7 . C8 . H81 . 107.8 no
H82 . C8 . H81 . 109.6 no
C7 . C8 . H83 . 109.7 no
H82 . C8 . H83 . 112.1 no
H81 . C8 . H83 . 108.6 no
C7 . C9 . H93 . 110.5 no
C7 . C9 . H91 . 107.7 no
H93 . C9 . H91 . 108.9 no
C7 . C9 . H92 . 110.5 no
H93 . C9 . H92 . 111.4 no
H91 . C9 . H92 . 107.7 no
C7 . C10 . H101 . 109.3 no
C7 . C10 . H102 . 107.5 no
H101 . C10 . H102 . 112.3 no
C7 . C10 . H103 . 107.2 no
H101 . C10 . H103 . 109.7 no
H102 . C10 . H103 . 110.5 no
C12 . C11 . C13 . 110.5(2) yes
C12 . C11 . C14 . 108.1(2) yes
C13 . C11 . C14 . 108.6(2) yes
C12 . C11 . P1 . 113.9(2) yes
C13 . C11 . P1 . 110.58(18) yes
C14 . C11 . P1 . 104.85(16) yes
C11 . C12 . H123 . 108.4 no
C11 . C12 . H121 . 106.6 no
H123 . C12 . H121 . 111.5 no
C11 . C12 . H122 . 107.9 no
H123 . C12 . H122 . 112.9 no
H121 . C12 . H122 . 109.2 no
C11 . C13 . H131 . 113.5 no
C11 . C13 . H132 . 109.8 no
H131 . C13 . H132 . 108.4 no
C11 . C13 . H133 . 110.0 no
H131 . C13 . H133 . 107.2 no
H132 . C13 . H133 . 107.7 no
C11 . C14 . H142 . 111.6 no
C11 . C14 . H143 . 111.6 no
H142 . C14 . H143 . 109.4 no
C11 . C14 . H141 . 109.4 no
H142 . C14 . H141 . 107.5 no
H143 . C14 . H141 . 107.2 no
C16 . C15 . C17 . 108.5(2) yes
C16 . C15 . C18 . 109.6(3) yes
C17 . C15 . C18 . 109.8(2) yes
C16 . C15 . P2 . 106.31(17) yes
C17 . C15 . P2 . 115.4(2) yes
C18 . C15 . P2 . 107.15(17) yes
C15 . C16 . H161 . 111.8 no
C15 . C16 . H162 . 110.3 no
H161 . C16 . H162 . 109.1 no
C15 . C16 . H163 . 108.5 no
H161 . C16 . H163 . 108.3 no
H162 . C16 . H163 . 108.7 no
C15 . C17 . H172 . 108.2 no
C15 . C17 . H173 . 110.3 no
H172 . C17 . H173 . 110.0 no
C15 . C17 . H171 . 107.1 no
H172 . C17 . H171 . 111.7 no
H173 . C17 . H171 . 109.5 no
C15 . C18 . H181 . 110.5 no
C15 . C18 . H183 . 109.7 no
H181 . C18 . H183 . 109.5 no
C15 . C18 . H182 . 110.3 no
H181 . C18 . H182 . 108.1 no
H183 . C18 . H182 . 108.7 no
C20 . C19 . C21 . 109.8(2) yes
C20 . C19 . C22 . 107.9(2) yes
C21 . C19 . C22 . 110.2(2) yes
C20 . C19 . P2 . 105.15(17) yes
C21 . C19 . P2 . 109.3(2) yes
C22 . C19 . P2 . 114.27(19) yes
C19 . C20 . H202 . 110.4 no
C19 . C20 . H201 . 108.5 no
H202 . C20 . H201 . 108.9 no
C19 . C20 . H203 . 110.0 no
H202 . C20 . H203 . 109.4 no
H201 . C20 . H203 . 109.5 no
C19 . C21 . H211 . 108.3 no
C19 . C21 . H213 . 108.6 no
H211 . C21 . H213 . 109.7 no
C19 . C21 . H212 . 109.4 no
H211 . C21 . H212 . 111.0 no
H213 . C21 . H212 . 109.9 no
C19 . C22 . H222 . 105.7 no
C19 . C22 . H221 . 109.5 no
H222 . C22 . H221 . 111.7 no
C19 . C22 . H223 . 109.1 no
H222 . C22 . H223 . 108.6 no
H221 . C22 . H223 . 112.0 no
C24 . C23 . C28 . 115.6(2) yes
C24 . C23 . Ti1 . 126.93(16) yes
C28 . C23 . Ti1 . 117.13(16) yes
C23 . C24 . C25 . 121.6(2) yes
C23 . C24 . H241 . 118.5 no
C25 . C24 . H241 . 120.0 no
C24 . C25 . C26 . 120.1(2) yes
C24 . C25 . H251 . 119.5 no
C26 . C25 . H251 . 120.4 no
C25 . C26 . C27 . 120.1(2) yes
C25 . C26 . H261 . 120.1 no
C27 . C26 . H261 . 119.8 no
C26 . C27 . C28 . 119.6(2) yes
C26 . C27 . H271 . 120.5 no
C28 . C27 . H271 . 119.8 no
C23 . C28 . C27 . 122.9(2) yes
C23 . C28 . H281 . 119.3 no
C27 . C28 . H281 . 117.7 no
C1 . Ti1 . C23 . 114.18(8) yes
C1 . Ti1 . Cl1 . 144.36(5) yes
C23 . Ti1 . Cl1 . 101.39(6) yes
C1 . Ti1 . P2 . 72.68(5) yes
C23 . Ti1 . P2 . 104.31(6) yes
Cl1 . Ti1 . P2 . 101.43(2) yes
C1 . Ti1 . P1 . 72.99(5) yes
C23 . Ti1 . P1 . 100.10(6) yes
Cl1 . Ti1 . P1 . 99.56(2) yes
P2 . Ti1 . P1 . 143.72(2) yes
C15 . P2 . C19 . 112.36(12) yes
C15 . P2 . Ti1 . 120.51(8) yes
C19 . P2 . Ti1 . 114.04(8) yes
C15 . P2 . O2 . 101.85(9) yes
C19 . P2 . O2 . 100.30(10) yes
Ti1 . P2 . O2 . 104.28(5) yes
C6 . O2 . P2 . 117.92(12) yes
C2 . O1 . P1 . 117.35(13) yes
C7 . P1 . C11 . 111.93(11) yes
C7 . P1 . Ti1 . 121.60(7) yes
C11 . P1 . Ti1 . 114.61(8) yes
C7 . P1 . O1 . 99.99(10) yes
C11 . P1 . O1 . 101.18(11) yes
Ti1 . P1 . O1 . 103.53(6) 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
C10 . H101 . C28 . 161 0.96 2.58 3.494(4) yes
C22 . H222 . C17 . 127 0.95 2.58 3.245(4) yes



# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 1 1 x .
0 0 2 x .
2 0 0 x .
-1 1 2 x .
2 1 1 x .
11 10 9 x .
# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# start Validation Reply Form
_vrf_PLAT922_6                   
;
PROBLEM: wR2 in the CIF and FCF Differ by ...............     0.0053 Check 
RESPONSE: CIF and FCF were created off the same model.
This discrepancy arises from the weighting scheme.
;
# end Validation Reply Form

####################################################################### 
# 
# 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 2204755'
loop_
_audit_author_name
_audit_author_address
'F. Mark Chadwick'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;


_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;

_cell_length_a                   19.8638(10)
_cell_length_b                   29.354(2)
_cell_length_c                   19.5939(11)
_cell_angle_alpha                90
_cell_angle_beta                 96.659(5)
_cell_angle_gamma                90
_cell_volume                     11347.8(12)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,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 0.2191 1.8069 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'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 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'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0181 0.0091 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            12

# Given Formula = C44 H78 Cl2 O4 P4 Ti1 
# Dc =      1.60 Fooo =   5880.00 Mu =     51.95 M =    913.80
# Found Formula = C29.33 H52 Cl1.33 O2.67 P2.67 Ti0.67 
# Dc =      1.07 FOOO =   3920.00 Mu =     34.63 M =    609.20

_chemical_formula_sum            'C29.33 H52 Cl1.33 O2.67 P2.67 Ti0.67'
_chemical_formula_moiety         'C29.33 H52 Cl1.33 O2.67 P2.67 Ti0.67'
_chemical_compound_source        .
_chemical_formula_weight         609.20


_cell_measurement_reflns_used    1638
_cell_measurement_theta_min      4
_cell_measurement_theta_max      64
_cell_measurement_temperature    173

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_max          0.100

_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3920
_exptl_absorpt_coefficient_mu    3.463

# Sheldrick geometric approximatio 0.84 0.84 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.84
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_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      173
_diffrn_reflns_number            37934
_diffrn_reflns_av_unetI/netI     0.357
_reflns_number_total             21794
_diffrn_reflns_av_R_equivalents  0.172
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 21794 
# Theoretical number of reflections is about 45949 


_diffrn_reflns_theta_min         3.356
_diffrn_reflns_theta_max         73.818
_diffrn_measured_fraction_theta_max 0.949

_diffrn_reflns_theta_full        33.957
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -24
_reflns_limit_h_max              24
_reflns_limit_k_min              0
_reflns_limit_k_max              35
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   2.82
_oxford_diffrn_Wilson_scale      6.14

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

_refine_diff_density_min         -2.53
_refine_diff_density_max         2.16


# 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_refine_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     991
_refine_ls_number_reflns         21794
_oxford_refine_ls_R_factor_ref   0.2724
_refine_ls_wR_factor_ref         0.4597
_refine_ls_goodness_of_fit_ref   1.4506
_refine_ls_shift/su_max          0.0006391
_refine_ls_shift/su_mean         0.0000573


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        21794
_refine_ls_R_factor_all          0.2724
_refine_ls_wR_factor_all         0.4597

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5778
_refine_ls_R_factor_gt           0.1184
_refine_ls_wR_factor_gt          0.2662


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #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: 
 934. 0.140E+04 731. 212. 24.6 
;

# 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 0.35646(17) 0.88653(13) 0.77721(17) 0.0585 1.0000 Uani . . . . . .
Ti2 Ti 0.85939(16) 0.63110(12) 0.77671(15) 0.0514 1.0000 Uani . . . . . .
Cl1 Cl 0.4364(2) 0.9380(2) 0.8245(2) 0.0749 1.0000 Uani . . . . . .
Cl2 Cl 0.2790(2) 0.94114(19) 0.7336(2) 0.0657 1.0000 Uani . . . . . .
Cl3 Cl 0.7917(2) 0.68142(18) 0.8304(2) 0.0617 1.0000 Uani . . . . . .
Cl4 Cl 0.9270(2) 0.68199(18) 0.7255(2) 0.0599 1.0000 Uani . . . . . .
O1 O 0.2911(7) 0.8429(5) 0.7757(6) 0.0697 1.0000 Uani . . . . . .
O2 O 0.1781(6) 0.8425(5) 0.9826(5) 0.0558 1.0000 Uani . . . . . .
O3 O 0.4202(6) 0.8419(5) 0.7728(7) 0.0706 1.0000 Uani . . . . . .
O4 O 0.5404(5) 0.8499(4) 0.5738(5) 0.0528 1.0000 Uani . . . . . .
O5 O 0.8747(5) 0.5863(4) 0.7128(5) 0.0520 1.0000 Uani . . . . . .
O6 O 0.7459(5) 0.6163(4) 0.4945(5) 0.0483 1.0000 Uani . . . . . .
O7 O 0.8441(6) 0.5849(4) 0.8359(6) 0.0558 1.0000 Uani . . . . . .
O8 O 0.9703(5) 0.6116(4) 1.0589(5) 0.0425 1.0000 Uani . . . . . .
P1 P 0.3097(2) 0.88395(19) 0.9036(2) 0.0535 1.0000 Uani . . . . . .
P2 P 0.1132(2) 0.82216(19) 1.0226(2) 0.0556 1.0000 Uani . . . . . .
P3 P 0.4070(2) 0.88962(18) 0.6522(2) 0.0526 1.0000 Uani . . . . . .
P4 P 0.6050(2) 0.83049(19) 0.5307(2) 0.0572 1.0000 Uani . . . . . .
P5 P 0.7655(2) 0.63994(17) 0.6636(2) 0.0466 1.0000 Uani . . . . . .
P6 P 0.7363(2) 0.60669(19) 0.4063(2) 0.0532 1.0000 Uani . . . . . .
P7 P 0.9522(2) 0.63771(17) 0.8902(2) 0.0478 1.0000 Uani . . . . . .
P8 P 0.9790(2) 0.60147(19) 1.1468(2) 0.0567 1.0000 Uani . . . . . .
C1 C 0.2407(8) 0.8420(6) 0.8807(8) 0.0483 1.0000 Uani . . . . . .
C2 C 0.1874(8) 0.8261(6) 0.9160(8) 0.0493 1.0000 Uani . . . . . .
C3 C 0.1435(9) 0.7924(7) 0.8842(10) 0.0652 1.0000 Uani . . . . . .
C4 C 0.1491(9) 0.7762(8) 0.8180(9) 0.0674 1.0000 Uani . . . . . .
C5 C 0.1994(9) 0.7945(7) 0.7820(8) 0.0629 1.0000 Uani . . . . . .
C6 C 0.2439(9) 0.8271(6) 0.8133(9) 0.0523 1.0000 Uani . . . . . .
C7 C 0.3717(10) 0.8515(9) 0.9658(9) 0.0781 1.0000 Uani . . . . . .
C8 C 0.4038(11) 0.8160(8) 0.9314(11) 0.0867 1.0000 Uani . . . . . .
C9 C 0.4266(9) 0.8893(8) 0.9988(10) 0.0776 1.0000 Uani . . . . . .
C10 C 0.3398(9) 0.8313(10) 1.0280(9) 0.0915 1.0000 Uani . . . . . .
C11 C 0.2749(9) 0.9368(7) 0.9381(8) 0.0573 1.0000 Uani . . . . . .
C12 C 0.2066(9) 0.9459(7) 0.8947(10) 0.0698 1.0000 Uani . . . . . .
C13 C 0.2619(9) 0.9356(8) 1.0161(8) 0.0725 1.0000 Uani . . . . . .
C14 C 0.3214(10) 0.9766(7) 0.9251(11) 0.0738 1.0000 Uani . . . . . .
C15 C 0.0530(9) 0.8693(7) 1.0153(9) 0.0548 1.0000 Uani . . . . . .
C16 C 0.0338(10) 0.8773(9) 0.9349(10) 0.0802 1.0000 Uani . . . . . .
C17 C 0.0713(10) 0.9159(7) 1.0435(11) 0.0740 1.0000 Uani . . . . . .
C18 C -0.0134(9) 0.8537(7) 1.0415(9) 0.0636 1.0000 Uani . . . . . .
C19 C 0.1571(11) 0.8180(8) 1.1121(10) 0.0718 1.0000 Uani . . . . . .
C20 C 0.2010(12) 0.7754(9) 1.1127(11) 0.0922 1.0000 Uani . . . . . .
C21 C 0.2004(10) 0.8601(7) 1.1393(8) 0.0642 1.0000 Uani . . . . . .
C22 C 0.1019(12) 0.8072(10) 1.1585(11) 0.1031 1.0000 Uani . . . . . .
C23 C 0.4756(9) 0.8465(6) 0.6699(8) 0.0511 1.0000 Uani . . . . . .
C24 C 0.4711(8) 0.8276(7) 0.7363(8) 0.0511 1.0000 Uani . . . . . .
C25 C 0.5137(11) 0.7931(7) 0.7633(10) 0.0715 1.0000 Uani . . . . . .
C26 C 0.5631(9) 0.7784(7) 0.7281(10) 0.0611 1.0000 Uani . . . . . .
C27 C 0.5712(9) 0.7953(6) 0.6637(8) 0.0559 1.0000 Uani . . . . . .
C28 C 0.5301(9) 0.8313(6) 0.6378(8) 0.0514 1.0000 Uani . . . . . .
C29 C 0.3448(8) 0.8623(8) 0.5820(8) 0.0624 1.0000 Uani . . . . . .
C30 C 0.3141(11) 0.8217(10) 0.6175(11) 0.0969 1.0000 Uani . . . . . .
C31 C 0.2893(10) 0.8990(11) 0.5592(11) 0.1157 1.0000 Uani . . . . . .
C32 C 0.3772(10) 0.8449(10) 0.5203(11) 0.0987 1.0000 Uani . . . . . .
C33 C 0.4424(8) 0.9445(8) 0.6224(10) 0.0662 1.0000 Uani . . . . . .
C34 C 0.3997(9) 0.9836(8) 0.6395(9) 0.0685 1.0000 Uani . . . . . .
C35 C 0.4525(10) 0.9457(8) 0.5469(9) 0.0751 1.0000 Uani . . . . . .
C36 C 0.5125(9) 0.9520(8) 0.6643(10) 0.0698 1.0000 Uani . . . . . .
C37 C 0.5625(8) 0.8271(8) 0.4407(8) 0.0607 1.0000 Uani . . . . . .
C38 C 0.5153(11) 0.7844(10) 0.4435(11) 0.1003 1.0000 Uani . . . . . .
C39 C 0.5200(10) 0.8687(9) 0.4148(11) 0.0887 1.0000 Uani . . . . . .
C40 C 0.6134(10) 0.8138(10) 0.3945(9) 0.0900 1.0000 Uani . . . . . .
C41 C 0.6655(8) 0.8802(7) 0.5404(9) 0.0548 1.0000 Uani . . . . . .
C42 C 0.6413(10) 0.9262(8) 0.5113(11) 0.0793 1.0000 Uani . . . . . .
C43 C 0.7280(9) 0.8640(9) 0.5096(10) 0.0769 1.0000 Uani . . . . . .
C44 C 0.6850(9) 0.8859(8) 0.6186(9) 0.0706 1.0000 Uani . . . . . .
C45 C 0.8076(8) 0.6026(6) 0.6080(9) 0.0499 1.0000 Uani . . . . . .
C46 C 0.8632(9) 0.5799(6) 0.6439(8) 0.0514 1.0000 Uani . . . . . .
C47 C 0.9018(9) 0.5462(7) 0.6157(8) 0.0581 1.0000 Uani . . . . . .
C48 C 0.8901(8) 0.5381(7) 0.5464(9) 0.0574 1.0000 Uani . . . . . .
C49 C 0.8370(8) 0.5611(6) 0.5054(7) 0.0479 1.0000 Uani . . . . . .
C50 C 0.7974(7) 0.5922(6) 0.5355(8) 0.0482 1.0000 Uani . . . . . .
C51 C 0.6867(8) 0.6091(7) 0.6793(8) 0.0519 1.0000 Uani . . . . . .
C52 C 0.6407(9) 0.5933(8) 0.6113(8) 0.0715 1.0000 Uani . . . . . .
C53 C 0.7094(10) 0.5641(7) 0.7182(9) 0.0643 1.0000 Uani . . . . . .
C54 C 0.6448(9) 0.6367(8) 0.7268(10) 0.0699 1.0000 Uani . . . . . .
C55 C 0.7483(8) 0.6977(6) 0.6234(8) 0.0517 1.0000 Uani . . . . . .
C56 C 0.8059(9) 0.7093(6) 0.5814(8) 0.0549 1.0000 Uani . . . . . .
C57 C 0.7466(9) 0.7332(6) 0.6813(10) 0.0593 1.0000 Uani . . . . . .
C58 C 0.6804(9) 0.7003(8) 0.576(1) 0.0665 1.0000 Uani . . . . . .
C59 C 0.6414(8) 0.5997(8) 0.3922(8) 0.0657 1.0000 Uani . . . . . .
C60 C 0.6288(10) 0.5532(8) 0.4208(9) 0.0848 1.0000 Uani . . . . . .
C61 C 0.5978(9) 0.6352(9) 0.4212(10) 0.0809 1.0000 Uani . . . . . .
C62 C 0.6228(8) 0.5987(10) 0.3106(8) 0.0990 1.0000 Uani . . . . . .
C63 C 0.7618(10) 0.6599(8) 0.3751(8) 0.0621 1.0000 Uani . . . . . .
C64 C 0.7286(11) 0.7050(9) 0.3934(10) 0.0823 1.0000 Uani . . . . . .
C65 C 0.7601(10) 0.6600(9) 0.2954(10) 0.0820 1.0000 Uani . . . . . .
C66 C 0.8402(9) 0.6656(8) 0.4009(8) 0.0654 1.0000 Uani . . . . . .
C67 C 0.9101(7) 0.6001(6) 0.9456(8) 0.0417 1.0000 Uani . . . . . .
C68 C 0.8570(7) 0.5750(6) 0.9050(8) 0.0444 1.0000 Uani . . . . . .
C69 C 0.8214(8) 0.5414(6) 0.9303(8) 0.0519 1.0000 Uani . . . . . .
C70 C 0.8362(8) 0.5285(7) 1.0004(9) 0.0573 1.0000 Uani . . . . . .
C71 C 0.8857(9) 0.5524(7) 1.0419(9) 0.0575 1.0000 Uani . . . . . .
C72 C 0.9222(8) 0.5867(6) 1.0167(7) 0.0435 1.0000 Uani . . . . . .
C73 C 0.9700(9) 0.6945(6) 0.9333(8) 0.0492 1.0000 Uani . . . . . .
C74 C 0.9715(9) 0.7313(6) 0.8786(8) 0.0535 1.0000 Uani . . . . . .
C75 C 1.0368(9) 0.6969(7) 0.9832(9) 0.0627 1.0000 Uani . . . . . .
C76 C 0.9107(8) 0.7072(7) 0.9736(8) 0.0552 1.0000 Uani . . . . . .
C77 C 1.0325(9) 0.6073(8) 0.8736(10) 0.0656 1.0000 Uani . . . . . .
C78 C 1.0101(11) 0.5638(8) 0.8319(12) 0.0832 1.0000 Uani . . . . . .
C79 C 1.0734(10) 0.5894(8) 0.9383(9) 0.0696 1.0000 Uani . . . . . .
C80 C 1.0753(8) 0.6378(7) 0.8353(8) 0.0632 1.0000 Uani . . . . . .
C81 C 1.0738(10) 0.5949(8) 1.1614(10) 0.0693 1.0000 Uani . . . . . .
C82 C 1.0867(12) 0.5501(8) 1.1302(14) 0.0970 1.0000 Uani . . . . . .
C83 C 1.0887(13) 0.5914(12) 1.2420(12) 0.1272 1.0000 Uani . . . . . .
C84 C 1.1176(8) 0.6317(7) 1.1372(11) 0.0702 1.0000 Uani . . . . . .
C85 C 0.9512(8) 0.6557(8) 1.1806(9) 0.0637 1.0000 Uani . . . . . .
C86 C 0.9539(11) 0.6520(10) 1.2571(9) 0.1011 1.0000 Uani . . . . . .
C87 C 0.8762(9) 0.6587(9) 1.1516(10) 0.0777 1.0000 Uani . . . . . .
C88 C 0.9844(10) 0.6992(7) 1.1592(9) 0.0686 1.0000 Uani . . . . . .
H31 H 0.1102 0.7805 0.9088 0.0781 1.0000 Uiso R . . . . .
H41 H 0.1195 0.7538 0.7981 0.0831 1.0000 Uiso R . . . . .
H51 H 0.2036 0.7851 0.7372 0.0820 1.0000 Uiso R . . . . .
H81 H 0.4358 0.7996 0.9630 0.1311 1.0000 Uiso R . . . . .
H82 H 0.4268 0.8295 0.8958 0.1310 1.0000 Uiso R . . . . .
H83 H 0.3701 0.7949 0.9114 0.1311 1.0000 Uiso R . . . . .
H93 H 0.4592 0.8743 1.0312 0.1261 1.0000 Uiso R . . . . .
H92 H 0.4030 0.9123 1.0220 0.1260 1.0000 Uiso R . . . . .
H91 H 0.4487 0.9031 0.9629 0.1260 1.0000 Uiso R . . . . .
H101 H 0.3749 0.8157 1.0578 0.1440 1.0000 Uiso R . . . . .
H102 H 0.3207 0.8564 1.0524 0.1437 1.0000 Uiso R . . . . .
H103 H 0.3045 0.8098 1.0109 0.1440 1.0000 Uiso R . . . . .
H121 H 0.1882 0.9744 0.9086 0.1090 1.0000 Uiso R . . . . .
H122 H 0.2133 0.9474 0.8467 0.1090 1.0000 Uiso R . . . . .
H123 H 0.1762 0.9213 0.9021 0.1090 1.0000 Uiso R . . . . .
H133 H 0.2474 0.9650 1.0301 0.1181 1.0000 Uiso R . . . . .
H132 H 0.3028 0.9271 1.0439 0.1180 1.0000 Uiso R . . . . .
H131 H 0.2271 0.9132 1.0215 0.1180 1.0000 Uiso R . . . . .
H141 H 0.3023 1.0046 0.9399 0.1191 1.0000 Uiso R . . . . .
H142 H 0.3655 0.9721 0.9501 0.1191 1.0000 Uiso R . . . . .
H143 H 0.3256 0.9783 0.8766 0.1190 1.0000 Uiso R . . . . .
H163 H -0.0017 0.8998 0.9276 0.1230 1.0000 Uiso R . . . . .
H162 H 0.0726 0.8880 0.9145 0.1229 1.0000 Uiso R . . . . .
H161 H 0.0182 0.8490 0.9138 0.1230 1.0000 Uiso R . . . . .
H171 H 0.0365 0.9377 1.0273 0.1181 1.0000 Uiso R . . . . .
H172 H 0.0755 0.9141 1.0933 0.1180 1.0000 Uiso R . . . . .
H173 H 0.1141 0.9251 1.0284 0.1180 1.0000 Uiso R . . . . .
H181 H -0.0488 0.8752 1.0280 0.1040 1.0000 Uiso R . . . . .
H182 H -0.0060 0.8523 1.0909 0.1042 1.0000 Uiso R . . . . .
H183 H -0.0260 0.8240 1.0231 0.1041 1.0000 Uiso R . . . . .
H203 H 0.2261 0.7713 1.1572 0.1370 1.0000 Uiso R . . . . .
H202 H 0.2318 0.7782 1.0785 0.1370 1.0000 Uiso R . . . . .
H201 H 0.1721 0.7492 1.1022 0.1370 1.0000 Uiso R . . . . .
H211 H 0.2160 0.8555 1.1870 0.1001 1.0000 Uiso R . . . . .
H212 H 0.1736 0.8874 1.1341 0.1001 1.0000 Uiso R . . . . .
H213 H 0.2386 0.8630 1.1135 0.1000 1.0000 Uiso R . . . . .
H221 H 0.1221 0.7964 1.2025 0.1460 1.0000 Uiso R . . . . .
H222 H 0.0763 0.8344 1.1646 0.1460 1.0000 Uiso R . . . . .
H223 H 0.0721 0.7840 1.1374 0.1459 1.0000 Uiso R . . . . .
H251 H 0.5076 0.7800 0.8054 0.0820 1.0000 Uiso R . . . . .
H261 H 0.5927 0.7558 0.7469 0.0800 1.0000 Uiso R . . . . .
H271 H 0.6041 0.7831 0.6388 0.0701 1.0000 Uiso R . . . . .
H301 H 0.2759 0.8101 0.5880 0.1461 1.0000 Uiso R . . . . .
H302 H 0.2993 0.8319 0.6602 0.1460 1.0000 Uiso R . . . . .
H303 H 0.3470 0.7977 0.6268 0.1460 1.0000 Uiso R . . . . .
H313 H 0.2587 0.8860 0.5226 0.1619 1.0000 Uiso R . . . . .
H312 H 0.3105 0.9257 0.5428 0.1620 1.0000 Uiso R . . . . .
H311 H 0.2652 0.9067 0.5974 0.1620 1.0000 Uiso R . . . . .
H321 H 0.3439 0.8293 0.4896 0.1500 1.0000 Uiso R . . . . .
H322 H 0.3946 0.8705 0.4974 0.1500 1.0000 Uiso R . . . . .
H323 H 0.4134 0.8241 0.5354 0.1499 1.0000 Uiso R . . . . .
H341 H 0.4220 1.0116 0.6294 0.1040 1.0000 Uiso R . . . . .
H342 H 0.3929 0.9827 0.6871 0.1040 1.0000 Uiso R . . . . .
H343 H 0.3568 0.9813 0.6117 0.1040 1.0000 Uiso R . . . . .
H353 H 0.4663 0.9761 0.5358 0.1160 1.0000 Uiso R . . . . .
H352 H 0.4110 0.9381 0.5191 0.1161 1.0000 Uiso R . . . . .
H351 H 0.4871 0.9240 0.5383 0.1161 1.0000 Uiso R . . . . .
H361 H 0.5296 0.9809 0.6511 0.1140 1.0000 Uiso R . . . . .
H362 H 0.5076 0.9524 0.7127 0.1140 1.0000 Uiso R . . . . .
H363 H 0.5428 0.9280 0.6543 0.1140 1.0000 Uiso R . . . . .
H383 H 0.4954 0.7767 0.3980 0.1400 1.0000 Uiso R . . . . .
H382 H 0.4802 0.7912 0.4717 0.1400 1.0000 Uiso R . . . . .
H381 H 0.5418 0.7591 0.4628 0.1400 1.0000 Uiso R . . . . .
H391 H 0.4900 0.8609 0.3749 0.1261 1.0000 Uiso R . . . . .
H392 H 0.5499 0.8924 0.4036 0.1260 1.0000 Uiso R . . . . .
H393 H 0.4941 0.8792 0.4504 0.1259 1.0000 Uiso R . . . . .
H401 H 0.5906 0.8065 0.3502 0.1339 1.0000 Uiso R . . . . .
H402 H 0.6431 0.8391 0.3909 0.1340 1.0000 Uiso R . . . . .
H403 H 0.6389 0.7878 0.4122 0.1341 1.0000 Uiso R . . . . .
H423 H 0.6744 0.9487 0.5262 0.1230 1.0000 Uiso R . . . . .
H422 H 0.5994 0.9338 0.5284 0.1230 1.0000 Uiso R . . . . .
H421 H 0.6346 0.9256 0.4622 0.1230 1.0000 Uiso R . . . . .
H431 H 0.7647 0.8842 0.5236 0.1180 1.0000 Uiso R . . . . .
H432 H 0.7389 0.8336 0.5255 0.1180 1.0000 Uiso R . . . . .
H433 H 0.7191 0.8641 0.4605 0.1181 1.0000 Uiso R . . . . .
H441 H 0.7217 0.9071 0.6269 0.1121 1.0000 Uiso R . . . . .
H442 H 0.6467 0.8976 0.6387 0.1118 1.0000 Uiso R . . . . .
H443 H 0.6983 0.8569 0.6389 0.1120 1.0000 Uiso R . . . . .
H471 H 0.9350 0.5303 0.6437 0.0692 1.0000 Uiso R . . . . .
H481 H 0.9166 0.5169 0.5262 0.0661 1.0000 Uiso R . . . . .
H491 H 0.8293 0.5560 0.4581 0.0641 1.0000 Uiso R . . . . .
H521 H 0.6052 0.5741 0.6249 0.1010 1.0000 Uiso R . . . . .
H522 H 0.6217 0.6199 0.5875 0.1011 1.0000 Uiso R . . . . .
H523 H 0.6682 0.5763 0.5827 0.1010 1.0000 Uiso R . . . . .
H533 H 0.6712 0.5438 0.7178 0.0960 1.0000 Uiso R . . . . .
H532 H 0.7267 0.5711 0.7648 0.0961 1.0000 Uiso R . . . . .
H531 H 0.7444 0.5497 0.6953 0.0960 1.0000 Uiso R . . . . .
H541 H 0.6095 0.6178 0.7406 0.1069 1.0000 Uiso R . . . . .
H542 H 0.6732 0.6469 0.7665 0.1070 1.0000 Uiso R . . . . .
H543 H 0.6257 0.6626 0.7016 0.1070 1.0000 Uiso R . . . . .
H561 H 0.7999 0.7405 0.5664 0.0930 1.0000 Uiso R . . . . .
H562 H 0.8484 0.7060 0.6095 0.0931 1.0000 Uiso R . . . . .
H563 H 0.8049 0.6894 0.5420 0.0930 1.0000 Uiso R . . . . .
H573 H 0.7387 0.7630 0.6611 0.0950 1.0000 Uiso R . . . . .
H572 H 0.7891 0.7334 0.7099 0.0951 1.0000 Uiso R . . . . .
H571 H 0.7107 0.7261 0.7086 0.0951 1.0000 Uiso R . . . . .
H581 H 0.6732 0.7310 0.5596 0.1030 1.0000 Uiso R . . . . .
H582 H 0.6433 0.6912 0.6002 0.1029 1.0000 Uiso R . . . . .
H583 H 0.6829 0.6805 0.5370 0.1030 1.0000 Uiso R . . . . .
H603 H 0.5832 0.5439 0.4070 0.1260 1.0000 Uiso R . . . . .
H602 H 0.6366 0.5543 0.4701 0.1260 1.0000 Uiso R . . . . .
H601 H 0.6592 0.5316 0.4040 0.1260 1.0000 Uiso R . . . . .
H611 H 0.5510 0.6290 0.4074 0.1180 1.0000 Uiso R . . . . .
H612 H 0.6096 0.6642 0.4030 0.1180 1.0000 Uiso R . . . . .
H613 H 0.6057 0.6361 0.4704 0.1180 1.0000 Uiso R . . . . .
H621 H 0.5760 0.5911 0.2996 0.1520 1.0000 Uiso R . . . . .
H622 H 0.6313 0.6285 0.2930 0.1520 1.0000 Uiso R . . . . .
H623 H 0.6505 0.5764 0.2912 0.1520 1.0000 Uiso R . . . . .
H643 H 0.7546 0.7306 0.3805 0.1159 1.0000 Uiso R . . . . .
H642 H 0.7258 0.7058 0.4422 0.1160 1.0000 Uiso R . . . . .
H641 H 0.6837 0.7063 0.3698 0.1160 1.0000 Uiso R . . . . .
H651 H 0.7896 0.6835 0.2821 0.1260 1.0000 Uiso R . . . . .
H652 H 0.7754 0.6309 0.2803 0.1260 1.0000 Uiso R . . . . .
H653 H 0.7150 0.6659 0.2747 0.1260 1.0000 Uiso R . . . . .
H661 H 0.8572 0.6927 0.3808 0.1070 1.0000 Uiso R . . . . .
H662 H 0.8456 0.6683 0.4503 0.1071 1.0000 Uiso R . . . . .
H663 H 0.8643 0.6392 0.3876 0.1070 1.0000 Uiso R . . . . .
H691 H 0.7884 0.5259 0.9015 0.0691 1.0000 Uiso R . . . . .
H701 H 0.8132 0.5045 1.0186 0.0771 1.0000 Uiso R . . . . .
H711 H 0.8932 0.5455 1.0888 0.0701 1.0000 Uiso R . . . . .
H741 H 0.9814 0.7604 0.9005 0.0890 1.0000 Uiso R . . . . .
H742 H 1.0058 0.7243 0.8493 0.0891 1.0000 Uiso R . . . . .
H743 H 0.9280 0.7326 0.8521 0.0890 1.0000 Uiso R . . . . .
H753 H 1.0401 0.7266 1.0049 0.0971 1.0000 Uiso R . . . . .
H752 H 1.0743 0.6924 0.9570 0.0969 1.0000 Uiso R . . . . .
H751 H 1.0372 0.6735 1.0178 0.0970 1.0000 Uiso R . . . . .
H761 H 0.9216 0.7353 0.9979 0.0890 1.0000 Uiso R . . . . .
H762 H 0.9037 0.6831 1.0057 0.0890 1.0000 Uiso R . . . . .
H763 H 0.8703 0.7114 0.9425 0.0891 1.0000 Uiso R . . . . .
H781 H 1.0492 0.5478 0.8197 0.1150 1.0000 Uiso R . . . . .
H782 H 0.9849 0.5440 0.8593 0.1151 1.0000 Uiso R . . . . .
H783 H 0.9817 0.5721 0.7906 0.1151 1.0000 Uiso R . . . . .
H793 H 1.1074 0.5686 0.9263 0.1180 1.0000 Uiso R . . . . .
H792 H 1.0943 0.6146 0.9637 0.1182 1.0000 Uiso R . . . . .
H791 H 1.0437 0.5735 0.9660 0.1180 1.0000 Uiso R . . . . .
H801 H 1.1141 0.6213 0.8237 0.1021 1.0000 Uiso R . . . . .
H802 H 1.0900 0.6642 0.8624 0.1021 1.0000 Uiso R . . . . .
H803 H 1.0493 0.6475 0.7937 0.1020 1.0000 Uiso R . . . . .
H823 H 1.1332 0.5419 1.1422 0.1451 1.0000 Uiso R . . . . .
H822 H 1.0584 0.5270 1.1474 0.1450 1.0000 Uiso R . . . . .
H821 H 1.0772 0.5515 1.0809 0.1450 1.0000 Uiso R . . . . .
H831 H 1.1348 0.5816 1.2536 0.1911 1.0000 Uiso R . . . . .
H832 H 1.0823 0.6211 1.2607 0.1910 1.0000 Uiso R . . . . .
H833 H 1.0582 0.5697 1.2592 0.1910 1.0000 Uiso R . . . . .
H841 H 1.1645 0.6240 1.1494 0.1021 1.0000 Uiso R . . . . .
H842 H 1.1072 0.6600 1.1592 0.1021 1.0000 Uiso R . . . . .
H843 H 1.1084 0.6350 1.0881 0.1021 1.0000 Uiso R . . . . .
H863 H 0.9265 0.6758 1.2735 0.1460 1.0000 Uiso R . . . . .
H862 H 0.9995 0.6554 1.2779 0.1460 1.0000 Uiso R . . . . .
H861 H 0.9365 0.6227 1.2687 0.1460 1.0000 Uiso R . . . . .
H871 H 0.8573 0.6868 1.1660 0.1140 1.0000 Uiso R . . . . .
H872 H 0.8534 0.6333 1.1696 0.1140 1.0000 Uiso R . . . . .
H873 H 0.8720 0.6573 1.1024 0.1140 1.0000 Uiso R . . . . .
H881 H 0.9613 0.7249 1.1765 0.1030 1.0000 Uiso R . . . . .
H882 H 1.0312 0.6996 1.1780 0.1030 1.0000 Uiso R . . . . .
H883 H 0.9818 0.7012 1.1100 0.1031 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.5807(18)
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 . Cl1 . 2.306(6) yes
Ti1 . Cl2 . 2.315(6) yes
Ti1 . O1 . 1.822(14) yes
Ti1 . O3 . 1.831(13) yes
Ti1 . P1 . 2.746(5) yes
Ti1 . P3 . 2.754(5) yes
Ti2 . Cl3 . 2.329(6) yes
Ti2 . Cl4 . 2.314(5) yes
Ti2 . O5 . 1.864(11) yes
Ti2 . O7 . 1.833(13) yes
Ti2 . P5 . 2.739(5) yes
Ti2 . P7 . 2.726(5) yes
O1 . C6 . 1.34(2) yes
O2 . P2 . 1.694(12) yes
O2 . C2 . 1.422(19) yes
O3 . C24 . 1.370(19) yes
O4 . P4 . 1.712(11) yes
O4 . C28 . 1.406(18) yes
O5 . C46 . 1.356(18) yes
O6 . P6 . 1.740(11) yes
O6 . C50 . 1.416(18) yes
O7 . C68 . 1.380(18) yes
O8 . P8 . 1.736(10) yes
O8 . C72 . 1.396(18) yes
P1 . C1 . 1.857(17) yes
P1 . C7 . 1.888(19) yes
P1 . C11 . 1.86(2) yes
P2 . C15 . 1.825(19) yes
P2 . C19 . 1.87(2) yes
P3 . C23 . 1.863(19) yes
P3 . C29 . 1.916(18) yes
P3 . C33 . 1.88(2) yes
P4 . C37 . 1.868(18) yes
P4 . C41 . 1.887(19) yes
P5 . C45 . 1.817(17) yes
P5 . C51 . 1.865(16) yes
P5 . C55 . 1.884(19) yes
P6 . C59 . 1.883(16) yes
P6 . C63 . 1.77(2) yes
P7 . C67 . 1.820(16) yes
P7 . C73 . 1.882(18) yes
P7 . C77 . 1.889(19) yes
P8 . C81 . 1.88(2) yes
P8 . C85 . 1.83(2) yes
C1 . C2 . 1.41(2) yes
C1 . C6 . 1.40(2) yes
C2 . C3 . 1.41(2) yes
C3 . C4 . 1.40(2) yes
C3 . H31 . 0.930 no
C4 . C5 . 1.40(2) yes
C4 . H41 . 0.935 no
C5 . C6 . 1.39(2) yes
C5 . H51 . 0.933 no
C7 . C8 . 1.43(3) yes
C7 . C9 . 1.64(3) yes
C7 . C10 . 1.55(3) yes
C8 . H81 . 0.962 no
C8 . H82 . 0.962 no
C8 . H83 . 0.963 no
C9 . H93 . 0.960 no
C9 . H92 . 0.965 no
C9 . H91 . 0.961 no
C10 . H101 . 0.971 no
C10 . H102 . 0.977 no
C10 . H103 . 0.973 no
C11 . C12 . 1.54(2) yes
C11 . C13 . 1.58(2) yes
C11 . C14 . 1.53(3) yes
C12 . H121 . 0.966 no
C12 . H122 . 0.966 no
C12 . H123 . 0.963 no
C13 . H133 . 0.962 no
C13 . H132 . 0.958 no
C13 . H131 . 0.967 no
C14 . H141 . 0.965 no
C14 . H142 . 0.962 no
C14 . H143 . 0.965 no
C15 . C16 . 1.59(2) yes
C15 . C17 . 1.50(3) yes
C15 . C18 . 1.54(2) yes
C16 . H163 . 0.964 no
C16 . H162 . 0.962 no
C16 . H161 . 0.964 no
C17 . H171 . 0.969 no
C17 . H172 . 0.971 no
C17 . H173 . 0.970 no
C18 . H181 . 0.960 no
C18 . H182 . 0.963 no
C18 . H183 . 0.967 no
C19 . C20 . 1.53(3) yes
C19 . C21 . 1.56(3) yes
C19 . C22 . 1.54(3) yes
C20 . H203 . 0.960 no
C20 . H202 . 0.961 no
C20 . H201 . 0.966 no
C21 . H211 . 0.959 no
C21 . H212 . 0.960 no
C21 . H213 . 0.962 no
C22 . H221 . 0.961 no
C22 . H222 . 0.962 no
C22 . H223 . 0.964 no
C23 . C24 . 1.43(2) yes
C23 . C28 . 1.39(2) yes
C24 . C25 . 1.39(3) yes
C25 . C26 . 1.33(2) yes
C25 . H251 . 0.930 no
C26 . C27 . 1.38(2) yes
C26 . H261 . 0.934 no
C27 . C28 . 1.39(2) yes
C27 . H271 . 0.931 no
C29 . C30 . 1.54(3) yes
C29 . C31 . 1.57(3) yes
C29 . C32 . 1.52(2) yes
C30 . H301 . 0.961 no
C30 . H302 . 0.964 no
C30 . H303 . 0.965 no
C31 . H313 . 0.962 no
C31 . H312 . 0.964 no
C31 . H311 . 0.961 no
C32 . H321 . 0.957 no
C32 . H322 . 0.961 no
C32 . H323 . 0.963 no
C33 . C34 . 1.49(3) yes
C33 . C35 . 1.52(2) yes
C33 . C36 . 1.55(2) yes
C34 . H341 . 0.964 no
C34 . H342 . 0.958 no
C34 . H343 . 0.958 no
C35 . H353 . 0.965 no
C35 . H352 . 0.961 no
C35 . H351 . 0.966 no
C36 . H361 . 0.960 no
C36 . H362 . 0.964 no
C36 . H363 . 0.961 no
C37 . C38 . 1.57(3) yes
C37 . C39 . 1.54(3) yes
C37 . C40 . 1.49(2) yes
C38 . H383 . 0.960 no
C38 . H382 . 0.960 no
C38 . H381 . 0.962 no
C39 . H391 . 0.955 no
C39 . H392 . 0.958 no
C39 . H393 . 0.963 no
C40 . H401 . 0.958 no
C40 . H402 . 0.956 no
C40 . H403 . 0.959 no
C41 . C42 . 1.52(3) yes
C41 . C43 . 1.52(2) yes
C41 . C44 . 1.54(2) yes
C42 . H423 . 0.955 no
C42 . H422 . 0.958 no
C42 . H421 . 0.957 no
C43 . H431 . 0.956 no
C43 . H432 . 0.960 no
C43 . H433 . 0.956 no
C44 . H441 . 0.959 no
C44 . H442 . 0.961 no
C44 . H443 . 0.962 no
C45 . C46 . 1.41(2) yes
C45 . C50 . 1.44(2) yes
C46 . C47 . 1.40(2) yes
C47 . C48 . 1.37(2) yes
C47 . H471 . 0.933 no
C48 . C49 . 1.42(2) yes
C48 . H481 . 0.932 no
C49 . C50 . 1.38(2) yes
C49 . H491 . 0.935 no
C51 . C52 . 1.59(2) yes
C51 . C53 . 1.56(3) yes
C51 . C54 . 1.55(2) yes
C52 . H521 . 0.963 no
C52 . H522 . 0.963 no
C52 . H523 . 0.965 no
C53 . H533 . 0.964 no
C53 . H532 . 0.960 no
C53 . H531 . 0.966 no
C54 . H541 . 0.958 no
C54 . H542 . 0.954 no
C54 . H543 . 0.959 no
C55 . C56 . 1.52(2) yes
C55 . C57 . 1.54(2) yes
C55 . C58 . 1.55(2) yes
C56 . H561 . 0.967 no
C56 . H562 . 0.958 no
C56 . H563 . 0.966 no
C57 . H573 . 0.966 no
C57 . H572 . 0.958 no
C57 . H571 . 0.962 no
C58 . H581 . 0.959 no
C58 . H582 . 0.961 no
C58 . H583 . 0.964 no
C59 . C60 . 1.51(3) yes
C59 . C61 . 1.51(3) yes
C59 . C62 . 1.60(2) yes
C60 . H603 . 0.955 no
C60 . H602 . 0.961 no
C60 . H601 . 0.960 no
C61 . H611 . 0.956 no
C61 . H612 . 0.961 no
C61 . H613 . 0.960 no
C62 . H621 . 0.958 no
C62 . H622 . 0.961 no
C62 . H623 . 0.963 no
C63 . C64 . 1.54(3) yes
C63 . C65 . 1.56(2) yes
C63 . C66 . 1.59(2) yes
C64 . H643 . 0.963 no
C64 . H642 . 0.964 no
C64 . H641 . 0.956 no
C65 . H651 . 0.959 no
C65 . H652 . 0.963 no
C65 . H653 . 0.955 no
C66 . H661 . 0.966 no
C66 . H662 . 0.963 no
C66 . H663 . 0.964 no
C67 . C68 . 1.45(2) yes
C67 . C72 . 1.44(2) yes
C68 . C69 . 1.34(2) yes
C69 . C70 . 1.42(2) yes
C69 . H691 . 0.932 no
C70 . C71 . 1.39(2) yes
C70 . H701 . 0.932 no
C71 . C72 . 1.37(2) yes
C71 . H711 . 0.936 no
C73 . C74 . 1.53(2) yes
C73 . C75 . 1.56(2) yes
C73 . C76 . 1.54(2) yes
C74 . H741 . 0.964 no
C74 . H742 . 0.963 no
C74 . H743 . 0.958 no
C75 . H753 . 0.967 no
C75 . H752 . 0.961 no
C75 . H751 . 0.965 no
C76 . H761 . 0.966 no
C76 . H762 . 0.966 no
C76 . H763 . 0.958 no
C77 . C78 . 1.55(3) yes
C77 . C79 . 1.52(2) yes
C77 . C80 . 1.49(2) yes
C78 . H781 . 0.962 no
C78 . H782 . 0.969 no
C78 . H783 . 0.963 no
C79 . H793 . 0.960 no
C79 . H792 . 0.960 no
C79 . H791 . 0.966 no
C80 . H801 . 0.959 no
C80 . H802 . 0.966 no
C80 . H803 . 0.958 no
C81 . C82 . 1.49(3) yes
C81 . C83 . 1.58(3) yes
C81 . C84 . 1.50(3) yes
C82 . H823 . 0.957 no
C82 . H822 . 0.966 no
C82 . H821 . 0.964 no
C83 . H831 . 0.960 no
C83 . H832 . 0.961 no
C83 . H833 . 0.965 no
C84 . H841 . 0.961 no
C84 . H842 . 0.969 no
C84 . H843 . 0.963 no
C85 . C86 . 1.50(2) yes
C85 . C87 . 1.54(2) yes
C85 . C88 . 1.52(3) yes
C86 . H863 . 0.961 no
C86 . H862 . 0.956 no
C86 . H861 . 0.964 no
C87 . H871 . 0.962 no
C87 . H872 . 0.961 no
C87 . H873 . 0.959 no
C88 . H881 . 0.964 no
C88 . H882 . 0.958 no
C88 . H883 . 0.961 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
Cl1 . Ti1 . Cl2 . 95.3(2) yes
Cl1 . Ti1 . O1 . 157.4(4) yes
Cl2 . Ti1 . O1 . 92.2(5) yes
Cl1 . Ti1 . O3 . 92.3(5) yes
Cl2 . Ti1 . O3 . 155.7(5) yes
O1 . Ti1 . O3 . 89.5(6) yes
Cl1 . Ti1 . P1 . 86.86(19) yes
Cl2 . Ti1 . P1 . 94.14(19) yes
O1 . Ti1 . P1 . 71.3(4) yes
O3 . Ti1 . P1 . 109.3(4) yes
Cl1 . Ti1 . P3 . 91.76(19) yes
Cl2 . Ti1 . P3 . 86.78(18) yes
O1 . Ti1 . P3 . 110.0(4) yes
O3 . Ti1 . P3 . 69.9(4) yes
P1 . Ti1 . P3 . 178.4(2) yes
Cl3 . Ti2 . Cl4 . 100.4(2) yes
Cl3 . Ti2 . O5 . 153.9(4) yes
Cl4 . Ti2 . O5 . 90.9(4) yes
Cl3 . Ti2 . O7 . 92.1(4) yes
Cl4 . Ti2 . O7 . 154.1(4) yes
O5 . Ti2 . O7 . 87.4(5) yes
Cl3 . Ti2 . P5 . 86.04(17) yes
Cl4 . Ti2 . P5 . 87.87(17) yes
O5 . Ti2 . P5 . 70.8(4) yes
O7 . Ti2 . P5 . 115.8(4) yes
Cl3 . Ti2 . P7 . 87.55(17) yes
Cl4 . Ti2 . P7 . 86.36(17) yes
O5 . Ti2 . P7 . 116.8(4) yes
O7 . Ti2 . P7 . 71.5(4) yes
P5 . Ti2 . P7 . 170.5(2) yes
Ti1 . O1 . C6 . 141.0(11) yes
P2 . O2 . C2 . 119.5(11) yes
Ti1 . O3 . C24 . 143.1(12) yes
P4 . O4 . C28 . 120.3(11) yes
Ti2 . O5 . C46 . 138.2(11) yes
P6 . O6 . C50 . 118.2(10) yes
Ti2 . O7 . C68 . 138.7(10) yes
P8 . O8 . C72 . 118.7(9) yes
Ti1 . P1 . C1 . 96.7(5) yes
Ti1 . P1 . C7 . 109.4(6) yes
C1 . P1 . C7 . 103.2(10) yes
Ti1 . P1 . C11 . 119.0(6) yes
C1 . P1 . C11 . 110.3(7) yes
C7 . P1 . C11 . 115.4(9) yes
O2 . P2 . C15 . 102.9(8) yes
O2 . P2 . C19 . 99.2(8) yes
C15 . P2 . C19 . 110.7(9) yes
Ti1 . P3 . C23 . 98.4(5) yes
Ti1 . P3 . C29 . 110.7(5) yes
C23 . P3 . C29 . 104.2(9) yes
Ti1 . P3 . C33 . 119.6(7) yes
C23 . P3 . C33 . 110.4(8) yes
C29 . P3 . C33 . 111.7(9) yes
O4 . P4 . C37 . 101.6(6) yes
O4 . P4 . C41 . 101.4(7) yes
C37 . P4 . C41 . 110.4(9) yes
Ti2 . P5 . C45 . 96.3(5) yes
Ti2 . P5 . C51 . 109.1(5) yes
C45 . P5 . C51 . 105.0(8) yes
Ti2 . P5 . C55 . 119.8(5) yes
C45 . P5 . C55 . 111.5(8) yes
C51 . P5 . C55 . 113.1(8) yes
O6 . P6 . C59 . 99.0(6) yes
O6 . P6 . C63 . 101.3(7) yes
C59 . P6 . C63 . 111.5(10) yes
Ti2 . P7 . C67 . 97.4(5) yes
Ti2 . P7 . C73 . 120.2(5) yes
C67 . P7 . C73 . 110.2(7) yes
Ti2 . P7 . C77 . 109.3(7) yes
C67 . P7 . C77 . 105.8(8) yes
C73 . P7 . C77 . 112.2(9) yes
O8 . P8 . C81 . 98.7(7) yes
O8 . P8 . C85 . 102.1(7) yes
C81 . P8 . C85 . 111.8(9) yes
P1 . C1 . C2 . 132.5(13) yes
P1 . C1 . C6 . 108.9(12) yes
C2 . C1 . C6 . 118.5(16) yes
O2 . C2 . C1 . 121.5(15) yes
O2 . C2 . C3 . 120.1(15) yes
C1 . C2 . C3 . 118.4(16) yes
C2 . C3 . C4 . 122.4(18) yes
C2 . C3 . H31 . 118.3 no
C4 . C3 . H31 . 119.3 no
C3 . C4 . C5 . 118.4(18) yes
C3 . C4 . H41 . 120.8 no
C5 . C4 . H41 . 120.9 no
C4 . C5 . C6 . 119.8(15) yes
C4 . C5 . H51 . 120.6 no
C6 . C5 . H51 . 119.7 no
C1 . C6 . C5 . 122.3(16) yes
C1 . C6 . O1 . 121.4(15) yes
C5 . C6 . O1 . 116.3(14) yes
P1 . C7 . C8 . 110.9(14) yes
P1 . C7 . C9 . 105.5(15) yes
C8 . C7 . C9 . 111.5(18) yes
P1 . C7 . C10 . 113.8(13) yes
C8 . C7 . C10 . 110(2) yes
C9 . C7 . C10 . 105.2(16) yes
C7 . C8 . H81 . 110.9 no
C7 . C8 . H82 . 108.5 no
H81 . C8 . H82 . 109.8 no
C7 . C8 . H83 . 109.5 no
H81 . C8 . H83 . 108.4 no
H82 . C8 . H83 . 109.7 no
C7 . C9 . H93 . 108.5 no
C7 . C9 . H92 . 108.9 no
H93 . C9 . H92 . 109.6 no
C7 . C9 . H91 . 109.6 no
H93 . C9 . H91 . 110.4 no
H92 . C9 . H91 . 109.8 no
C7 . C10 . H101 . 108.8 no
C7 . C10 . H102 . 108.3 no
H101 . C10 . H102 . 110.7 no
C7 . C10 . H103 . 108.7 no
H101 . C10 . H103 . 109.7 no
H102 . C10 . H103 . 110.6 no
P1 . C11 . C12 . 106.5(12) yes
P1 . C11 . C13 . 116.2(15) yes
C12 . C11 . C13 . 107.8(14) yes
P1 . C11 . C14 . 108.7(12) yes
C12 . C11 . C14 . 106.7(18) yes
C13 . C11 . C14 . 110.5(15) yes
C11 . C12 . H121 . 109.3 no
C11 . C12 . H122 . 109.5 no
H121 . C12 . H122 . 109.5 no
C11 . C12 . H123 . 108.4 no
H121 . C12 . H123 . 110.1 no
H122 . C12 . H123 . 110.1 no
C11 . C13 . H133 . 110.0 no
C11 . C13 . H132 . 109.5 no
H133 . C13 . H132 . 109.5 no
C11 . C13 . H131 . 108.7 no
H133 . C13 . H131 . 109.7 no
H132 . C13 . H131 . 109.4 no
C11 . C14 . H141 . 109.6 no
C11 . C14 . H142 . 110.0 no
H141 . C14 . H142 . 109.3 no
C11 . C14 . H143 . 109.2 no
H141 . C14 . H143 . 109.4 no
H142 . C14 . H143 . 109.3 no
P2 . C15 . C16 . 105.6(13) yes
P2 . C15 . C17 . 122.2(13) yes
C16 . C15 . C17 . 104.4(17) yes
P2 . C15 . C18 . 109.1(14) yes
C16 . C15 . C18 . 104.9(14) yes
C17 . C15 . C18 . 109.2(16) yes
C15 . C16 . H163 . 109.6 no
C15 . C16 . H162 . 110.3 no
H163 . C16 . H162 . 108.9 no
C15 . C16 . H161 . 109.0 no
H163 . C16 . H161 . 109.5 no
H162 . C16 . H161 . 109.5 no
C15 . C17 . H171 . 110.5 no
C15 . C17 . H172 . 108.0 no
H171 . C17 . H172 . 109.8 no
C15 . C17 . H173 . 109.0 no
H171 . C17 . H173 . 109.5 no
H172 . C17 . H173 . 110.1 no
C15 . C18 . H181 . 109.9 no
C15 . C18 . H182 . 108.2 no
H181 . C18 . H182 . 109.1 no
C15 . C18 . H183 . 109.8 no
H181 . C18 . H183 . 109.9 no
H182 . C18 . H183 . 109.8 no
P2 . C19 . C20 . 105.3(15) yes
P2 . C19 . C21 . 116.5(13) yes
C20 . C19 . C21 . 110.8(19) yes
P2 . C19 . C22 . 106.3(16) yes
C20 . C19 . C22 . 105.8(19) yes
C21 . C19 . C22 . 111.4(18) yes
C19 . C20 . H203 . 110.2 no
C19 . C20 . H202 . 109.4 no
H203 . C20 . H202 . 109.7 no
C19 . C20 . H201 . 108.9 no
H203 . C20 . H201 . 109.2 no
H202 . C20 . H201 . 109.4 no
C19 . C21 . H211 . 109.0 no
C19 . C21 . H212 . 110.3 no
H211 . C21 . H212 . 109.4 no
C19 . C21 . H213 . 109.1 no
H211 . C21 . H213 . 109.9 no
H212 . C21 . H213 . 109.3 no
C19 . C22 . H221 . 110.2 no
C19 . C22 . H222 . 109.0 no
H221 . C22 . H222 . 109.6 no
C19 . C22 . H223 . 109.8 no
H221 . C22 . H223 . 108.9 no
H222 . C22 . H223 . 109.4 no
P3 . C23 . C24 . 108.1(13) yes
P3 . C23 . C28 . 136.6(13) yes
C24 . C23 . C28 . 115.0(16) yes
C23 . C24 . O3 . 119.1(16) yes
C23 . C24 . C25 . 122.1(16) yes
O3 . C24 . C25 . 118.6(15) yes
C24 . C25 . C26 . 119.4(17) yes
C24 . C25 . H251 . 120.3 no
C26 . C25 . H251 . 120.3 no
C25 . C26 . C27 . 121.9(17) yes
C25 . C26 . H261 . 119.4 no
C27 . C26 . H261 . 118.8 no
C26 . C27 . C28 . 118.6(15) yes
C26 . C27 . H271 . 120.3 no
C28 . C27 . H271 . 121.0 no
O4 . C28 . C27 . 118.8(14) yes
O4 . C28 . C23 . 118.7(15) yes
C27 . C28 . C23 . 122.2(15) yes
P3 . C29 . C30 . 104.8(12) yes
P3 . C29 . C31 . 106.9(15) yes
C30 . C29 . C31 . 110.9(17) yes
P3 . C29 . C32 . 114.4(13) yes
C30 . C29 . C32 . 109(2) yes
C31 . C29 . C32 . 110.6(17) yes
C29 . C30 . H301 . 109.1 no
C29 . C30 . H302 . 109.1 no
H301 . C30 . H302 . 109.6 no
C29 . C30 . H303 . 110.7 no
H301 . C30 . H303 . 108.9 no
H302 . C30 . H303 . 109.4 no
C29 . C31 . H313 . 107.5 no
C29 . C31 . H312 . 109.6 no
H313 . C31 . H312 . 109.8 no
C29 . C31 . H311 . 109.7 no
H313 . C31 . H311 . 110.3 no
H312 . C31 . H311 . 110.0 no
C29 . C32 . H321 . 109.4 no
C29 . C32 . H322 . 108.4 no
H321 . C32 . H322 . 110.0 no
C29 . C32 . H323 . 109.8 no
H321 . C32 . H323 . 109.1 no
H322 . C32 . H323 . 110.2 no
P3 . C33 . C34 . 110.4(12) yes
P3 . C33 . C35 . 115.0(16) yes
C34 . C33 . C35 . 110.1(17) yes
P3 . C33 . C36 . 107.7(14) yes
C34 . C33 . C36 . 105.7(18) yes
C35 . C33 . C36 . 107.5(14) yes
C33 . C34 . H341 . 109.0 no
C33 . C34 . H342 . 110.3 no
H341 . C34 . H342 . 110.0 no
C33 . C34 . H343 . 108.0 no
H341 . C34 . H343 . 110.0 no
H342 . C34 . H343 . 109.6 no
C33 . C35 . H353 . 108.5 no
C33 . C35 . H352 . 110.2 no
H353 . C35 . H352 . 109.5 no
C33 . C35 . H351 . 109.4 no
H353 . C35 . H351 . 110.1 no
H352 . C35 . H351 . 109.1 no
C33 . C36 . H361 . 107.9 no
C33 . C36 . H362 . 109.6 no
H361 . C36 . H362 . 109.6 no
C33 . C36 . H363 . 109.4 no
H361 . C36 . H363 . 110.0 no
H362 . C36 . H363 . 110.3 no
P4 . C37 . C38 . 102.4(13) yes
P4 . C37 . C39 . 116.1(14) yes
C38 . C37 . C39 . 109.7(16) yes
P4 . C37 . C40 . 108.9(12) yes
C38 . C37 . C40 . 105.3(19) yes
C39 . C37 . C40 . 113.3(18) yes
C37 . C38 . H383 . 109.9 no
C37 . C38 . H382 . 109.4 no
H383 . C38 . H382 . 109.6 no
C37 . C38 . H381 . 109.1 no
H383 . C38 . H381 . 109.2 no
H382 . C38 . H381 . 109.6 no
C37 . C39 . H391 . 110.3 no
C37 . C39 . H392 . 108.7 no
H391 . C39 . H392 . 109.3 no
C37 . C39 . H393 . 109.6 no
H391 . C39 . H393 . 109.7 no
H392 . C39 . H393 . 109.3 no
C37 . C40 . H401 . 109.1 no
C37 . C40 . H402 . 108.1 no
H401 . C40 . H402 . 109.9 no
C37 . C40 . H403 . 111.0 no
H401 . C40 . H403 . 108.8 no
H402 . C40 . H403 . 110.0 no
P4 . C41 . C42 . 118.6(12) yes
P4 . C41 . C43 . 104.9(14) yes
C42 . C41 . C43 . 111.5(16) yes
P4 . C41 . C44 . 105.5(13) yes
C42 . C41 . C44 . 108.0(17) yes
C43 . C41 . C44 . 107.8(14) yes
C41 . C42 . H423 . 108.8 no
C41 . C42 . H422 . 108.9 no
H423 . C42 . H422 . 109.2 no
C41 . C42 . H421 . 111.2 no
H423 . C42 . H421 . 109.3 no
H422 . C42 . H421 . 109.4 no
C41 . C43 . H431 . 108.7 no
C41 . C43 . H432 . 109.1 no
H431 . C43 . H432 . 110.2 no
C41 . C43 . H433 . 109.6 no
H431 . C43 . H433 . 109.4 no
H432 . C43 . H433 . 109.8 no
C41 . C44 . H441 . 109.7 no
C41 . C44 . H442 . 109.0 no
H441 . C44 . H442 . 108.7 no
C41 . C44 . H443 . 109.9 no
H441 . C44 . H443 . 109.8 no
H442 . C44 . H443 . 109.8 no
P5 . C45 . C46 . 112.1(12) yes
P5 . C45 . C50 . 134.0(13) yes
C46 . C45 . C50 . 113.9(15) yes
C45 . C46 . O5 . 117.6(16) yes
C45 . C46 . C47 . 124.7(15) yes
O5 . C46 . C47 . 117.0(15) yes
C46 . C47 . C48 . 118.3(17) yes
C46 . C47 . H471 . 120.1 no
C48 . C47 . H471 . 121.5 no
C47 . C48 . C49 . 120.5(16) yes
C47 . C48 . H481 . 119.8 no
C49 . C48 . H481 . 119.8 no
C48 . C49 . C50 . 119.6(15) yes
C48 . C49 . H491 . 120.6 no
C50 . C49 . H491 . 119.7 no
C45 . C50 . O6 . 117.6(14) yes
C45 . C50 . C49 . 122.5(15) yes
O6 . C50 . C49 . 119.8(14) yes
P5 . C51 . C52 . 114.5(11) yes
P5 . C51 . C53 . 106.8(11) yes
C52 . C51 . C53 . 105.5(16) yes
P5 . C51 . C54 . 111.3(13) yes
C52 . C51 . C54 . 111.1(14) yes
C53 . C51 . C54 . 107.1(14) yes
C51 . C52 . H521 . 107.8 no
C51 . C52 . H522 . 108.9 no
H521 . C52 . H522 . 110.5 no
C51 . C52 . H523 . 109.1 no
H521 . C52 . H523 . 109.9 no
H522 . C52 . H523 . 110.6 no
C51 . C53 . H533 . 109.5 no
C51 . C53 . H532 . 109.5 no
H533 . C53 . H532 . 109.5 no
C51 . C53 . H531 . 108.9 no
H533 . C53 . H531 . 109.6 no
H532 . C53 . H531 . 109.8 no
C51 . C54 . H541 . 109.0 no
C51 . C54 . H542 . 110.3 no
H541 . C54 . H542 . 109.6 no
C51 . C54 . H543 . 108.3 no
H541 . C54 . H543 . 110.1 no
H542 . C54 . H543 . 109.5 no
P5 . C55 . C56 . 108.4(12) yes
P5 . C55 . C57 . 108.6(12) yes
C56 . C55 . C57 . 109.2(15) yes
P5 . C55 . C58 . 113.5(13) yes
C56 . C55 . C58 . 108.6(14) yes
C57 . C55 . C58 . 108.5(14) yes
C55 . C56 . H561 . 107.6 no
C55 . C56 . H562 . 109.6 no
H561 . C56 . H562 . 109.8 no
C55 . C56 . H563 . 110.6 no
H561 . C56 . H563 . 109.7 no
H562 . C56 . H563 . 109.6 no
C55 . C57 . H573 . 109.0 no
C55 . C57 . H572 . 109.9 no
H573 . C57 . H572 . 109.0 no
C55 . C57 . H571 . 110.0 no
H573 . C57 . H571 . 109.3 no
H572 . C57 . H571 . 109.7 no
C55 . C58 . H581 . 109.3 no
C55 . C58 . H582 . 110.5 no
H581 . C58 . H582 . 109.5 no
C55 . C58 . H583 . 108.9 no
H581 . C58 . H583 . 109.0 no
H582 . C58 . H583 . 109.6 no
P6 . C59 . C60 . 104.5(14) yes
P6 . C59 . C61 . 118.6(15) yes
C60 . C59 . C61 . 111.0(17) yes
P6 . C59 . C62 . 105.0(11) yes
C60 . C59 . C62 . 109.0(18) yes
C61 . C59 . C62 . 108.2(17) yes
C59 . C60 . H603 . 110.2 no
C59 . C60 . H602 . 109.1 no
H603 . C60 . H602 . 109.4 no
C59 . C60 . H601 . 109.4 no
H603 . C60 . H601 . 109.2 no
H602 . C60 . H601 . 109.5 no
C59 . C61 . H611 . 110.2 no
C59 . C61 . H612 . 107.2 no
H611 . C61 . H612 . 109.6 no
C59 . C61 . H613 . 111.3 no
H611 . C61 . H613 . 109.2 no
H612 . C61 . H613 . 109.4 no
C59 . C62 . H621 . 109.6 no
C59 . C62 . H622 . 108.2 no
H621 . C62 . H622 . 109.7 no
C59 . C62 . H623 . 109.4 no
H621 . C62 . H623 . 109.6 no
H622 . C62 . H623 . 110.3 no
P6 . C63 . C64 . 122.0(14) yes
P6 . C63 . C65 . 112.0(15) yes
C64 . C63 . C65 . 105.7(16) yes
P6 . C63 . C66 . 107.0(13) yes
C64 . C63 . C66 . 105.3(17) yes
C65 . C63 . C66 . 103.0(15) yes
C63 . C64 . H643 . 110.7 no
C63 . C64 . H642 . 109.0 no
H643 . C64 . H642 . 109.7 no
C63 . C64 . H641 . 108.7 no
H643 . C64 . H641 . 109.9 no
H642 . C64 . H641 . 108.8 no
C63 . C65 . H651 . 109.3 no
C63 . C65 . H652 . 109.5 no
H651 . C65 . H652 . 109.3 no
C63 . C65 . H653 . 109.6 no
H651 . C65 . H653 . 109.1 no
H652 . C65 . H653 . 110.0 no
C63 . C66 . H661 . 109.4 no
C63 . C66 . H662 . 108.6 no
H661 . C66 . H662 . 109.8 no
C63 . C66 . H663 . 109.1 no
H661 . C66 . H663 . 110.2 no
H662 . C66 . H663 . 109.7 no
P7 . C67 . C68 . 109.7(11) yes
P7 . C67 . C72 . 134.8(12) yes
C68 . C67 . C72 . 115.1(14) yes
C67 . C68 . O7 . 118.3(14) yes
C67 . C68 . C69 . 123.6(15) yes
O7 . C68 . C69 . 118.1(14) yes
C68 . C69 . C70 . 119.5(15) yes
C68 . C69 . H691 . 119.9 no
C70 . C69 . H691 . 120.5 no
C69 . C70 . C71 . 118.9(17) yes
C69 . C70 . H701 . 121.0 no
C71 . C70 . H701 . 120.1 no
C70 . C71 . C72 . 122.0(16) yes
C70 . C71 . H711 . 119.1 no
C72 . C71 . H711 . 118.9 no
C67 . C72 . O8 . 117.1(14) yes
C67 . C72 . C71 . 120.9(15) yes
O8 . C72 . C71 . 121.9(13) yes
P7 . C73 . C74 . 109.3(11) yes
P7 . C73 . C75 . 115.1(13) yes
C74 . C73 . C75 . 108.8(14) yes
P7 . C73 . C76 . 109.3(12) yes
C74 . C73 . C76 . 105.5(14) yes
C75 . C73 . C76 . 108.3(13) yes
C73 . C74 . H741 . 109.5 no
C73 . C74 . H742 . 109.8 no
H741 . C74 . H742 . 109.6 no
C73 . C74 . H743 . 108.6 no
H741 . C74 . H743 . 109.3 no
H742 . C74 . H743 . 109.9 no
C73 . C75 . H753 . 109.1 no
C73 . C75 . H752 . 108.4 no
H753 . C75 . H752 . 110.0 no
C73 . C75 . H751 . 110.2 no
H753 . C75 . H751 . 109.7 no
H752 . C75 . H751 . 109.4 no
C73 . C76 . H761 . 108.6 no
C73 . C76 . H762 . 109.5 no
H761 . C76 . H762 . 110.1 no
C73 . C76 . H763 . 109.8 no
H761 . C76 . H763 . 109.1 no
H762 . C76 . H763 . 109.6 no
P7 . C77 . C78 . 106.4(13) yes
P7 . C77 . C79 . 113.5(13) yes
C78 . C77 . C79 . 104.3(18) yes
P7 . C77 . C80 . 110.2(14) yes
C78 . C77 . C80 . 112.0(17) yes
C79 . C77 . C80 . 110.3(16) yes
C77 . C78 . H781 . 109.9 no
C77 . C78 . H782 . 109.7 no
H781 . C78 . H782 . 109.3 no
C77 . C78 . H783 . 109.7 no
H781 . C78 . H783 . 109.0 no
H782 . C78 . H783 . 109.2 no
C77 . C79 . H793 . 109.7 no
C77 . C79 . H792 . 108.8 no
H793 . C79 . H792 . 110.1 no
C77 . C79 . H791 . 109.6 no
H793 . C79 . H791 . 108.9 no
H792 . C79 . H791 . 109.8 no
C77 . C80 . H801 . 109.6 no
C77 . C80 . H802 . 111.0 no
H801 . C80 . H802 . 109.7 no
C77 . C80 . H803 . 108.9 no
H801 . C80 . H803 . 108.5 no
H802 . C80 . H803 . 109.2 no
P8 . C81 . C82 . 104.2(16) yes
P8 . C81 . C83 . 103.2(14) yes
C82 . C81 . C83 . 109(2) yes
P8 . C81 . C84 . 119.1(14) yes
C82 . C81 . C84 . 112.0(19) yes
C83 . C81 . C84 . 108(2) yes
C81 . C82 . H823 . 109.2 no
C81 . C82 . H822 . 110.1 no
H823 . C82 . H822 . 108.8 no
C81 . C82 . H821 . 110.5 no
H823 . C82 . H821 . 109.2 no
H822 . C82 . H821 . 109.0 no
C81 . C83 . H831 . 108.6 no
C81 . C83 . H832 . 107.7 no
H831 . C83 . H832 . 110.2 no
C81 . C83 . H833 . 109.9 no
H831 . C83 . H833 . 109.9 no
H832 . C83 . H833 . 110.5 no
C81 . C84 . H841 . 109.4 no
C81 . C84 . H842 . 108.4 no
H841 . C84 . H842 . 109.9 no
C81 . C84 . H843 . 109.8 no
H841 . C84 . H843 . 109.8 no
H842 . C84 . H843 . 109.4 no
P8 . C85 . C86 . 108.7(16) yes
P8 . C85 . C87 . 103.7(15) yes
C86 . C85 . C87 . 107.1(15) yes
P8 . C85 . C88 . 118.2(13) yes
C86 . C85 . C88 . 111.8(19) yes
C87 . C85 . C88 . 106.5(16) yes
C85 . C86 . H863 . 109.0 no
C85 . C86 . H862 . 109.9 no
H863 . C86 . H862 . 109.0 no
C85 . C86 . H861 . 109.3 no
H863 . C86 . H861 . 109.6 no
H862 . C86 . H861 . 109.9 no
C85 . C87 . H871 . 109.6 no
C85 . C87 . H872 . 107.3 no
H871 . C87 . H872 . 110.1 no
C85 . C87 . H873 . 109.6 no
H871 . C87 . H873 . 109.9 no
H872 . C87 . H873 . 110.3 no
C85 . C88 . H881 . 108.7 no
C85 . C88 . H882 . 109.5 no
H881 . C88 . H882 . 109.8 no
C85 . C88 . H883 . 110.6 no
H881 . C88 . H883 . 109.5 no
H882 . C88 . H883 . 108.7 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
C8 . H82 . O3 . 144 0.96 2.43 3.25(3) yes
C13 . H131 . O2 . 146 0.97 2.38 3.23(3) yes
C30 . H302 . O1 . 163 0.96 2.31 3.24(3) yes
C35 . H351 . O4 . 145 0.97 2.48 3.32(3) yes
C56 . H563 . O6 . 139 0.97 2.57 3.36(3) yes
C58 . H583 . O6 . 144 0.96 2.46 3.29(3) yes
C75 . H751 . O8 . 143 0.97 2.44 3.27(3) yes
C78 . H783 . O5 . 158 0.96 2.50 3.42(3) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
# looking for PLATON_SQD.SQF 

# SQUEEZE RESULTS (Version = 291119) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 1107 235 ' '
2 0.000 0.500 0.000 7 1 ' '
3 0.500 0.500 0.500 1107 235 ' '
4 0.844 0.000 0.250 7 1 ' '
5 0.156 0.500 0.250 7 1 ' '
6 0.000 0.000 0.500 7 1 ' '
7 0.156 0.000 0.750 7 1 ' '
8 0.844 0.500 0.750 7 1 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
# end of PLATON_SQD.SQF 

# start Validation Reply Form
_vrf_PLAT026_3                   
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        27% Check 
RESPONSE: Crystal data extremely weak and only used for connectivity
;
_vrf_PLAT027_3                   
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      33.96 Degree
RESPONSE: Crystal data extremely weak and only used for connectivity
;
_vrf_PLAT084_3                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.46 Report
RESPONSE: Crystal data extremely weak and only used for connectivity
;
_vrf_PLAT213_3                   
;
PROBLEM: Atom C62             has ADP max/min Ratio .....        7.6 prolat
RESPONSE: Crystal data extremely weak and only used for connectivity
;
_vrf_DIFMN02_3                   
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: Crystal data extremely weak and only used for connectivity
;
_vrf_PLAT098_3                   
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -2.53 eA-3  
RESPONSE: Crystal data extremely weak and only used for connectivity
;
_vrf_PLAT341_3                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02625 Ang.  
RESPONSE: Crystal data extremely weak and only used for connectivity
;
_vrf_PLAT934_3                   
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          2 Check 
RESPONSE: This is not a significant number of outliers 
and there is no systematic issue.
;
_vrf_PLAT990_3                   
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ...          ! Note 
RESPONSE: Noted as Squeeze.
;
# end Validation Reply Form


