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

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

data_SMR208
_database_code_depnum_ccdc_archive 'CCDC 759070'
_audit_update_record             
;
2009-12-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'SMR208.cif'

_audit_creation_date             09-10-02
_audit_creation_method           CRYSTALS_ver_12.87

_oxford_structure_analysis_title 'smr208 in P -1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.2836(6)
_cell_length_b                   10.7520(7)
_cell_length_c                   20.6254(10)
_cell_angle_alpha                83.935(5)
_cell_angle_beta                 79.557(6)
_cell_angle_gamma                68.034(6)
_cell_volume                     1876.1(2)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
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'
Nb -2.0727 0.6215 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957
3.7559 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C30 H60 Cl12 Nb6 O15 Sn6
# Dc = 4.17 Fooo = 984.00 Mu = 66.14 M = 2355.81
# Found Formula = C21 H50 Cl7 Nb1 O7 Sn2
# Dc = 1.76 FOOO = 984.00 Mu = 21.53 M = 993.08

_chemical_formula_sum            'C21 H50 Cl7 Nb1 O7 Sn2'
_chemical_formula_moiety         
;
C15 H35 Cl4 Nb O5 Sn, 0.5(C12 H30 Cl6 O4 Sn2)
;
_chemical_compound_source        ?
_chemical_formula_weight         993.08


_cell_measurement_reflns_used    9352
_cell_measurement_theta_min      3.3426
_cell_measurement_theta_max      29.4203
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.197
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_max          0.452

_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             984
_exptl_absorpt_coefficient_mu    2.153

# Sheldrick geometric approximatio 0.48 0.65
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_T_max  0.701
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;

_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            14493
_reflns_number_total             8720
_diffrn_reflns_av_R_equivalents  0.032
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 8720
# Theoretical number of reflections is about 20949


_diffrn_reflns_theta_min         3.355
_diffrn_reflns_theta_max         29.519
_diffrn_measured_fraction_theta_max 0.833

_diffrn_reflns_theta_full        25.977
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              -14
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              28

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -1.70
_refine_diff_density_max         1.31


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


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         8707
_refine_ls_number_restraints     0
_refine_ls_number_parameters     343
_oxford_refine_ls_R_factor_ref   0.0513
_refine_ls_wR_factor_ref         0.1109
_refine_ls_goodness_of_fit_ref   0.9527
_refine_ls_shift/su_max          0.0015505
_refine_ls_shift/su_mean         0.2104872


# The values computed from all data
_oxford_reflns_number_all        8707
_refine_ls_R_factor_all          0.0513
_refine_ls_wR_factor_all         0.1109

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7052
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_gt          0.1053

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method= Modified Sheldrick
w=1/[σ²(F²) + ( 0.07P)² + 3.14P]
,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 atomsattached to an atom.

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
C1 C -0.1563(4) 0.9720(4) 0.6734(2) 0.0265 1.0000 Uani . . . . . . .
C2 C -0.2415(5) 0.9100(6) 0.7282(3) 0.0421 1.0000 Uani . . . . . . .
C3 C -0.1769(5) 0.9450(5) 0.6061(2) 0.0324 1.0000 Uani . . . . . . .
C4 C 0.3884(5) 0.8609(4) 0.5508(2) 0.0278 1.0000 Uani . . . . . . .
C5 C 0.5530(5) 0.8091(5) 0.5694(3) 0.0374 1.0000 Uani . . . . . . .
C6 C 0.3715(6) 0.7738(5) 0.5027(2) 0.0334 1.0000 Uani . . . . . . .
C7 C 0.0724(5) 0.5843(4) 0.5756(2) 0.0306 1.0000 Uani . . . . . . .
C8 C -0.0184(7) 0.5206(6) 0.6267(3) 0.0524 1.0000 Uani . . . . . . .
C9 C 0.2125(7) 0.4836(6) 0.5372(3) 0.0530 1.0000 Uani . . . . . . .
C10 C 0.0447(6) 0.6299(5) 0.8112(2) 0.0318 1.0000 Uani . . . . . . .
C11 C 0.0100(8) 0.5043(6) 0.8113(3) 0.0522 1.0000 Uani . . . . . . .
C12 C 0.1591(8) 0.6185(7) 0.8560(3) 0.0531 1.0000 Uani . . . . . . .
C13 C 0.5446(5) 0.5063(5) 0.6782(3) 0.0354 1.0000 Uani . . . . . . .
C14 C 0.5982(6) 0.5543(5) 0.7318(3) 0.0415 1.0000 Uani . . . . . . .
C15 C 0.5214(8) 0.3749(6) 0.6964(4) 0.0680 1.0000 Uani . . . . . . .
C16 C 0.6500(9) 0.9411(7) 1.1073(3) 0.0612 1.0000 Uani . . . . . . .
C17 C 0.8136(8) 0.9269(9) 1.0915(3) 0.0780 1.0000 Uani . . . . . . .
C18 C 0.5989(8) 0.8490(8) 1.1555(3) 0.0732 1.0000 Uani . . . . . . .
C19 C 0.3859(6) 0.6767(5) 1.0358(3) 0.0415 1.0000 Uani . . . . . . .
C20 C 0.3718(10) 0.6321(7) 1.1069(3) 0.0739 1.0000 Uani . . . . . . .
C21 C 0.2398(12) 0.7035(10) 1.0082(5) 0.0989 1.0000 Uani . . . . . . .
O1 O 0.0118(3) 0.9211(3) 0.67907(13) 0.0208 1.0000 Uani . . . . . . .
O2 O 0.2705(3) 0.8715(3) 0.60933(14) 0.0230 1.0000 Uani . . . . . . .
O3 O 0.1232(3) 0.6700(3) 0.60743(14) 0.0229 1.0000 Uani . . . . . . .
O4 O 0.1057(3) 0.6610(3) 0.74462(14) 0.0259 1.0000 Uani . . . . . . .
O5 O 0.3975(3) 0.6052(3) 0.66382(15) 0.0268 1.0000 Uani . . . . . . .
O6 O 0.5698(4) 0.9693(3) 1.04877(14) 0.0292 1.0000 Uani . . . . . . .
O7 O 0.4225(4) 0.7984(3) 1.02792(17) 0.0382 1.0000 Uani . . . . . . .
Sn1 Sn 0.14374(3) 1.04558(3) 0.663866(14) 0.0214 1.0000 Uani . . . . . . .
Nb1 Nb 0.19503(4) 0.72877(3) 0.669689(17) 0.0183 1.0000 Uani . . . . . . .
Cl4 Cl 0.26988(12) 0.87284(10) 0.74971(5) 0.0276 1.0000 Uani . . . . . . .
H62 H 0.4429 0.7724 0.4626 0.0498 1.0000 Uiso R . . . . . .
H63 H 0.3956 0.6836 0.5209 0.0502 1.0000 Uiso R . . . . . .
H61 H 0.2659 0.8080 0.4929 0.0497 1.0000 Uiso R . . . . . .
H52 H 0.6280 0.8189 0.5324 0.0557 1.0000 Uiso R . . . . . .
H53 H 0.5540 0.8609 0.6043 0.0560 1.0000 Uiso R . . . . . .
H51 H 0.5830 0.7167 0.5845 0.0557 1.0000 Uiso R . . . . . .
H41 H 0.3646 0.9510 0.5308 0.0328 1.0000 Uiso R . . . . . .
H33 H -0.2837 0.9927 0.6004 0.0489 1.0000 Uiso R . . . . . .
H32 H -0.1518 0.8509 0.6026 0.0490 1.0000 Uiso R . . . . . .
H31 H -0.1092 0.9754 0.5727 0.0488 1.0000 Uiso R . . . . . .
H23 H -0.3516 0.9445 0.7248 0.0627 1.0000 Uiso R . . . . . .
H22 H -0.2308 0.9336 0.7705 0.0627 1.0000 Uiso R . . . . . .
H21 H -0.2009 0.8129 0.7258 0.0629 1.0000 Uiso R . . . . . .
H11 H -0.1964 1.0688 0.6773 0.0320 1.0000 Uiso R . . . . . .
H123 H 0.1135 0.6049 0.9006 0.0798 1.0000 Uiso R . . . . . .
H121 H 0.2548 0.5428 0.8437 0.0798 1.0000 Uiso R . . . . . .
H122 H 0.1822 0.6989 0.8524 0.0801 1.0000 Uiso R . . . . . .
H113 H -0.0275 0.4810 0.8555 0.0782 1.0000 Uiso R . . . . . .
H111 H 0.1035 0.4322 0.7943 0.0778 1.0000 Uiso R . . . . . .
H112 H -0.0689 0.5190 0.7843 0.0782 1.0000 Uiso R . . . . . .
H101 H -0.0525 0.7043 0.8242 0.0381 1.0000 Uiso R . . . . . .
H141 H 0.6972 0.4896 0.7410 0.0620 1.0000 Uiso R . . . . . .
H143 H 0.5205 0.5645 0.7706 0.0617 1.0000 Uiso R . . . . . .
H142 H 0.6089 0.6395 0.7183 0.0619 1.0000 Uiso R . . . . . .
H151 H 0.6167 0.3079 0.7083 0.1018 1.0000 Uiso R . . . . . .
H153 H 0.4365 0.3873 0.7327 0.1022 1.0000 Uiso R . . . . . .
H152 H 0.4946 0.3467 0.6588 0.1019 1.0000 Uiso R . . . . . .
H131 H 0.6237 0.4975 0.6387 0.0422 1.0000 Uiso R . . . . . .
H92 H 0.1780 0.4227 0.5195 0.0798 1.0000 Uiso R . . . . . .
H91 H 0.2877 0.4357 0.5659 0.0799 1.0000 Uiso R . . . . . .
H93 H 0.2576 0.5302 0.5022 0.0797 1.0000 Uiso R . . . . . .
H82 H -0.0614 0.4711 0.6052 0.0787 1.0000 Uiso R . . . . . .
H81 H 0.0509 0.4612 0.6559 0.0788 1.0000 Uiso R . . . . . .
H83 H -0.1020 0.5899 0.6516 0.0788 1.0000 Uiso R . . . . . .
H71 H 0.0026 0.6420 0.5447 0.0369 1.0000 Uiso R . . . . . .
Cl1 Cl 0.03251(14) 1.16957(11) 0.57151(6) 0.0341 1.0000 Uani . . . . . . .
Cl2 Cl -0.03019(14) 1.19520(11) 0.74420(6) 0.0348 1.0000 Uani . . . . . . .
Cl3 Cl 0.35027(14) 1.12928(12) 0.64916(6) 0.0371 1.0000 Uani . . . . . . .
Sn2 Sn 0.61293(4) 0.84822(3) 0.968921(15) 0.0297 1.0000 Uani . . . . . . .
Cl6 Cl 0.59449(17) 0.73797(14) 0.88014(6) 0.0460 1.0000 Uani . . . . . . .
Cl5 Cl 0.79355(17) 0.64892(12) 1.01030(7) 0.0490 1.0000 Uani . . . . . . .
Cl7 Cl 0.80752(14) 0.93384(12) 0.91126(6) 0.0376 1.0000 Uani . . . . . . .
H213 H 0.2226 0.6213 1.0071 0.1480 1.0000 Uiso R . . . . . .
H212 H 0.1526 0.7643 1.0357 0.1479 1.0000 Uiso R . . . . . .
H211 H 0.2475 0.7431 0.9645 0.1479 1.0000 Uiso R . . . . . .
H203 H 0.4672 0.6187 1.1233 0.1109 1.0000 Uiso R . . . . . .
H202 H 0.2857 0.6994 1.1314 0.1108 1.0000 Uiso R . . . . . .
H201 H 0.3527 0.5497 1.1121 0.1109 1.0000 Uiso R . . . . . .
H191 H 0.4736 0.6065 1.0108 0.0501 1.0000 Uiso R . . . . . .
H173 H 0.8553 0.9225 1.1310 0.1168 1.0000 Uiso R . . . . . .
H172 H 0.8220 1.0026 1.0639 0.1167 1.0000 Uiso R . . . . . .
H171 H 0.8695 0.8453 1.0687 0.1172 1.0000 Uiso R . . . . . .
H183 H 0.6359 0.8486 1.1963 0.1098 1.0000 Uiso R . . . . . .
H182 H 0.4866 0.8745 1.1633 0.1097 1.0000 Uiso R . . . . . .
H181 H 0.6455 0.7600 1.1389 0.1101 1.0000 Uiso R . . . . . .
H161 H 0.6005 1.0270 1.1301 0.0745 1.0000 Uiso R . . . . . .
H7 H 0.3471 0.8622 1.0430 0.0570 1.0000 Uiso R . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.84(4)
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 . 1.502(6) yes
C1 . C3 . 1.506(6) yes
C1 . O1 . 1.470(5) yes
C1 . H11 . 0.973 no
C2 . H23 . 0.961 no
C2 . H22 . 0.966 no
C2 . H21 . 0.972 no
C3 . H33 . 0.953 no
C3 . H32 . 0.957 no
C3 . H31 . 0.962 no
C4 . C5 . 1.524(6) yes
C4 . C6 . 1.500(6) yes
C4 . O2 . 1.458(5) yes
C4 . H41 . 0.973 no
C5 . H52 . 0.962 no
C5 . H53 . 0.958 no
C5 . H51 . 0.959 no
C6 . H62 . 0.959 no
C6 . H63 . 0.960 no
C6 . H61 . 0.960 no
C7 . C8 . 1.500(7) yes
C7 . C9 . 1.499(7) yes
C7 . O3 . 1.437(5) yes
C7 . H71 . 0.989 no
C8 . H82 . 0.955 no
C8 . H81 . 0.967 no
C8 . H83 . 0.961 no
C9 . H92 . 0.956 no
C9 . H91 . 0.958 no
C9 . H93 . 0.959 no
C10 . C11 . 1.500(7) yes
C10 . C12 . 1.493(7) yes
C10 . O4 . 1.443(5) yes
C10 . H101 . 0.972 no
C11 . H113 . 0.959 no
C11 . H111 . 0.960 no
C11 . H112 . 0.956 no
C12 . H123 . 0.962 no
C12 . H121 . 0.968 no
C12 . H122 . 0.958 no
C13 . C14 . 1.499(7) yes
C13 . C15 . 1.506(8) yes
C13 . O5 . 1.441(5) yes
C13 . H131 . 0.980 no
C14 . H141 . 0.960 no
C14 . H143 . 0.961 no
C14 . H142 . 0.964 no
C15 . H151 . 0.962 no
C15 . H153 . 0.964 no
C15 . H152 . 0.964 no
C16 . C17 . 1.446(10) yes
C16 . C18 . 1.472(10) yes
C16 . O6 . 1.478(6) yes
C16 . H161 . 0.991 no
C17 . H173 . 0.954 no
C17 . H172 . 0.962 no
C17 . H171 . 0.958 no
C18 . H183 . 0.964 no
C18 . H182 . 0.960 no
C18 . H181 . 0.963 no
C19 . C20 . 1.493(8) yes
C19 . C21 . 1.482(10) yes
C19 . O7 . 1.457(5) yes
C19 . H191 . 0.984 no
C20 . H203 . 0.961 no
C20 . H202 . 0.957 no
C20 . H201 . 0.958 no
C21 . H213 . 0.959 no
C21 . H212 . 0.959 no
C21 . H211 . 0.959 no
O1 . Sn1 . 2.095(3) yes
O1 . Nb1 . 2.131(3) yes
O2 . Sn1 . 2.115(3) yes
O2 . Nb1 . 2.116(3) yes
O3 . Nb1 . 1.814(3) yes
O4 . Nb1 . 1.832(3) yes
O5 . Nb1 . 1.843(3) yes
O6 . Sn2 2_677 2.108(3) yes
O6 . Sn2 . 2.096(3) yes
O7 . Sn2 . 2.164(3) yes
O7 . H7 . 0.815 no
Sn1 . Cl4 . 2.5269(10) yes
Sn1 . Cl1 . 2.3704(11) yes
Sn1 . Cl2 . 2.3644(11) yes
Sn1 . Cl3 . 2.3665(11) yes
Nb1 . Cl4 . 2.7144(10) yes
Sn2 . Cl6 . 2.3477(12) yes
Sn2 . Cl5 . 2.3614(13) yes
Sn2 . Cl7 . 2.3999(12) 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 . C3 . 112.6(4) yes
C2 . C1 . O1 . 109.4(3) yes
C3 . C1 . O1 . 109.9(3) yes
C2 . C1 . H11 . 109.6 no
C3 . C1 . H11 . 107.6 no
O1 . C1 . H11 . 107.6 no
C1 . C2 . H23 . 109.3 no
C1 . C2 . H22 . 110.3 no
H23 . C2 . H22 . 107.6 no
C1 . C2 . H21 . 110.9 no
H23 . C2 . H21 . 109.2 no
H22 . C2 . H21 . 109.4 no
C1 . C3 . H33 . 108.6 no
C1 . C3 . H32 . 109.8 no
H33 . C3 . H32 . 109.5 no
C1 . C3 . H31 . 109.7 no
H33 . C3 . H31 . 109.5 no
H32 . C3 . H31 . 109.7 no
C5 . C4 . C6 . 112.3(4) yes
C5 . C4 . O2 . 110.7(4) yes
C6 . C4 . O2 . 109.4(3) yes
C5 . C4 . H41 . 109.8 no
C6 . C4 . H41 . 108.0 no
O2 . C4 . H41 . 106.4 no
C4 . C5 . H52 . 110.5 no
C4 . C5 . H53 . 109.1 no
H52 . C5 . H53 . 108.1 no
C4 . C5 . H51 . 110.8 no
H52 . C5 . H51 . 109.7 no
H53 . C5 . H51 . 108.6 no
C4 . C6 . H62 . 109.8 no
C4 . C6 . H63 . 110.0 no
H62 . C6 . H63 . 108.6 no
C4 . C6 . H61 . 110.0 no
H62 . C6 . H61 . 109.1 no
H63 . C6 . H61 . 109.3 no
C8 . C7 . C9 . 112.9(4) yes
C8 . C7 . O3 . 109.1(4) yes
C9 . C7 . O3 . 109.3(4) yes
C8 . C7 . H71 . 109.4 no
C9 . C7 . H71 . 108.9 no
O3 . C7 . H71 . 107.1 no
C7 . C8 . H82 . 109.1 no
C7 . C8 . H81 . 109.4 no
H82 . C8 . H81 . 110.1 no
C7 . C8 . H83 . 108.9 no
H82 . C8 . H83 . 109.7 no
H81 . C8 . H83 . 109.7 no
C7 . C9 . H92 . 108.3 no
C7 . C9 . H91 . 109.4 no
H92 . C9 . H91 . 110.0 no
C7 . C9 . H93 . 108.6 no
H92 . C9 . H93 . 110.2 no
H91 . C9 . H93 . 110.3 no
C11 . C10 . C12 . 113.2(5) yes
C11 . C10 . O4 . 108.5(4) yes
C12 . C10 . O4 . 109.5(4) yes
C11 . C10 . H101 . 109.4 no
C12 . C10 . H101 . 109.1 no
O4 . C10 . H101 . 106.9 no
C10 . C11 . H113 . 109.3 no
C10 . C11 . H111 . 110.0 no
H113 . C11 . H111 . 109.5 no
C10 . C11 . H112 . 109.8 no
H113 . C11 . H112 . 109.1 no
H111 . C11 . H112 . 109.1 no
C10 . C12 . H123 . 108.7 no
C10 . C12 . H121 . 108.9 no
H123 . C12 . H121 . 110.0 no
C10 . C12 . H122 . 110.2 no
H123 . C12 . H122 . 109.5 no
H121 . C12 . H122 . 109.6 no
C14 . C13 . C15 . 113.0(5) yes
C14 . C13 . O5 . 109.4(4) yes
C15 . C13 . O5 . 108.2(4) yes
C14 . C13 . H131 . 107.5 no
C15 . C13 . H131 . 110.2 no
O5 . C13 . H131 . 108.5 no
C13 . C14 . H141 . 109.8 no
C13 . C14 . H143 . 108.1 no
H141 . C14 . H143 . 109.6 no
C13 . C14 . H142 . 109.8 no
H141 . C14 . H142 . 109.8 no
H143 . C14 . H142 . 109.7 no
C13 . C15 . H151 . 110.0 no
C13 . C15 . H153 . 109.2 no
H151 . C15 . H153 . 110.2 no
C13 . C15 . H152 . 108.6 no
H151 . C15 . H152 . 109.5 no
H153 . C15 . H152 . 109.2 no
C17 . C16 . C18 . 121.4(6) yes
C17 . C16 . O6 . 113.4(5) yes
C18 . C16 . O6 . 111.5(5) yes
C17 . C16 . H161 . 103.1 no
C18 . C16 . H161 . 101.8 no
O6 . C16 . H161 . 102.7 no
C16 . C17 . H173 . 109.9 no
C16 . C17 . H172 . 109.2 no
H173 . C17 . H172 . 109.8 no
C16 . C17 . H171 . 107.9 no
H173 . C17 . H171 . 109.6 no
H172 . C17 . H171 . 110.5 no
C16 . C18 . H183 . 108.6 no
C16 . C18 . H182 . 112.1 no
H183 . C18 . H182 . 109.7 no
C16 . C18 . H181 . 108.7 no
H183 . C18 . H181 . 108.8 no
H182 . C18 . H181 . 108.9 no
C20 . C19 . C21 . 112.3(6) yes
C20 . C19 . O7 . 109.6(5) yes
C21 . C19 . O7 . 108.9(5) yes
C20 . C19 . H191 . 108.7 no
C21 . C19 . H191 . 109.5 no
O7 . C19 . H191 . 107.8 no
C19 . C20 . H203 . 109.8 no
C19 . C20 . H202 . 109.1 no
H203 . C20 . H202 . 109.6 no
C19 . C20 . H201 . 109.9 no
H203 . C20 . H201 . 109.3 no
H202 . C20 . H201 . 109.1 no
C19 . C21 . H213 . 109.8 no
C19 . C21 . H212 . 109.2 no
H213 . C21 . H212 . 109.1 no
C19 . C21 . H211 . 110.3 no
H213 . C21 . H211 . 109.4 no
H212 . C21 . H211 . 109.0 no
C1 . O1 . Sn1 . 122.3(2) yes
C1 . O1 . Nb1 . 133.9(2) yes
Sn1 . O1 . Nb1 . 100.54(11) yes
C4 . O2 . Sn1 . 126.0(2) yes
C4 . O2 . Nb1 . 133.2(2) yes
Sn1 . O2 . Nb1 . 100.38(11) yes
C7 . O3 . Nb1 . 159.2(3) yes
C10 . O4 . Nb1 . 166.3(3) yes
C13 . O5 . Nb1 . 164.5(3) yes
C16 . O6 . Sn2 2_677 123.5(3) yes
C16 . O6 . Sn2 . 129.1(3) yes
Sn2 2_677 O6 . Sn2 . 107.43(12) yes
C19 . O7 . Sn2 . 132.5(3) yes
C19 . O7 . H7 . 110.9 no
Sn2 . O7 . H7 . 115.3 no
O2 . Sn1 . O1 . 71.67(10) yes
O2 . Sn1 . Cl4 . 76.63(8) yes
O1 . Sn1 . Cl4 . 76.54(8) yes
O2 . Sn1 . Cl1 . 92.70(8) yes
O1 . Sn1 . Cl1 . 96.16(8) yes
Cl4 . Sn1 . Cl1 . 168.48(4) yes
O2 . Sn1 . Cl2 . 162.67(8) yes
O1 . Sn1 . Cl2 . 92.60(8) yes
Cl4 . Sn1 . Cl2 . 92.97(4) yes
Cl1 . Sn1 . Cl2 . 96.29(4) yes
O2 . Sn1 . Cl3 . 96.14(8) yes
O1 . Sn1 . Cl3 . 164.25(8) yes
Cl4 . Sn1 . Cl3 . 91.17(4) yes
Cl1 . Sn1 . Cl3 . 94.32(4) yes
Cl2 . Sn1 . Cl3 . 97.91(4) yes
O1 . Nb1 . O2 . 70.94(10) yes
O1 . Nb1 . O5 . 157.16(12) yes
O2 . Nb1 . O5 . 91.82(12) yes
O1 . Nb1 . O4 . 92.31(12) yes
O2 . Nb1 . O4 . 156.67(12) yes
O5 . Nb1 . O4 . 99.23(13) yes
O1 . Nb1 . O3 . 96.76(11) yes
O2 . Nb1 . O3 . 97.84(12) yes
O5 . Nb1 . O3 . 100.46(13) yes
O4 . Nb1 . O3 . 100.25(13) yes
O1 . Nb1 . Cl4 . 71.87(7) yes
O2 . Nb1 . Cl4 . 72.47(8) yes
O5 . Nb1 . Cl4 . 88.99(9) yes
O4 . Nb1 . Cl4 . 87.15(9) yes
O3 . Nb1 . Cl4 . 166.82(9) yes
Nb1 . Cl4 . Sn1 . 76.56(3) yes
O7 . Sn2 . O6 2_677 82.91(12) yes
O7 . Sn2 . O6 . 81.22(13) yes
O6 2_677 Sn2 . O6 . 72.57(12) yes
O7 . Sn2 . Cl6 . 89.70(10) yes
O6 2_677 Sn2 . Cl6 . 95.80(9) yes
O6 . Sn2 . Cl6 . 165.96(10) yes
O7 . Sn2 . Cl5 . 89.15(10) yes
O6 2_677 Sn2 . Cl5 . 168.84(9) yes
O6 . Sn2 . Cl5 . 98.53(9) yes
Cl6 . Sn2 . Cl5 . 91.98(5) yes
O7 . Sn2 . Cl7 . 171.70(9) yes
O6 2_677 Sn2 . Cl7 . 91.35(9) yes
O6 . Sn2 . Cl7 . 91.36(9) yes
Cl6 . Sn2 . Cl7 . 96.88(5) yes
Cl5 . Sn2 . Cl7 . 95.66(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
C3 . H32 . O3 . 124 0.96 2.58 3.218(9) yes
O7 . H7 . Cl7 2_677 163 0.815 2.313 3.101(3) yes
####################################################################### 
# 
# 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_SMR214
_database_code_depnum_ccdc_archive 'CCDC 759071'
_audit_update_record             
;
2009-12-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'SMR214.cif'

_audit_creation_date             09-12-01
_audit_creation_method           CRYSTALS_ver_12.87

_oxford_structure_analysis_title 'smr214 in C 1 c 1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   17.5030(10)
_cell_length_b                   11.6510(10)
_cell_length_c                   19.801(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.935(7)
_cell_angle_gamma                90
_cell_volume                     4032.7(6)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 c 1 '
_symmetry_space_group_name_Hall  'C -2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
x,-y,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'
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'
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'
Nb -2.0727 0.6215 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957
3.7559 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C75 H75 Cl12.50 Nb5 O25 Sn5
# Dc = 2.37 Fooo = 2208.00 Mu = 26.98 M = 1438.77
# Found Formula = C40 H104 Cl12 Nb4 O24 Sn4
# Dc = 1.85 FOOO = 2208.00 Mu = 22.22 M = 1120.53

_chemical_formula_sum            'C20 H52 Cl6 Nb2 O12 Sn2'
_chemical_formula_moiety         'C20 H52 Cl6 Nb2 O12 Sn2'
_chemical_compound_source        ?
_chemical_formula_weight         1120.56


_cell_measurement_reflns_used    8760
_cell_measurement_theta_min      3.4886
_cell_measurement_theta_max      29.6553
_cell_measurement_temperature    150

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.069
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_max          0.205

_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             2208
_exptl_absorpt_coefficient_mu    2.222

# Sheldrick geometric approximatio 0.81 0.86
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_T_max  0.86
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            17791
_reflns_number_total             8759
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 8759
# Number of reflections with Friedels Law is 0
# Theoretical number of reflections is about 5732


_diffrn_reflns_theta_min         3.497
_diffrn_reflns_theta_max         29.717
_diffrn_measured_fraction_theta_max 0.866

_diffrn_reflns_theta_full        26.448
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -18
_reflns_limit_h_max              23
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              -27
_reflns_limit_l_max              26

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -1.56
_refine_diff_density_max         1.75


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


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         8759
_refine_ls_number_restraints     48
_refine_ls_number_parameters     399
_oxford_refine_ls_R_factor_ref   0.0564
_refine_ls_wR_factor_ref         0.1107
_refine_ls_goodness_of_fit_ref   0.9620
_refine_ls_shift/su_max          0.0010479


# The values computed from all data
_oxford_reflns_number_all        8759
_refine_ls_R_factor_all          0.0564
_refine_ls_wR_factor_all         0.1107

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7267
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_gt          0.1042

_refine_ls_abs_structure_Flack   0.61(3)
_refine_ls_abs_structure_details 'Flack (1983), 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    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method= Modified Sheldrick
w=1/[σ²(F²) + ( 0.05P)² +50.09P]
,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 atomsattached to an atom.

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
C1 C 0.7294(5) 0.5544(8) 0.6068(6) 0.0359 1.0000 Uani . . . . . . .
C2 C 0.7470(7) 0.4293(9) 0.6027(8) 0.0521 1.0000 Uani . . . . . . .
C3 C 0.4340(5) 0.5880(8) 0.5409(6) 0.0369 1.0000 Uani . U . . . . .
C4 C 0.3863(6) 0.6967(9) 0.5403(7) 0.0511 1.0000 Uani . U . . . . .
C5 C 0.7735(6) 0.9392(7) 0.6390(6) 0.0336 1.0000 Uani . . . . . . .
C6 C 0.8200(6) 0.8311(8) 0.6449(6) 0.0419 1.0000 Uani . . . . . . .
C7 C 0.4797(5) 0.9732(8) 0.5766(5) 0.0315 1.0000 Uani . U . . . . .
C8 C 0.4605(8) 1.0994(11) 0.5838(7) 0.0582 1.0000 Uani . U . . . . .
C9 C 0.6275(8) 1.1540(11) 0.7556(7) 0.0632 1.0000 Uani D U . . . . .
C10 C 0.7040(9) 1.2109(15) 0.7757(9) 0.0957 1.0000 Uani D U . . . . .
C11 C 0.4463(8) 0.9136(13) 0.7588(9) 0.0868 1.0000 Uani D . . . . . .
C12 C 0.3952(8) 1.0195(14) 0.7537(8) 0.0887 1.0000 Uani D . . . . . .
C13 C 0.7260(9) 0.8948(10) 0.8150(7) 0.0646 1.0000 Uani D . . . . . .
C14 C 0.7427(12) 0.7811(12) 0.8509(9) 0.0978 1.0000 Uani D . . . . . .
C15 C 0.5639(8) 0.3662(9) 0.4277(7) 0.0613 1.0000 Uani . . . . . . .
C16 C 0.4774(11) 0.3285(14) 0.4211(9) 0.1107 1.0000 Uani . . . . . . .
C17 C 0.7420(6) 0.5279(12) 0.4191(7) 0.0636 1.0000 Uani D U . . . . .
C18 C 0.8208(8) 0.5823(14) 0.4288(8) 0.0873 1.0000 Uani D U . . . . .
C19 C 0.4925(18) 0.630(2) 0.3567(14) 0.0655 0.5000 Uani . U . 2 2 . .
C20 C 0.4552(17) 0.732(3) 0.3361(18) 0.0712 0.5000 Uani . U . 2 2 . .
C21 C 0.4762(15) 0.708(2) 0.3778(12) 0.0672 0.5000 Uani . U . 2 1 . .
C22 C 0.4589(15) 0.643(3) 0.3190(13) 0.0657 0.5000 Uani . U . 2 1 . .
O1 O 0.5836(4) 0.7459(6) 0.6685(4) 0.0317 1.0000 Uani . . . . . . .
O2 O 0.6206(4) 0.7794(5) 0.5107(3) 0.0303 1.0000 Uani . . . . . . .
O3 O 0.6473(4) 0.5743(5) 0.5884(4) 0.0284 1.0000 Uani . . . . . . .
O4 O 0.5137(4) 0.6137(6) 0.5613(4) 0.0317 1.0000 Uani . . . . . . .
O5 O 0.6943(4) 0.9114(5) 0.6191(4) 0.0267 1.0000 Uani . . . . . . .
O6 O 0.5589(4) 0.9523(5) 0.5923(4) 0.0264 1.0000 Uani . . . . . . .
O7 O 0.6349(5) 1.0851(5) 0.6979(4) 0.0368 1.0000 Uani . . . . . . .
O8 O 0.5161(5) 0.9341(6) 0.7285(4) 0.0381 1.0000 Uani . . . . . . .
O9 O 0.6755(4) 0.8782(6) 0.7598(4) 0.0384 1.0000 Uani . . . . . . .
O10 O 0.5757(5) 0.4393(5) 0.4850(4) 0.0402 1.0000 Uani . . . . . . .
O11 O 0.6907(5) 0.5923(6) 0.4526(4) 0.0378 1.0000 Uani . . . . . . .
O12 O 0.5332(5) 0.6437(6) 0.4213(5) 0.0459 1.0000 Uani . . . . . . .
Sn2 Sn 0.64533(10) 0.95042(5) 0.52321(9) 0.0275 1.0000 Uani . . . . . . .
Cl5 Cl 0.76128(18) 0.9256(2) 0.46844(16) 0.0391 1.0000 Uani . . . . . . .
Cl6 Cl 0.66918(17) 1.15156(19) 0.54588(16) 0.0375 1.0000 Uani . . . . . . .
Cl4 Cl 0.56318(19) 0.9942(2) 0.42724(16) 0.0452 1.0000 Uani . . . . . . .
Nb2 Nb 0.60195(10) 0.63214(6) 0.49417(9) 0.0265 1.0000 Uani . . . . . . .
Sn1 Sn 0.56134(10) 0.57465(5) 0.65773(9) 0.0289 1.0000 Uani . . . . . . .
Cl3 Cl 0.53816(18) 0.3737(2) 0.63477(17) 0.0418 1.0000 Uani . . . . . . .
Cl2 Cl 0.64357(19) 0.5328(2) 0.75356(16) 0.0458 1.0000 Uani . . . . . . .
Cl1 Cl 0.44513(19) 0.5974(2) 0.71263(18) 0.0487 1.0000 Uani . . . . . . .
Nb1 Nb 0.60527(10) 0.89271(6) 0.68681(9) 0.0249 1.0000 Uani . . . . . . .
H11 H 0.7403 0.5809 0.6526 0.0431 1.0000 Uiso R . . . . . .
H12 H 0.7603 0.5975 0.5756 0.0428 1.0000 Uiso R . . . . . .
H22 H 0.8004 0.4176 0.6138 0.0779 1.0000 Uiso R . . . . . .
H21 H 0.7176 0.3872 0.6337 0.0779 1.0000 Uiso R . . . . . .
H23 H 0.7357 0.4017 0.5575 0.0779 1.0000 Uiso R . . . . . .
H32 H 0.4144 0.5332 0.5724 0.0439 1.0000 Uiso R . . . . . .
H31 H 0.4313 0.5540 0.4964 0.0439 1.0000 Uiso R . . . . . .
H41 H 0.3343 0.6782 0.5265 0.0760 1.0000 Uiso R . . . . . .
H43 H 0.3877 0.7292 0.5851 0.0760 1.0000 Uiso R . . . . . .
H42 H 0.4060 0.7510 0.5092 0.0758 1.0000 Uiso R . . . . . .
H51 H 0.7756 0.9799 0.6818 0.0399 1.0000 Uiso R . . . . . .
H52 H 0.7936 0.9887 0.6044 0.0401 1.0000 Uiso R . . . . . .
H62 H 0.8718 0.8498 0.6594 0.0629 1.0000 Uiso R . . . . . .
H61 H 0.7984 0.7807 0.6769 0.0628 1.0000 Uiso R . . . . . .
H63 H 0.8195 0.7937 0.6015 0.0629 1.0000 Uiso R . . . . . .
H72 H 0.4505 0.9284 0.6077 0.0379 1.0000 Uiso R . . . . . .
H71 H 0.4673 0.9492 0.5306 0.0380 1.0000 Uiso R . . . . . .
H81 H 0.4063 1.1094 0.5772 0.0880 1.0000 Uiso R . . . . . .
H83 H 0.4765 1.1249 0.6285 0.0878 1.0000 Uiso R . . . . . .
H82 H 0.4858 1.1433 0.5506 0.0879 1.0000 Uiso R . . . . . .
H91 H 0.6119 1.1063 0.7927 0.0760 1.0000 Uiso R . . . . . .
H92 H 0.5891 1.2123 0.7455 0.0761 1.0000 Uiso R . . . . . .
H103 H 0.6937 1.2745 0.8049 0.1420 1.0000 Uiso R . . . . . .
H102 H 0.7373 1.1572 0.7992 0.1421 1.0000 Uiso R . . . . . .
H101 H 0.7278 1.2374 0.7357 0.1420 1.0000 Uiso R . . . . . .
H112 H 0.4562 0.8943 0.8062 0.1070 1.0000 Uiso R . . . . . .
H111 H 0.4190 0.8504 0.7364 0.1072 1.0000 Uiso R . . . . . .
H121 H 0.3499 1.0035 0.7773 0.1370 1.0000 Uiso R . . . . . .
H122 H 0.4212 1.0848 0.7737 0.1370 1.0000 Uiso R . . . . . .
H123 H 0.3818 1.0353 0.7070 0.1370 1.0000 Uiso R . . . . . .
H132 H 0.7032 0.9472 0.8467 0.0792 1.0000 Uiso R . . . . . .
H131 H 0.7743 0.9268 0.8008 0.0790 1.0000 Uiso R . . . . . .
H143 H 0.7757 0.7953 0.8903 0.1430 1.0000 Uiso R . . . . . .
H142 H 0.6954 0.7477 0.8641 0.1430 1.0000 Uiso R . . . . . .
H141 H 0.7674 0.7304 0.8205 0.1429 1.0000 Uiso R . . . . . .
H151 H 0.5955 0.2985 0.4326 0.0740 1.0000 Uiso R . . . . . .
H152 H 0.5767 0.4074 0.3874 0.0741 1.0000 Uiso R . . . . . .
H162 H 0.4683 0.2804 0.3821 0.1521 1.0000 Uiso R . . . . . .
H161 H 0.4645 0.2868 0.4610 0.1520 1.0000 Uiso R . . . . . .
H163 H 0.4456 0.3959 0.4166 0.1520 1.0000 Uiso R . . . . . .
H172 H 0.7429 0.4494 0.4362 0.0759 1.0000 Uiso R . . . . . .
H171 H 0.7273 0.5273 0.3709 0.0762 1.0000 Uiso R . . . . . .
H181 H 0.8559 0.5308 0.4082 0.1320 1.0000 Uiso R . . . . . .
H183 H 0.8339 0.5889 0.4767 0.1320 1.0000 Uiso R . . . . . .
H182 H 0.8213 0.6577 0.4080 0.1316 1.0000 Uiso R . . . . . .
H191 H 0.5282 0.6073 0.3232 0.0819 0.5000 Uiso R . . 2 2 . .
H192 H 0.4538 0.5710 0.3611 0.0820 0.5000 Uiso R . . 2 2 . .
H202 H 0.4148 0.7129 0.3033 0.1090 0.5000 Uiso R . . 2 2 . .
H201 H 0.4917 0.7810 0.3161 0.1091 0.5000 Uiso R . . 2 2 . .
H203 H 0.4342 0.7695 0.3742 0.1090 0.5000 Uiso R . . 2 2 . .
H212 H 0.4973 0.7813 0.3656 0.0830 0.5000 Uiso R . . 2 1 . .
H211 H 0.4300 0.7198 0.4021 0.0830 0.5000 Uiso R . . 2 1 . .
H221 H 0.4237 0.6849 0.2891 0.1029 0.5000 Uiso R . . 2 1 . .
H223 H 0.5056 0.6270 0.2963 0.1030 0.5000 Uiso R . . 2 1 . .
H222 H 0.4353 0.5712 0.3318 0.1029 0.5000 Uiso R . . 2 1 . .
H7 H 0.6479 1.1126 0.6621 0.0548 1.0000 Uiso R . . . . . .
H10 H 0.5696 0.4000 0.5186 0.0607 1.0000 Uiso R . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.6414(10)

loop_
_oxford_twin_element_scale_factors
0.38(4)
0.62(4)
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 . 1.494(14) yes
C1 . O3 . 1.483(12) yes
C1 . H11 . 0.968 no
C1 . H12 . 0.979 no
C2 . H22 . 0.959 no
C2 . H21 . 0.957 no
C2 . H23 . 0.962 no
C3 . C4 . 1.517(14) yes
C3 . O4 . 1.464(12) yes
C3 . H32 . 0.967 no
C3 . H31 . 0.966 no
C4 . H41 . 0.961 no
C4 . H43 . 0.965 no
C4 . H42 . 0.960 no
C5 . C6 . 1.500(13) yes
C5 . O5 . 1.458(12) yes
C5 . H51 . 0.972 no
C5 . H52 . 0.974 no
C6 . H62 . 0.963 no
C6 . H61 . 0.956 no
C6 . H63 . 0.962 no
C7 . C8 . 1.517(14) yes
C7 . O6 . 1.427(12) yes
C7 . H72 . 0.972 no
C7 . H71 . 0.966 no
C8 . H81 . 0.958 no
C8 . H83 . 0.963 no
C8 . H82 . 0.959 no
C9 . C10 . 1.528(9) yes
C9 . O7 . 1.407(14) yes
C9 . H91 . 0.973 no
C9 . H92 . 0.969 no
C10 . H103 . 0.962 no
C10 . H102 . 0.959 no
C10 . H101 . 0.964 no
C11 . C12 . 1.524(9) yes
C11 . O8 . 1.408(15) yes
C11 . H112 . 0.973 no
C11 . H111 . 0.972 no
C12 . H121 . 0.959 no
C12 . H122 . 0.961 no
C12 . H123 . 0.961 no
C13 . C14 . 1.525(9) yes
C13 . O9 . 1.385(16) yes
C13 . H132 . 0.976 no
C13 . H131 . 0.979 no
C14 . H143 . 0.961 no
C14 . H142 . 0.962 no
C14 . H141 . 0.962 no
C15 . C16 . 1.57(2) yes
C15 . O10 . 1.425(13) yes
C15 . H151 . 0.966 no
C15 . H152 . 0.969 no
C16 . H162 . 0.962 no
C16 . H161 . 0.963 no
C16 . H163 . 0.964 no
C17 . C18 . 1.522(9) yes
C17 . O11 . 1.367(13) yes
C17 . H172 . 0.975 no
C17 . H171 . 0.974 no
C18 . H181 . 0.963 no
C18 . H183 . 0.967 no
C18 . H182 . 0.970 no
C19 . C20 . 1.40(4) yes
C19 . O12 . 1.44(3) yes
C19 . H191 . 0.971 no
C19 . H192 . 0.973 no
C20 . H202 . 0.961 no
C20 . H201 . 0.960 no
C20 . H203 . 0.962 no
C21 . C22 . 1.41(3) yes
C21 . O12 . 1.48(2) yes
C21 . H212 . 0.970 no
C21 . H211 . 0.973 no
C22 . H221 . 0.966 no
C22 . H223 . 0.970 no
C22 . H222 . 0.969 no
O1 . Sn1 . 2.041(7) yes
O1 . Nb1 . 1.786(7) yes
O2 . Sn2 . 2.051(6) yes
O2 . Nb2 . 1.774(6) yes
O3 . Nb2 . 2.101(8) yes
O3 . Sn1 . 2.088(7) yes
O4 . Nb2 . 2.100(7) yes
O4 . Sn1 . 2.093(7) yes
O5 . Sn2 . 2.093(7) yes
O5 . Nb1 . 2.119(6) yes
O6 . Sn2 . 2.091(7) yes
O6 . Nb1 . 2.117(7) yes
O7 . Nb1 . 2.309(6) yes
O7 . H7 . 0.820 no
O8 . Nb1 . 1.866(8) yes
O9 . Nb1 . 1.856(8) yes
O10 . Nb2 . 2.299(6) yes
O10 . H10 . 0.818 no
O11 . Nb2 . 1.854(8) yes
O12 . Nb2 . 1.836(8) yes
O12 . Nb2 . 1.836(8) yes
Sn2 . Cl5 . 2.367(3) yes
Sn2 . Cl6 . 2.418(2) yes
Sn2 . Cl4 . 2.379(3) yes
Sn1 . Cl3 . 2.415(2) yes
Sn1 . Cl2 . 2.373(3) yes
Sn1 . Cl1 . 2.370(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 . O3 . 109.8(8) yes
C2 . C1 . H11 . 109.3 no
O3 . C1 . H11 . 108.7 no
C2 . C1 . H12 . 110.2 no
O3 . C1 . H12 . 108.9 no
H11 . C1 . H12 . 109.9 no
C1 . C2 . H22 . 109.1 no
C1 . C2 . H21 . 110.2 no
H22 . C2 . H21 . 109.2 no
C1 . C2 . H23 . 110.1 no
H22 . C2 . H23 . 108.6 no
H21 . C2 . H23 . 109.6 no
C4 . C3 . O4 . 110.3(8) yes
C4 . C3 . H32 . 110.0 no
O4 . C3 . H32 . 108.8 no
C4 . C3 . H31 . 109.4 no
O4 . C3 . H31 . 109.8 no
H32 . C3 . H31 . 108.4 no
C3 . C4 . H41 . 109.2 no
C3 . C4 . H43 . 109.5 no
H41 . C4 . H43 . 109.1 no
C3 . C4 . H42 . 109.9 no
H41 . C4 . H42 . 109.3 no
H43 . C4 . H42 . 109.8 no
C6 . C5 . O5 . 109.8(7) yes
C6 . C5 . H51 . 110.2 no
O5 . C5 . H51 . 109.6 no
C6 . C5 . H52 . 109.8 no
O5 . C5 . H52 . 108.3 no
H51 . C5 . H52 . 109.0 no
C5 . C6 . H62 . 109.4 no
C5 . C6 . H61 . 109.7 no
H62 . C6 . H61 . 109.8 no
C5 . C6 . H63 . 109.3 no
H62 . C6 . H63 . 109.5 no
H61 . C6 . H63 . 109.2 no
C8 . C7 . O6 . 111.2(8) yes
C8 . C7 . H72 . 109.5 no
O6 . C7 . H72 . 107.9 no
C8 . C7 . H71 . 109.2 no
O6 . C7 . H71 . 109.0 no
H72 . C7 . H71 . 110.0 no
C7 . C8 . H81 . 109.2 no
C7 . C8 . H83 . 109.3 no
H81 . C8 . H83 . 109.1 no
C7 . C8 . H82 . 109.8 no
H81 . C8 . H82 . 109.4 no
H83 . C8 . H82 . 110.0 no
C10 . C9 . O7 . 110.1(12) yes
C10 . C9 . H91 . 109.1 no
O7 . C9 . H91 . 109.2 no
C10 . C9 . H92 . 109.9 no
O7 . C9 . H92 . 108.9 no
H91 . C9 . H92 . 109.6 no
C9 . C10 . H103 . 107.6 no
C9 . C10 . H102 . 110.2 no
H103 . C10 . H102 . 109.7 no
C9 . C10 . H101 . 109.5 no
H103 . C10 . H101 . 110.4 no
H102 . C10 . H101 . 109.3 no
C12 . C11 . O8 . 110.7(12) yes
C12 . C11 . H112 . 108.9 no
O8 . C11 . H112 . 109.6 no
C12 . C11 . H111 . 108.1 no
O8 . C11 . H111 . 110.6 no
H112 . C11 . H111 . 108.8 no
C11 . C12 . H121 . 107.9 no
C11 . C12 . H122 . 110.5 no
H121 . C12 . H122 . 109.8 no
C11 . C12 . H123 . 109.4 no
H121 . C12 . H123 . 109.8 no
H122 . C12 . H123 . 109.4 no
C14 . C13 . O9 . 110.3(11) yes
C14 . C13 . H132 . 108.7 no
O9 . C13 . H132 . 109.2 no
C14 . C13 . H131 . 108.5 no
O9 . C13 . H131 . 110.6 no
H132 . C13 . H131 . 109.6 no
C13 . C14 . H143 . 108.7 no
C13 . C14 . H142 . 109.3 no
H143 . C14 . H142 . 109.9 no
C13 . C14 . H141 . 108.8 no
H143 . C14 . H141 . 110.1 no
H142 . C14 . H141 . 110.0 no
C16 . C15 . O10 . 109.5(12) yes
C16 . C15 . H151 . 109.0 no
O10 . C15 . H151 . 110.4 no
C16 . C15 . H152 . 109.4 no
O10 . C15 . H152 . 109.3 no
H151 . C15 . H152 . 109.4 no
C15 . C16 . H162 . 110.3 no
C15 . C16 . H161 . 109.7 no
H162 . C16 . H161 . 109.2 no
C15 . C16 . H163 . 109.2 no
H162 . C16 . H163 . 109.3 no
H161 . C16 . H163 . 109.2 no
C18 . C17 . O11 . 108.9(11) yes
C18 . C17 . H172 . 110.4 no
O11 . C17 . H172 . 110.2 no
C18 . C17 . H171 . 108.6 no
O11 . C17 . H171 . 109.4 no
H172 . C17 . H171 . 109.4 no
C17 . C18 . H181 . 106.3 no
C17 . C18 . H183 . 109.0 no
H181 . C18 . H183 . 109.9 no
C17 . C18 . H182 . 110.5 no
H181 . C18 . H182 . 111.5 no
H183 . C18 . H182 . 109.7 no
C20 . C19 . O12 . 112(2) yes
C20 . C19 . H191 . 109.8 no
O12 . C19 . H191 . 109.2 no
C20 . C19 . H192 . 108.0 no
O12 . C19 . H192 . 108.2 no
H191 . C19 . H192 . 110.0 no
C19 . C20 . H202 . 108.7 no
C19 . C20 . H201 . 108.4 no
H202 . C20 . H201 . 109.7 no
C19 . C20 . H203 . 110.5 no
H202 . C20 . H203 . 109.7 no
H201 . C20 . H203 . 109.8 no
C22 . C21 . O12 . 109(2) yes
C22 . C21 . H212 . 109.7 no
O12 . C21 . H212 . 109.7 no
C22 . C21 . H211 . 109.6 no
O12 . C21 . H211 . 109.8 no
H212 . C21 . H211 . 109.4 no
C21 . C22 . H221 . 109.6 no
C21 . C22 . H223 . 109.4 no
H221 . C22 . H223 . 109.8 no
C21 . C22 . H222 . 108.7 no
H221 . C22 . H222 . 109.4 no
H223 . C22 . H222 . 110.0 no
Sn1 . O1 . Nb1 . 174.2(4) yes
Sn2 . O2 . Nb2 . 175.9(4) yes
C1 . O3 . Nb2 . 125.8(6) yes
C1 . O3 . Sn1 . 124.1(7) yes
Nb2 . O3 . Sn1 . 109.4(3) yes
C3 . O4 . Nb2 . 124.6(7) yes
C3 . O4 . Sn1 . 122.5(6) yes
Nb2 . O4 . Sn1 . 109.2(3) yes
C5 . O5 . Sn2 . 122.4(6) yes
C5 . O5 . Nb1 . 124.9(6) yes
Sn2 . O5 . Nb1 . 108.4(3) yes
C7 . O6 . Sn2 . 125.9(6) yes
C7 . O6 . Nb1 . 125.0(6) yes
Sn2 . O6 . Nb1 . 108.5(3) yes
C9 . O7 . Nb1 . 127.0(8) yes
C9 . O7 . H7 . 121.3 no
Nb1 . O7 . H7 . 111.6 no
C11 . O8 . Nb1 . 155.2(8) yes
C13 . O9 . Nb1 . 166.7(7) yes
C15 . O10 . Nb2 . 131.9(7) yes
C15 . O10 . H10 . 107.0 no
Nb2 . O10 . H10 . 121.1 no
C17 . O11 . Nb2 . 159.8(8) yes
C21 . O12 . Nb2 . 152.4(11) yes
C19 . O12 . Nb2 . 164.7(13) yes
O5 . Sn2 . O6 . 71.6(3) yes
O5 . Sn2 . O2 . 88.4(2) yes
O6 . Sn2 . O2 . 86.2(2) yes
O5 . Sn2 . Cl5 . 93.89(18) yes
O6 . Sn2 . Cl5 . 165.2(2) yes
O2 . Sn2 . Cl5 . 90.4(2) yes
O5 . Sn2 . Cl6 . 89.04(17) yes
O6 . Sn2 . Cl6 . 89.55(16) yes
O2 . Sn2 . Cl6 . 175.6(2) yes
Cl5 . Sn2 . Cl6 . 93.42(9) yes
O5 . Sn2 . Cl4 . 166.93(19) yes
O6 . Sn2 . Cl4 . 95.3(2) yes
O2 . Sn2 . Cl4 . 89.80(19) yes
Cl5 . Sn2 . Cl4 . 99.07(10) yes
Cl6 . Sn2 . Cl4 . 91.84(9) yes
O10 . Nb2 . O3 . 79.7(3) yes
O10 . Nb2 . O4 . 78.4(3) yes
O3 . Nb2 . O4 . 70.2(3) yes
O10 . Nb2 . O11 . 83.6(3) yes
O3 . Nb2 . O11 . 91.6(3) yes
O4 . Nb2 . O11 . 156.3(3) yes
O10 . Nb2 . O12 . 83.7(3) yes
O3 . Nb2 . O12 . 157.5(3) yes
O4 . Nb2 . O12 . 91.8(3) yes
O11 . Nb2 . O12 . 101.5(4) yes
O10 . Nb2 . O2 . 173.8(3) yes
O3 . Nb2 . O2 . 95.1(3) yes
O4 . Nb2 . O2 . 96.7(3) yes
O11 . Nb2 . O2 . 100.0(3) yes
O12 . Nb2 . O2 . 100.4(3) yes
O4 . Sn1 . O3 . 70.6(3) yes
O4 . Sn1 . O1 . 87.0(3) yes
O3 . Sn1 . O1 . 86.0(3) yes
O4 . Sn1 . Cl3 . 89.08(19) yes
O3 . Sn1 . Cl3 . 89.65(17) yes
O1 . Sn1 . Cl3 . 174.9(2) yes
O4 . Sn1 . Cl2 . 166.1(2) yes
O3 . Sn1 . Cl2 . 95.6(2) yes
O1 . Sn1 . Cl2 . 90.7(2) yes
Cl3 . Sn1 . Cl2 . 92.33(10) yes
O4 . Sn1 . Cl1 . 94.8(2) yes
O3 . Sn1 . Cl1 . 165.0(2) yes
O1 . Sn1 . Cl1 . 90.4(2) yes
Cl3 . Sn1 . Cl1 . 93.14(9) yes
Cl2 . Sn1 . Cl1 . 98.97(12) yes
O7 . Nb1 . O5 . 78.0(3) yes
O7 . Nb1 . O6 . 80.8(3) yes
O5 . Nb1 . O6 . 70.6(3) yes
O7 . Nb1 . O8 . 84.0(3) yes
O5 . Nb1 . O8 . 155.9(3) yes
O6 . Nb1 . O8 . 90.9(3) yes
O7 . Nb1 . O9 . 83.0(3) yes
O5 . Nb1 . O9 . 91.3(3) yes
O6 . Nb1 . O9 . 157.8(3) yes
O8 . Nb1 . O9 . 102.4(4) yes
O7 . Nb1 . O1 . 173.7(3) yes
O5 . Nb1 . O1 . 97.2(3) yes
O6 . Nb1 . O1 . 93.8(3) yes
O8 . Nb1 . O1 . 99.4(3) yes
O9 . Nb1 . O1 . 101.3(3) 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
C12 . H122 . C20 3_575 165 0.96 2.53 3.46(2) yes
####################################################################### 
# 
# 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_SMR222
_database_code_depnum_ccdc_archive 'CCDC 759073'
_audit_update_record             
;
2009-12-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'SMR222.cif'

_audit_creation_date             09-11-20
_audit_creation_method           CRYSTALS_ver_12.87

_oxford_structure_analysis_title 'numerical in P 1 21/n 1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   10.5050(10)
_cell_length_b                   14.7630(10)
_cell_length_c                   17.790(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.443(9)
_cell_angle_gamma                90
_cell_volume                     2721.6(4)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ta -0.7052 6.5227 29.2024 1.7733 15.2293 9.3705 14.5135 0.2960 4.7649 63.3644
9.2435 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C16 H42 Cl3 O6 Sn1 Ta1
# Dc = 1.80 Fooo = 1424.00 Mu = 52.54 M = 736.50
# Found Formula = C16 H38 Cl3 O6 Sn1 Ta1
# Dc = 1.79 FOOO = 1424.00 Mu = 52.54 M = 732.47

_chemical_formula_sum            'C16 H38 Cl3 O6 Sn1 Ta1'
_chemical_formula_moiety         'C16 H38 Cl3 O6 Sn1 Ta1'
_chemical_compound_source        ?
_chemical_formula_weight         732.47


_cell_measurement_reflns_used    6079
_cell_measurement_theta_min      3.4709
_cell_measurement_theta_max      29.3466
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.5133
_exptl_crystal_size_mid          0.5002
_exptl_crystal_size_min          0.3231

_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1424


# Sheldrick geometric approximatio 1.00 1.00
_exptl_absorpt_coefficient_mu    5.224
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_T_max  0.268
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            13273
_reflns_number_total             6424
_diffrn_reflns_av_R_equivalents  0.036
# Number of reflections without Friedels Law is 9862
# Number of reflections with Friedels Law is 6424
# Theoretical number of reflections is about 7593


_diffrn_reflns_theta_min         3.476
_diffrn_reflns_theta_max         29.513
_diffrn_measured_fraction_theta_max 0.845

_diffrn_reflns_theta_full        25.972
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -2.27
_refine_diff_density_max         2.56


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


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         6424
_refine_ls_number_restraints     96
_refine_ls_number_parameters     244
_oxford_refine_ls_R_factor_ref   0.0931
_refine_ls_wR_factor_ref         0.1844
_refine_ls_goodness_of_fit_ref   0.9571
_refine_ls_shift/su_max          0.0002675


# The values computed from all data
_oxford_reflns_number_all        6424
_refine_ls_R_factor_all          0.0931
_refine_ls_wR_factor_all         0.1844

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4208
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_gt          0.1394

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
0.503E+04 0.806E+04 0.513E+04 0.225E+04 651.
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
C1 C 0.004(3) 0.2459(17) 0.5383(7) 0.1358 1.0000 Uani D U . . . . .
C2 C 0.099(3) 0.1713(19) 0.5726(15) 0.1485 1.0000 Uani D U . . . . .
C3 C -0.039(3) 0.0596(9) 0.3136(13) 0.1522 1.0000 Uani D U . . . . .
C4 C -0.060(3) 0.065(2) 0.2261(13) 0.1532 1.0000 Uani D U . . . . .
C5 C -0.135(3) 0.397(2) 0.2991(13) 0.1371 1.0000 Uani D U . . . . .
C6 C -0.074(3) 0.4765(19) 0.3377(16) 0.1445 1.0000 Uani . U . . . . .
C7 C -0.095(2) 0.4093(18) 0.2203(13) 0.1343 1.0000 Uani D U . . . . .
C8 C 0.321(2) 0.1045(18) 0.4283(14) 0.1195 1.0000 Uani . U . . . . .
C9 C 0.414(2) 0.1385(17) 0.4946(13) 0.1193 1.0000 Uani . U . . . . .
C10 C 0.380(2) 0.0727(19) 0.3644(14) 0.1260 1.0000 Uani . U . . . . .
C11 C 0.206(2) 0.257(2) 0.2113(14) 0.1344 1.0000 Uani D U . . . . .
C12 C 0.306(3) 0.323(2) 0.2122(16) 0.1460 1.0000 Uani . U . . . . .
C13 C 0.121(3) 0.263(2) 0.1330(14) 0.1449 1.0000 Uani D U . . . . .
C14 C 0.245(2) 0.4319(18) 0.4475(15) 0.1239 1.0000 Uani . U . . . . .
C15 C 0.305(2) 0.4815(18) 0.3925(14) 0.1305 1.0000 Uani . U . . . . .
C16 C 0.348(2) 0.4057(18) 0.5111(14) 0.1297 1.0000 Uani . U . . . . .
Ta1 Ta 0.10063(5) 0.25418(3) 0.36759(3) 0.0437 1.0000 Uani . . . . . . .
Sn1 Sn -0.18635(9) 0.22126(7) 0.38441(6) 0.0548 1.0000 Uani . . . . . . .
O3 O -0.0802(8) 0.3193(6) 0.3364(5) 0.0506 1.0000 Uani . . . . . . .
O1 O -0.0101(8) 0.2358(6) 0.4558(5) 0.0532 1.0000 Uani D . . . . . .
O2 O -0.0446(9) 0.1551(6) 0.3337(5) 0.0594 1.0000 Uani D . . . . . .
Cl2 Cl -0.3470(4) 0.2078(4) 0.2768(3) 0.1082 1.0000 Uani . . . . . . .
Cl3 Cl -0.2422(4) 0.0901(4) 0.4473(3) 0.0953 1.0000 Uani . . . . . . .
Cl1 Cl -0.3005(5) 0.3254(4) 0.4470(4) 0.1154 1.0000 Uani . . . . . . .
O5 O 0.1405(10) 0.2651(9) 0.2713(6) 0.0780 1.0000 Uani . . . . . . .
O4 O 0.2214(8) 0.1681(7) 0.4053(6) 0.0640 1.0000 Uani . . . . . . .
O6 O 0.1837(10) 0.3540(7) 0.4125(7) 0.0768 1.0000 Uani . . . . . . .
H11 H 0.0357 0.3044 0.5536 0.1526 1.0000 Uiso R . . . . . .
H12 H -0.0768 0.2366 0.5547 0.1526 1.0000 Uiso R . . . . . .
H21 H 0.1109 0.1753 0.6266 0.1682 1.0000 Uiso R . . . . . .
H22 H 0.1794 0.1808 0.5558 0.1682 1.0000 Uiso R . . . . . .
H23 H 0.0669 0.1129 0.5570 0.1682 1.0000 Uiso R . . . . . .
H31 H -0.1066 0.0272 0.3310 0.1748 1.0000 Uiso R . . . . . .
H32 H 0.0417 0.0334 0.3346 0.1748 1.0000 Uiso R . . . . . .
H41 H -0.0585 0.0048 0.2074 0.1760 1.0000 Uiso R . . . . . .
H42 H -0.1400 0.0925 0.2065 0.1760 1.0000 Uiso R . . . . . .
H43 H 0.0083 0.0987 0.2101 0.1760 1.0000 Uiso R . . . . . .
H51 H -0.2260 0.3953 0.2953 0.1555 1.0000 Uiso R . . . . . .
H61 H -0.0963 0.4723 0.3873 0.1632 1.0000 Uiso R . . . . . .
H62 H -0.1101 0.5303 0.3136 0.1632 1.0000 Uiso R . . . . . .
H63 H 0.0169 0.4778 0.3414 0.1632 1.0000 Uiso R . . . . . .
H71 H -0.1281 0.3586 0.1904 0.1515 1.0000 Uiso R . . . . . .
H72 H -0.1309 0.4634 0.1968 0.1515 1.0000 Uiso R . . . . . .
H73 H -0.0039 0.4110 0.2245 0.1515 1.0000 Uiso R . . . . . .
H81 H 0.2809 0.0532 0.4468 0.1350 1.0000 Uiso R . . . . . .
H91 H 0.3695 0.1570 0.5343 0.1355 1.0000 Uiso R . . . . . .
H92 H 0.4752 0.0928 0.5131 0.1355 1.0000 Uiso R . . . . . .
H93 H 0.4581 0.1890 0.4777 0.1355 1.0000 Uiso R . . . . . .
H101 H 0.3153 0.0503 0.3253 0.1436 1.0000 Uiso R . . . . . .
H102 H 0.4405 0.0259 0.3808 0.1436 1.0000 Uiso R . . . . . .
H103 H 0.4234 0.1221 0.3454 0.1436 1.0000 Uiso R . . . . . .
H111 H 0.2436 0.1983 0.2144 0.1536 1.0000 Uiso R . . . . . .
H121 H 0.3581 0.3172 0.2611 0.1674 1.0000 Uiso R . . . . . .
H122 H 0.2732 0.3830 0.2062 0.1674 1.0000 Uiso R . . . . . .
H123 H 0.3573 0.3110 0.1739 0.1674 1.0000 Uiso R . . . . . .
H131 H 0.0532 0.2196 0.1311 0.1667 1.0000 Uiso R . . . . . .
H132 H 0.0856 0.3217 0.1260 0.1667 1.0000 Uiso R . . . . . .
H133 H 0.1697 0.2498 0.0937 0.1667 1.0000 Uiso R . . . . . .
H141 H 0.1832 0.4686 0.4667 0.1416 1.0000 Uiso R . . . . . .
H151 H 0.2400 0.5004 0.3521 0.1497 1.0000 Uiso R . . . . . .
H152 H 0.3495 0.5330 0.4157 0.1497 1.0000 Uiso R . . . . . .
H153 H 0.3648 0.4433 0.3728 0.1497 1.0000 Uiso R . . . . . .
H161 H 0.3103 0.3733 0.5482 0.1508 1.0000 Uiso R . . . . . .
H162 H 0.3915 0.4575 0.5340 0.1508 1.0000 Uiso R . . . . . .
H163 H 0.4069 0.3677 0.4911 0.1508 1.0000 Uiso R . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.79(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 . 1.545(10) yes
C1 . O1 . 1.458(9) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C2 . H21 . 0.950 no
C2 . H22 . 0.950 no
C2 . H23 . 0.950 no
C3 . C4 . 1.539(10) yes
C3 . O2 . 1.459(10) yes
C3 . H31 . 0.950 no
C3 . H32 . 0.950 no
C4 . H41 . 0.950 no
C4 . H42 . 0.950 no
C4 . H43 . 0.950 no
C5 . C6 . 1.45(4) yes
C5 . C7 . 1.536(10) yes
C5 . O3 . 1.40(3) yes
C5 . H51 . 0.950 no
C6 . H61 . 0.950 no
C6 . H62 . 0.950 no
C6 . H63 . 0.950 no
C7 . H71 . 0.950 no
C7 . H72 . 0.950 no
C7 . H73 . 0.950 no
C8 . C9 . 1.49(3) yes
C8 . C10 . 1.46(3) yes
C8 . O4 . 1.42(2) yes
C8 . H81 . 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 . 1.43(3) yes
C11 . C13 . 1.530(10) yes
C11 . O5 . 1.37(3) yes
C11 . H111 . 0.950 no
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 . C15 . 1.45(3) yes
C14 . C16 . 1.48(3) yes
C14 . O6 . 1.41(2) yes
C14 . H141 . 0.950 no
C15 . H151 . 0.950 no
C15 . H152 . 0.950 no
C15 . H153 . 0.950 no
C16 . H161 . 0.950 no
C16 . H162 . 0.950 no
C16 . H163 . 0.950 no
Ta1 . Sn1 . 3.1161(10) yes
Ta1 . O3 . 2.121(8) yes
Ta1 . O1 . 2.119(8) yes
Ta1 . O2 . 2.127(9) yes
Ta1 . O5 . 1.837(9) yes
Ta1 . O4 . 1.843(9) yes
Ta1 . O6 . 1.828(10) yes
Sn1 . O3 . 2.093(8) yes
Sn1 . O1 . 2.077(8) yes
Sn1 . O2 . 2.104(10) yes
Sn1 . Cl2 . 2.344(4) yes
Sn1 . Cl3 . 2.358(4) yes
Sn1 . Cl1 . 2.340(5) 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 . O1 . 106.1(16) yes
C2 . C1 . H11 . 111.1 no
O1 . C1 . H11 . 110.7 no
C2 . C1 . H12 . 109.1 no
O1 . C1 . H12 . 110.4 no
H11 . C1 . H12 . 109.5 no
C1 . C2 . H21 . 108.8 no
C1 . C2 . H22 . 108.8 no
H21 . C2 . H22 . 109.5 no
C1 . C2 . H23 . 110.8 no
H21 . C2 . H23 . 109.5 no
H22 . C2 . H23 . 109.5 no
C4 . C3 . O2 . 101.1(17) yes
C4 . C3 . H31 . 111.6 no
O2 . C3 . H31 . 110.1 no
C4 . C3 . H32 . 112.9 no
O2 . C3 . H32 . 111.5 no
H31 . C3 . H32 . 109.5 no
C3 . C4 . H41 . 107.2 no
C3 . C4 . H42 . 111.2 no
H41 . C4 . H42 . 109.5 no
C3 . C4 . H43 . 109.9 no
H41 . C4 . H43 . 109.5 no
H42 . C4 . H43 . 109.5 no
C6 . C5 . C7 . 100(2) yes
C6 . C5 . O3 . 109(2) yes
C7 . C5 . O3 . 112.2(20) yes
C6 . C5 . H51 . 114.5 no
C7 . C5 . H51 . 111.0 no
O3 . C5 . H51 . 109.9 no
C5 . C6 . H61 . 103.5 no
C5 . C6 . H62 . 110.6 no
H61 . C6 . H62 . 109.5 no
C5 . C6 . H63 . 114.1 no
H61 . C6 . H63 . 109.5 no
H62 . C6 . H63 . 109.5 no
C5 . C7 . H71 . 106.9 no
C5 . C7 . H72 . 110.8 no
H71 . C7 . H72 . 109.5 no
C5 . C7 . H73 . 110.7 no
H71 . C7 . H73 . 109.5 no
H72 . C7 . H73 . 109.5 no
C9 . C8 . C10 . 115(2) yes
C9 . C8 . O4 . 111(2) yes
C10 . C8 . O4 . 112.1(19) yes
C9 . C8 . H81 . 105.4 no
C10 . C8 . H81 . 106.4 no
O4 . C8 . H81 . 106.3 no
C8 . C9 . H91 . 110.0 no
C8 . C9 . H92 . 110.7 no
H91 . C9 . H92 . 109.5 no
C8 . C9 . H93 . 107.7 no
H91 . C9 . H93 . 109.5 no
H92 . C9 . H93 . 109.5 no
C8 . C10 . H101 . 109.7 no
C8 . C10 . H102 . 110.0 no
H101 . C10 . H102 . 109.5 no
C8 . C10 . H103 . 108.7 no
H101 . C10 . H103 . 109.5 no
H102 . C10 . H103 . 109.5 no
C12 . C11 . C13 . 107(2) yes
C12 . C11 . O5 . 113(2) yes
C13 . C11 . O5 . 114(2) yes
C12 . C11 . H111 . 109.0 no
C13 . C11 . H111 . 106.1 no
O5 . C11 . H111 . 106.8 no
C11 . C12 . H121 . 104.9 no
C11 . C12 . H122 . 112.1 no
H121 . C12 . H122 . 109.5 no
C11 . C12 . H123 . 111.3 no
H121 . C12 . H123 . 109.5 no
H122 . C12 . H123 . 109.5 no
C11 . C13 . H131 . 108.6 no
C11 . C13 . H132 . 109.0 no
H131 . C13 . H132 . 109.5 no
C11 . C13 . H133 . 110.7 no
H131 . C13 . H133 . 109.5 no
H132 . C13 . H133 . 109.5 no
C15 . C14 . C16 . 108(2) yes
C15 . C14 . O6 . 109(2) yes
C16 . C14 . O6 . 110(2) yes
C15 . C14 . H141 . 110.8 no
C16 . C14 . H141 . 109.1 no
O6 . C14 . H141 . 109.6 no
C14 . C15 . H151 . 108.4 no
C14 . C15 . H152 . 110.3 no
H151 . C15 . H152 . 109.5 no
C14 . C15 . H153 . 109.7 no
H151 . C15 . H153 . 109.5 no
H152 . C15 . H153 . 109.5 no
C14 . C16 . H161 . 109.3 no
C14 . C16 . H162 . 111.1 no
H161 . C16 . H162 . 109.5 no
C14 . C16 . H163 . 107.9 no
H161 . C16 . H163 . 109.5 no
H162 . C16 . H163 . 109.5 no
Sn1 . Ta1 . O3 . 42.0(2) yes
Sn1 . Ta1 . O1 . 41.5(2) yes
O3 . Ta1 . O1 . 71.0(3) yes
Sn1 . Ta1 . O2 . 42.3(3) yes
O3 . Ta1 . O2 . 70.6(3) yes
O1 . Ta1 . O2 . 70.5(4) yes
Sn1 . Ta1 . O5 . 118.4(4) yes
O3 . Ta1 . O5 . 92.7(4) yes
O1 . Ta1 . O5 . 159.9(4) yes
O2 . Ta1 . O5 . 93.3(5) yes
Sn1 . Ta1 . O4 . 118.4(3) yes
O3 . Ta1 . O4 . 160.3(4) yes
O1 . Ta1 . O4 . 94.1(4) yes
O2 . Ta1 . O4 . 92.7(4) yes
O5 . Ta1 . O4 . 98.7(5) yes
Sn1 . Ta1 . O6 . 118.9(4) yes
O3 . Ta1 . O6 . 95.3(4) yes
O1 . Ta1 . O6 . 93.4(4) yes
O2 . Ta1 . O6 . 161.2(5) yes
O5 . Ta1 . O6 . 99.9(6) yes
O4 . Ta1 . O6 . 98.4(5) yes
Ta1 . Sn1 . O3 . 42.6(2) yes
Ta1 . Sn1 . O1 . 42.6(2) yes
O3 . Sn1 . O1 . 72.3(3) yes
Ta1 . Sn1 . O2 . 42.9(2) yes
O3 . Sn1 . O2 . 71.6(3) yes
O1 . Sn1 . O2 . 71.8(3) yes
Ta1 . Sn1 . Cl2 . 120.87(15) yes
O3 . Sn1 . Cl2 . 94.9(3) yes
O1 . Sn1 . Cl2 . 163.4(3) yes
O2 . Sn1 . Cl2 . 94.3(3) yes
Ta1 . Sn1 . Cl3 . 119.57(12) yes
O3 . Sn1 . Cl3 . 162.2(3) yes
O1 . Sn1 . Cl3 . 93.5(3) yes
O2 . Sn1 . Cl3 . 94.1(3) yes
Cl2 . Sn1 . Cl3 . 96.67(18) yes
Ta1 . Sn1 . Cl1 . 121.48(16) yes
O3 . Sn1 . Cl1 . 95.1(3) yes
O1 . Sn1 . Cl1 . 96.6(3) yes
O2 . Sn1 . Cl1 . 164.3(3) yes
Cl2 . Sn1 . Cl1 . 95.0(2) yes
Cl3 . Sn1 . Cl1 . 97.3(2) yes
C5 . O3 . Ta1 . 140.8(13) yes
C5 . O3 . Sn1 . 123.8(13) yes
Ta1 . O3 . Sn1 . 95.4(3) yes
C1 . O1 . Ta1 . 139.1(12) yes
C1 . O1 . Sn1 . 123.9(12) yes
Ta1 . O1 . Sn1 . 95.9(3) yes
C3 . O2 . Ta1 . 132.7(14) yes
C3 . O2 . Sn1 . 127.9(14) yes
Ta1 . O2 . Sn1 . 94.9(3) yes
C11 . O5 . Ta1 . 160.3(14) yes
C8 . O4 . Ta1 . 174.2(13) yes
C14 . O6 . Ta1 . 178.6(14) yes
####################################################################### 
# 
# 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_SMR224c_2
_database_code_depnum_ccdc_archive 'CCDC 759074'
_audit_update_record             
;
2009-12-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'SMR224c_2.cif'

_audit_creation_date             09-12-18
_audit_creation_method           CRYSTALS_ver_12.87

_oxford_structure_analysis_title 'smr224c_2 in P -1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.8500(10)
_cell_length_b                   14.698(2)
_cell_length_c                   16.507(2)
_cell_angle_alpha                90.914(9)
_cell_angle_beta                 91.216(9)
_cell_angle_gamma                96.418(9)
_cell_volume                     2373.9(5)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
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'
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'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C48 H60 Cl8 O16 Sn2 Ti2
# Dc = 2.11 Fooo = 1168.00 Mu = 18.93 M = 1509.80
# Found Formula = C24 H64 Cl8 O12 Sn2 Ti2
# Dc = 1.62 FOOO = 1168.00 Mu = 18.59 M = 1161.57

_chemical_formula_sum            'C12 H32 Cl4 O6 Sn Ti'
_chemical_formula_moiety         'C12 H32 Cl4 O6 Sn Ti'
_chemical_compound_source        ?
_chemical_formula_weight         580.76


_cell_measurement_reflns_used    4541
_cell_measurement_theta_min      3.3897
_cell_measurement_theta_max      29.2459
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.093
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_max          0.279

_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1168
_exptl_absorpt_coefficient_mu    1.859

# Sheldrick geometric approximatio 0.65 0.84
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            10650
_reflns_number_total             7946
_diffrn_reflns_av_R_equivalents  0.039
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 7946
# Theoretical number of reflections is about 26231


_diffrn_reflns_theta_min         3.408
_diffrn_reflns_theta_max         29.406
_diffrn_measured_fraction_theta_max 0.605

_diffrn_reflns_theta_full        25.289
_diffrn_measured_fraction_theta_full 0.752


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              -19
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              21

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -1.49
_refine_diff_density_max         1.81


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


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         7944
_refine_ls_number_restraints     54
_refine_ls_number_parameters     434
_oxford_refine_ls_R_factor_ref   0.1230
_refine_ls_wR_factor_ref         0.1899
_refine_ls_goodness_of_fit_ref   0.9789
_refine_ls_shift/su_max          0.0008058
_refine_ls_shift/su_mean         5.2932830


# The values computed from all data
_oxford_reflns_number_all        7944
_refine_ls_R_factor_all          0.1230
_refine_ls_wR_factor_all         0.1899

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4883
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_gt          0.1685

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
654. 874. 461. 138.
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
C1 C 0.1338(14) 0.4123(10) -0.5161(9) 0.0502 1.0000 Uani . . . . . . .
C2 C 0.2821(19) 0.4176(13) -0.5342(12) 0.0793 1.0000 Uani . . . . . . .
C3 C -0.1371(14) 0.0822(10) -0.5132(9) 0.0491 1.0000 Uani . . . . . . .
C4 C -0.2934(14) 0.0851(12) -0.5056(11) 0.0626 1.0000 Uani . . . . . . .
C5 C 0.233(2) 0.1779(17) -0.6776(14) 0.1033 1.0000 Uani D U . . . . .
C6 C 0.324(2) 0.1036(15) -0.6691(13) 0.1077 1.0000 Uani D . . . . . .
C7 C 0.113(3) 0.3566(18) -0.7641(16) 0.1242 1.0000 Uani D U . . . . .
C8 C 0.061(3) 0.445(2) -0.7422(16) 0.1488 1.0000 Uani D U . . . . .
C9 C -0.2200(19) 0.1201(17) -0.7351(12) 0.0918 1.0000 Uani D U . . . . .
C10 C -0.128(2) 0.084(2) -0.7957(14) 0.1441 1.0000 Uani D U . . . . .
C11 C -0.285(2) 0.3418(19) -0.6353(13) 0.1056 1.0000 Uani D U . . . . .
C12 C -0.409(2) 0.378(2) -0.6029(16) 0.1567 1.0000 Uani D U . . . . .
C13 C 0.7122(18) 0.3777(14) 0.0534(12) 0.0845 1.0000 Uani D U . . . . .
C14 C 0.814(2) 0.3195(16) 0.0863(15) 0.1116 1.0000 Uani D U . . . . .
C15 C 0.3235(15) 0.1376(12) -0.0987(10) 0.0627 1.0000 Uani . U . . . . .
C16 C 0.2142(19) 0.1811(15) -0.1423(13) 0.0881 1.0000 Uani . U . . . . .
C17 C 0.7732(14) 0.0810(10) -0.1094(9) 0.0491 1.0000 Uani . . . . . . .
C18 C 0.8820(15) 0.0824(12) -0.0496(11) 0.0641 1.0000 Uani . . . . . . .
C19 C 0.9059(14) 0.3244(12) -0.1599(9) 0.0583 1.0000 Uani . . . . . . .
C20 C 1.0061(14) 0.3798(13) -0.1030(11) 0.0712 1.0000 Uani . . . . . . .
C21 C 0.505(3) 0.0931(11) -0.2997(13) 0.1023 1.0000 Uani D U . . . . .
C22 C 0.520(2) 0.1944(11) -0.2877(9) 0.0746 1.0000 Uani D . . . . . .
C23 C 0.4594(18) 0.4158(14) -0.1895(10) 0.0720 1.0000 Uani . . . . . . .
C24 C 0.570(3) 0.4442(16) -0.2482(13) 0.1090 1.0000 Uani . U . . . . .
O1 O 0.0715(9) 0.3181(7) -0.5157(5) 0.0460 1.0000 Uani . . . . . . .
O2 O -0.0701(9) 0.1753(6) -0.5106(5) 0.0402 1.0000 Uani . . . . . . .
O3 O 0.1331(11) 0.1672(9) -0.6181(6) 0.0670 1.0000 Uani . . . . . . .
O4 O 0.0476(13) 0.3281(10) -0.6808(7) 0.0872 1.0000 Uani . . . . . . .
O5 O -0.1356(11) 0.1773(8) -0.6761(6) 0.0641 1.0000 Uani . . . . . . .
O6 O -0.1767(10) 0.3269(9) -0.5840(6) 0.0673 1.0000 Uani . . . . . . .
O7 O 0.6155(9) 0.2898(7) 0.0110(6) 0.0524 1.0000 Uani . . . . . . .
O8 O 0.4222(8) 0.2052(6) -0.0605(5) 0.0374 1.0000 Uani . . . . . . .
O9 O 0.6589(9) 0.1269(6) -0.0809(6) 0.0447 1.0000 Uani . . . . . . .
O10 O 0.7787(9) 0.2984(7) -0.1206(6) 0.0527 1.0000 Uani . . . . . . .
O11 O 0.5533(9) 0.2215(7) -0.2077(5) 0.0479 1.0000 Uani . . . . . . .
O12 O 0.5313(10) 0.3804(7) -0.1195(6) 0.0538 1.0000 Uani . . . . . . .
Cl1 Cl 0.2225(4) 0.1608(3) -0.4385(3) 0.0666 1.0000 Uani . . . . . . .
Cl2 Cl 0.1601(4) 0.3473(3) -0.3234(2) 0.0609 1.0000 Uani . . . . . . .
Cl3 Cl -0.0597(5) 0.1369(3) -0.3178(2) 0.0656 1.0000 Uani . . . . . . .
Cl4 Cl -0.1700(4) 0.3323(3) -0.3981(2) 0.0555 1.0000 Uani . . . . . . .
Cl5 Cl 0.5208(3) 0.0964(3) 0.0883(2) 0.0496 1.0000 Uani . . . . . . .
Cl6 Cl 0.4901(4) 0.2941(3) 0.1945(2) 0.0572 1.0000 Uani . . . . . . .
Cl7 Cl 0.2031(3) 0.1751(3) 0.0869(2) 0.0513 1.0000 Uani . . . . . . .
Cl8 Cl 0.3486(4) 0.3872(3) 0.0286(2) 0.0560 1.0000 Uani . . . . . . .
Sn2 Sn 0.42916(9) 0.24076(7) 0.06092(6) 0.0411 1.0000 Uani . . . . . . .
Ti2 Ti 0.6081(2) 0.25448(17) -0.10951(14) 0.0383 1.0000 Uani . . . . . . .
Sn1 Sn 0.02698(9) 0.24460(7) -0.41293(6) 0.0422 1.0000 Uani . . . . . . .
Ti1 Ti -0.0258(3) 0.2488(2) -0.61294(15) 0.0497 1.0000 Uani . . . . . . .
H11 H 0.0881 0.4456 -0.5572 0.0620 1.0000 Uiso R . . . . . .
H12 H 0.1242 0.4406 -0.4633 0.0620 1.0000 Uiso R . . . . . .
H21 H 0.3129 0.4752 -0.5582 0.1210 1.0000 Uiso R . . . . . .
H22 H 0.2980 0.3684 -0.5710 0.1209 1.0000 Uiso R . . . . . .
H23 H 0.3330 0.4119 -0.4845 0.1210 1.0000 Uiso R . . . . . .
H31 H -0.1183 0.0532 -0.5641 0.0589 1.0000 Uiso R . . . . . .
H32 H -0.1028 0.0482 -0.4689 0.0590 1.0000 Uiso R . . . . . .
H41 H -0.3390 0.0245 -0.4979 0.0929 1.0000 Uiso R . . . . . .
H42 H -0.3294 0.1099 -0.5540 0.0930 1.0000 Uiso R . . . . . .
H43 H -0.3110 0.1231 -0.4605 0.0930 1.0000 Uiso R . . . . . .
H51 H 0.1879 0.1720 -0.7301 0.1270 1.0000 Uiso R . . . . . .
H52 H 0.2861 0.2373 -0.6715 0.1269 1.0000 Uiso R . . . . . .
H61 H 0.3614 0.0908 -0.7206 0.1610 1.0000 Uiso R . . . . . .
H62 H 0.2734 0.0493 -0.6494 0.1610 1.0000 Uiso R . . . . . .
H63 H 0.3966 0.1240 -0.6313 0.1610 1.0000 Uiso R . . . . . .
H71 H 0.0685 0.3263 -0.8123 0.1530 1.0000 Uiso R . . . . . .
H72 H 0.2116 0.3585 -0.7680 0.1531 1.0000 Uiso R . . . . . .
H81 H 0.1111 0.4949 -0.7696 0.2271 1.0000 Uiso R . . . . . .
H82 H -0.0345 0.4422 -0.7565 0.2269 1.0000 Uiso R . . . . . .
H83 H 0.0744 0.4538 -0.6847 0.2270 1.0000 Uiso R . . . . . .
H91 H -0.2832 0.1562 -0.7617 0.1120 1.0000 Uiso R . . . . . .
H92 H -0.2708 0.0696 -0.7082 0.1120 1.0000 Uiso R . . . . . .
H101 H -0.1830 0.0463 -0.8344 0.2200 1.0000 Uiso R . . . . . .
H102 H -0.0793 0.1344 -0.8225 0.2200 1.0000 Uiso R . . . . . .
H103 H -0.0652 0.0494 -0.7685 0.2200 1.0000 Uiso R . . . . . .
H131 H 0.7501 0.4218 0.0147 0.1020 1.0000 Uiso R . . . . . .
H132 H 0.6668 0.4096 0.0953 0.1019 1.0000 Uiso R . . . . . .
H141 H 0.8818 0.3581 0.1182 0.1671 1.0000 Uiso R . . . . . .
H142 H 0.8568 0.2911 0.0423 0.1671 1.0000 Uiso R . . . . . .
H143 H 0.7687 0.2725 0.1197 0.1669 1.0000 Uiso R . . . . . .
H151 H 0.3690 0.1020 -0.1374 0.0759 1.0000 Uiso R . . . . . .
H152 H 0.2822 0.0977 -0.0575 0.0761 1.0000 Uiso R . . . . . .
H161 H 0.1620 0.1359 -0.1761 0.1329 1.0000 Uiso R . . . . . .
H162 H 0.2548 0.2294 -0.1752 0.1329 1.0000 Uiso R . . . . . .
H163 H 0.1556 0.2055 -0.1040 0.1330 1.0000 Uiso R . . . . . .
H171 H 0.8101 0.1124 -0.1567 0.0592 1.0000 Uiso R . . . . . .
H172 H 0.7408 0.0183 -0.1237 0.0589 1.0000 Uiso R . . . . . .
H181 H 0.9382 0.0352 -0.0627 0.0970 1.0000 Uiso R . . . . . .
H182 H 0.9357 0.1404 -0.0494 0.0970 1.0000 Uiso R . . . . . .
H183 H 0.8439 0.0722 0.0029 0.0970 1.0000 Uiso R . . . . . .
H191 H 0.8895 0.3608 -0.2068 0.0710 1.0000 Uiso R . . . . . .
H192 H 0.9455 0.2697 -0.1769 0.0710 1.0000 Uiso R . . . . . .
H201 H 1.0939 0.3898 -0.1275 0.1071 1.0000 Uiso R . . . . . .
H202 H 0.9743 0.4377 -0.0914 0.1070 1.0000 Uiso R . . . . . .
H203 H 1.0142 0.3477 -0.0533 0.1069 1.0000 Uiso R . . . . . .
H211 H 0.4641 0.0774 -0.3521 0.1521 1.0000 Uiso R . . . . . .
H212 H 0.5935 0.0721 -0.2961 0.1521 1.0000 Uiso R . . . . . .
H213 H 0.4482 0.0651 -0.2585 0.1520 1.0000 Uiso R . . . . . .
H221 H 0.5913 0.2217 -0.3218 0.0902 1.0000 Uiso R . . . . . .
H222 H 0.4342 0.2162 -0.3027 0.0901 1.0000 Uiso R . . . . . .
H231 H 0.4106 0.4674 -0.1748 0.0859 1.0000 Uiso R . . . . . .
H232 H 0.3948 0.3675 -0.2129 0.0860 1.0000 Uiso R . . . . . .
H241 H 0.5311 0.4405 -0.3025 0.1621 1.0000 Uiso R . . . . . .
H242 H 0.6080 0.5063 -0.2360 0.1621 1.0000 Uiso R . . . . . .
H243 H 0.6415 0.4043 -0.2441 0.1620 1.0000 Uiso R . . . . . .
H121 H -0.4891 0.3546 -0.6347 0.2380 1.0000 Uiso R . . . . . .
H122 H -0.3917 0.4432 -0.6080 0.2380 1.0000 Uiso R . . . . . .
H123 H -0.4224 0.3623 -0.5470 0.2380 1.0000 Uiso R . . . . . .
H111 H -0.2477 0.3810 -0.6782 0.1291 1.0000 Uiso R . . . . . .
H112 H -0.3205 0.2820 -0.6570 0.1290 1.0000 Uiso R . . . . . .
H6 H -0.1803 0.3382 -0.5352 0.0990 1.0000 Uiso R . . . . . .
H3 H 0.1751 0.1909 -0.5774 0.0991 1.0000 Uiso R . . . . . .
H244 H 0.4976 0.4050 -0.0809 0.0811 1.0000 Uiso R . . . . . .
H9 H 0.5786 0.1236 -0.0672 0.0662 1.0000 Uiso R . . . . . .

_refine_ls_extinction_coef       35(7)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          1.438(11)
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 . 1.49(2) yes
C1 . O1 . 1.452(16) yes
C1 . H11 . 0.973 no
C1 . H12 . 0.971 no
C2 . H21 . 0.961 no
C2 . H22 . 0.966 no
C2 . H23 . 0.961 no
C3 . C4 . 1.55(2) yes
C3 . O2 . 1.451(16) yes
C3 . H31 . 0.966 no
C3 . H32 . 0.969 no
C4 . H41 . 0.963 no
C4 . H42 . 0.960 no
C4 . H43 . 0.955 no
C5 . C6 . 1.494(10) yes
C5 . O3 . 1.40(2) yes
C5 . H51 . 0.963 no
C5 . H52 . 0.970 no
C6 . H61 . 0.958 no
C6 . H62 . 0.958 no
C6 . H63 . 0.957 no
C7 . C8 . 1.490(10) yes
C7 . O4 . 1.57(3) yes
C7 . H71 . 0.975 no
C7 . H72 . 0.975 no
C8 . H81 . 0.960 no
C8 . H82 . 0.963 no
C8 . H83 . 0.961 no
C9 . C10 . 1.490(10) yes
C9 . O5 . 1.46(2) yes
C9 . H91 . 0.964 no
C9 . H92 . 0.968 no
C10 . H101 . 0.957 no
C10 . H102 . 0.954 no
C10 . H103 . 0.958 no
C11 . C12 . 1.485(10) yes
C11 . O6 . 1.39(2) yes
C11 . H111 . 0.973 no
C11 . H112 . 0.969 no
C12 . H121 . 0.965 no
C12 . H122 . 0.965 no
C12 . H123 . 0.962 no
C13 . C14 . 1.488(9) yes
C13 . O7 . 1.65(2) yes
C13 . H131 . 0.968 no
C13 . H132 . 0.974 no
C14 . H141 . 0.967 no
C14 . H142 . 0.961 no
C14 . H143 . 0.965 no
C15 . C16 . 1.49(2) yes
C15 . O8 . 1.439(19) yes
C15 . H151 . 0.967 no
C15 . H152 . 0.971 no
C16 . H161 . 0.958 no
C16 . H162 . 0.957 no
C16 . H163 . 0.957 no
C17 . C18 . 1.440(19) yes
C17 . O9 . 1.458(16) yes
C17 . H171 . 0.969 no
C17 . H172 . 0.966 no
C18 . H181 . 0.960 no
C18 . H182 . 0.952 no
C18 . H183 . 0.958 no
C19 . C20 . 1.51(2) yes
C19 . O10 . 1.440(16) yes
C19 . H191 . 0.969 no
C19 . H192 . 0.973 no
C20 . H201 . 0.960 no
C20 . H202 . 0.956 no
C20 . H203 . 0.958 no
C21 . C22 . 1.489(9) yes
C21 . H211 . 0.959 no
C21 . H212 . 0.959 no
C21 . H213 . 0.958 no
C22 . O11 . 1.394(17) yes
C22 . H221 . 0.964 no
C22 . H222 . 0.968 no
C23 . C24 . 1.50(3) yes
C23 . O12 . 1.475(17) yes
C23 . H231 . 0.972 no
C23 . H232 . 0.969 no
C24 . H241 . 0.966 no
C24 . H242 . 0.963 no
C24 . H243 . 0.966 no
O1 . Sn1 . 2.055(8) yes
O1 . Ti1 . 2.048(10) yes
O2 . Sn1 . 2.053(9) yes
O2 . Ti1 . 2.048(8) yes
O3 . Ti1 . 2.078(12) yes
O3 . H3 . 0.834 no
O4 . Ti1 . 1.739(11) yes
O5 . Ti1 . 1.739(11) yes
O6 . Ti1 . 2.037(12) yes
O6 . H6 . 0.822 no
O7 . Sn2 . 2.087(9) yes
O7 . Ti2 . 2.045(11) yes
O8 . Sn2 . 2.060(9) yes
O8 . Ti2 . 2.077(8) yes
O9 . Ti2 . 2.054(9) yes
O9 . H9 . 0.824 no
O10 . Ti2 . 1.746(9) yes
O11 . Ti2 . 1.742(9) yes
O12 . Ti2 . 2.084(10) yes
O12 . H244 . 0.821 no
Cl1 . Sn1 . 2.439(4) yes
Cl2 . Sn1 . 2.364(4) yes
Cl3 . Sn1 . 2.352(4) yes
Cl4 . Sn1 . 2.460(4) yes
Cl5 . Sn2 . 2.443(4) yes
Cl6 . Sn2 . 2.371(4) yes
Cl7 . Sn2 . 2.377(3) yes
Cl8 . Sn2 . 2.439(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 . O1 . 111.3(14) yes
C2 . C1 . H11 . 109.0 no
O1 . C1 . H11 . 109.2 no
C2 . C1 . H12 . 108.5 no
O1 . C1 . H12 . 109.3 no
H11 . C1 . H12 . 109.4 no
C1 . C2 . H21 . 110.6 no
C1 . C2 . H22 . 109.8 no
H21 . C2 . H22 . 109.2 no
C1 . C2 . H23 . 109.1 no
H21 . C2 . H23 . 109.0 no
H22 . C2 . H23 . 109.1 no
C4 . C3 . O2 . 108.7(13) yes
C4 . C3 . H31 . 109.8 no
O2 . C3 . H31 . 109.4 no
C4 . C3 . H32 . 109.9 no
O2 . C3 . H32 . 109.6 no
H31 . C3 . H32 . 109.5 no
C3 . C4 . H41 . 110.6 no
C3 . C4 . H42 . 109.6 no
H41 . C4 . H42 . 109.2 no
C3 . C4 . H43 . 109.8 no
H41 . C4 . H43 . 108.9 no
H42 . C4 . H43 . 108.8 no
C6 . C5 . O3 . 108.7(17) yes
C6 . C5 . H51 . 109.0 no
O3 . C5 . H51 . 108.5 no
C6 . C5 . H52 . 110.1 no
O3 . C5 . H52 . 110.2 no
H51 . C5 . H52 . 110.3 no
C5 . C6 . H61 . 109.6 no
C5 . C6 . H62 . 110.1 no
H61 . C6 . H62 . 109.5 no
C5 . C6 . H63 . 108.6 no
H61 . C6 . H63 . 109.5 no
H62 . C6 . H63 . 109.4 no
C8 . C7 . O4 . 82(2) yes
C8 . C7 . H71 . 114.1 no
O4 . C7 . H71 . 116.1 no
C8 . C7 . H72 . 115.6 no
O4 . C7 . H72 . 117.5 no
H71 . C7 . H72 . 109.7 no
C7 . C8 . H81 . 110.7 no
C7 . C8 . H82 . 109.7 no
H81 . C8 . H82 . 109.7 no
C7 . C8 . H83 . 107.1 no
H81 . C8 . H83 . 109.6 no
H82 . C8 . H83 . 110.0 no
C10 . C9 . O5 . 108.3(16) yes
C10 . C9 . H91 . 110.1 no
O5 . C9 . H91 . 109.6 no
C10 . C9 . H92 . 109.8 no
O5 . C9 . H92 . 110.0 no
H91 . C9 . H92 . 109.1 no
C9 . C10 . H101 . 108.8 no
C9 . C10 . H102 . 109.3 no
H101 . C10 . H102 . 109.8 no
C9 . C10 . H103 . 109.3 no
H101 . C10 . H103 . 110.0 no
H102 . C10 . H103 . 109.6 no
C12 . C11 . O6 . 120.7(19) yes
C12 . C11 . H111 . 109.8 no
O6 . C11 . H111 . 106.9 no
C12 . C11 . H112 . 103.0 no
O6 . C11 . H112 . 105.6 no
H111 . C11 . H112 . 110.6 no
C11 . C12 . H121 . 110.8 no
C11 . C12 . H122 . 104.8 no
H121 . C12 . H122 . 109.8 no
C11 . C12 . H123 . 112.0 no
H121 . C12 . H123 . 109.5 no
H122 . C12 . H123 . 109.9 no
C14 . C13 . O7 . 93.5(15) yes
C14 . C13 . H131 . 113.3 no
O7 . C13 . H131 . 113.4 no
C14 . C13 . H132 . 113.4 no
O7 . C13 . H132 . 113.9 no
H131 . C13 . H132 . 108.9 no
C13 . C14 . H141 . 108.4 no
C13 . C14 . H142 . 109.4 no
H141 . C14 . H142 . 110.0 no
C13 . C14 . H143 . 109.7 no
H141 . C14 . H143 . 110.2 no
H142 . C14 . H143 . 109.1 no
C16 . C15 . O8 . 111.3(15) yes
C16 . C15 . H151 . 108.5 no
O8 . C15 . H151 . 109.1 no
C16 . C15 . H152 . 109.1 no
O8 . C15 . H152 . 108.9 no
H151 . C15 . H152 . 109.8 no
C15 . C16 . H161 . 109.0 no
C15 . C16 . H162 . 109.6 no
H161 . C16 . H162 . 109.4 no
C15 . C16 . H163 . 109.7 no
H161 . C16 . H163 . 109.6 no
H162 . C16 . H163 . 109.5 no
C18 . C17 . O9 . 112.5(13) yes
C18 . C17 . H171 . 107.8 no
O9 . C17 . H171 . 108.7 no
C18 . C17 . H172 . 109.1 no
O9 . C17 . H172 . 109.0 no
H171 . C17 . H172 . 109.8 no
C17 . C18 . H181 . 109.0 no
C17 . C18 . H182 . 109.6 no
H181 . C18 . H182 . 109.6 no
C17 . C18 . H183 . 109.5 no
H181 . C18 . H183 . 110.0 no
H182 . C18 . H183 . 109.3 no
C20 . C19 . O10 . 110.9(13) yes
C20 . C19 . H191 . 108.9 no
O10 . C19 . H191 . 109.5 no
C20 . C19 . H192 . 108.6 no
O10 . C19 . H192 . 109.4 no
H191 . C19 . H192 . 109.5 no
C19 . C20 . H201 . 109.9 no
C19 . C20 . H202 . 109.6 no
H201 . C20 . H202 . 109.2 no
C19 . C20 . H203 . 109.7 no
H201 . C20 . H203 . 109.4 no
H202 . C20 . H203 . 109.0 no
C22 . C21 . H211 . 109.6 no
C22 . C21 . H212 . 108.8 no
H211 . C21 . H212 . 109.7 no
C22 . C21 . H213 . 109.6 no
H211 . C21 . H213 . 109.7 no
H212 . C21 . H213 . 109.5 no
C21 . C22 . O11 . 112.9(15) yes
C21 . C22 . H221 . 109.5 no
O11 . C22 . H221 . 108.3 no
C21 . C22 . H222 . 108.0 no
O11 . C22 . H222 . 108.5 no
H221 . C22 . H222 . 109.6 no
C24 . C23 . O12 . 104.7(15) yes
C24 . C23 . H231 . 110.8 no
O12 . C23 . H231 . 112.3 no
C24 . C23 . H232 . 110.6 no
O12 . C23 . H232 . 109.5 no
H231 . C23 . H232 . 108.8 no
C23 . C24 . H241 . 108.8 no
C23 . C24 . H242 . 109.4 no
H241 . C24 . H242 . 109.4 no
C23 . C24 . H243 . 110.2 no
H241 . C24 . H243 . 109.6 no
H242 . C24 . H243 . 109.4 no
C1 . O1 . Sn1 . 124.6(8) yes
C1 . O1 . Ti1 . 125.2(8) yes
Sn1 . O1 . Ti1 . 108.7(4) yes
C3 . O2 . Sn1 . 127.5(8) yes
C3 . O2 . Ti1 . 122.7(8) yes
Sn1 . O2 . Ti1 . 108.8(4) yes
C5 . O3 . Ti1 . 122.2(11) yes
C5 . O3 . H3 . 102.2 no
Ti1 . O3 . H3 . 95.2 no
C7 . O4 . Ti1 . 153.3(15) yes
C9 . O5 . Ti1 . 174.8(11) yes
C11 . O6 . Ti1 . 124.6(13) yes
C11 . O6 . H6 . 119.9 no
Ti1 . O6 . H6 . 113.6 no
C13 . O7 . Sn2 . 120.6(9) yes
C13 . O7 . Ti2 . 125.8(8) yes
Sn2 . O7 . Ti2 . 108.3(4) yes
C15 . O8 . Sn2 . 125.1(8) yes
C15 . O8 . Ti2 . 124.8(8) yes
Sn2 . O8 . Ti2 . 108.0(4) yes
C17 . O9 . Ti2 . 128.5(7) yes
C17 . O9 . H9 . 149.0 no
Ti2 . O9 . H9 . 78.1 no
C19 . O10 . Ti2 . 158.9(9) yes
C22 . O11 . Ti2 . 175.5(11) yes
C23 . O12 . Ti2 . 128.0(11) yes
C23 . O12 . H244 . 102.5 no
Ti2 . O12 . H244 . 121.9 no
Cl5 . Sn2 . Cl8 . 176.77(13) yes
Cl5 . Sn2 . O7 . 89.1(3) yes
Cl8 . Sn2 . O7 . 87.8(3) yes
Cl5 . Sn2 . Cl7 . 91.60(13) yes
Cl8 . Sn2 . Cl7 . 91.29(13) yes
O7 . Sn2 . Cl7 . 167.0(3) yes
Cl5 . Sn2 . Cl6 . 90.41(14) yes
Cl8 . Sn2 . Cl6 . 90.62(15) yes
O7 . Sn2 . Cl6 . 95.2(3) yes
Cl7 . Sn2 . Cl6 . 97.75(14) yes
Cl5 . Sn2 . O8 . 88.3(3) yes
Cl8 . Sn2 . O8 . 90.0(3) yes
O7 . Sn2 . O8 . 71.6(4) yes
Cl7 . Sn2 . O8 . 95.4(2) yes
Cl6 . Sn2 . O8 . 166.8(2) yes
O12 . Ti2 . O8 . 87.2(4) yes
O12 . Ti2 . O9 . 168.8(4) yes
O8 . Ti2 . O9 . 83.0(4) yes
O12 . Ti2 . O7 . 82.1(4) yes
O8 . Ti2 . O7 . 72.1(3) yes
O9 . Ti2 . O7 . 89.7(4) yes
O12 . Ti2 . O10 . 95.2(4) yes
O8 . Ti2 . O10 . 163.1(4) yes
O9 . Ti2 . O10 . 92.6(4) yes
O7 . Ti2 . O10 . 91.6(4) yes
O12 . Ti2 . O11 . 92.1(4) yes
O8 . Ti2 . O11 . 92.9(4) yes
O9 . Ti2 . O11 . 93.8(4) yes
O7 . Ti2 . O11 . 164.1(4) yes
O10 . Ti2 . O11 . 103.7(5) yes
Cl4 . Sn1 . Cl1 . 175.62(14) yes
Cl4 . Sn1 . O1 . 87.1(3) yes
Cl1 . Sn1 . O1 . 88.8(3) yes
Cl4 . Sn1 . Cl2 . 90.80(15) yes
Cl1 . Sn1 . Cl2 . 91.11(16) yes
O1 . Sn1 . Cl2 . 95.8(3) yes
Cl4 . Sn1 . O2 . 89.5(3) yes
Cl1 . Sn1 . O2 . 87.7(3) yes
O1 . Sn1 . O2 . 71.1(3) yes
Cl2 . Sn1 . O2 . 166.9(2) yes
Cl4 . Sn1 . Cl3 . 91.75(15) yes
Cl1 . Sn1 . Cl3 . 91.87(17) yes
O1 . Sn1 . Cl3 . 165.6(3) yes
Cl2 . Sn1 . Cl3 . 98.58(14) yes
O2 . Sn1 . Cl3 . 94.5(3) yes
O3 . Ti1 . O1 . 89.0(4) yes
O3 . Ti1 . O2 . 82.3(4) yes
O1 . Ti1 . O2 . 71.4(3) yes
O3 . Ti1 . O6 . 168.8(4) yes
O1 . Ti1 . O6 . 82.2(4) yes
O2 . Ti1 . O6 . 88.2(4) yes
O3 . Ti1 . O4 . 94.1(6) yes
O1 . Ti1 . O4 . 92.2(5) yes
O2 . Ti1 . O4 . 163.2(5) yes
O6 . Ti1 . O4 . 93.2(6) yes
O3 . Ti1 . O5 . 94.7(5) yes
O1 . Ti1 . O5 . 165.1(4) yes
O2 . Ti1 . O5 . 94.8(4) yes
O6 . Ti1 . O5 . 92.1(5) yes
O4 . Ti1 . O5 . 101.9(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
O9 . H9 . C15 . 151 0.82 2.59 3.33(3) yes
O9 . H9 . O8 . 139 0.82 2.06 2.74(3) yes
####################################################################### 
# 
# 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_SMR224b
_database_code_depnum_ccdc_archive 'CCDC 759076'
_audit_update_record             
;
2009-12-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'SMR224b.cif'

_audit_creation_date             09-12-18
_audit_creation_method           CRYSTALS_ver_12.87

_oxford_structure_analysis_title 'smr224b in P 1 21/n 1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   11.5427(9)
_cell_length_b                   19.876(2)
_cell_length_c                   18.1660(10)
_cell_angle_alpha                90
_cell_angle_beta                 101.309(8)
_cell_angle_gamma                90
_cell_volume                     4086.8(6)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
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'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C31.25 H50 Cl5 O20 Sn1.25 Ti2.50
# Dc = 1.94 Fooo = 1808.00 Mu = 16.36 M = 1191.10
# Found Formula = C27 H65 Cl3 O10 Sn1 Ti2
# Dc = 1.41 FOOO = 1808.00 Mu = 12.27 M = 870.66

_chemical_formula_sum            'C27 H65 Cl3 O10 Sn1 Ti2'
_chemical_formula_moiety         'C27 H65 Cl3 O10 Sn1 Ti2'
_chemical_compound_source        ?
_chemical_formula_weight         870.66


_cell_measurement_reflns_used    9045
_cell_measurement_theta_min      3.5348
_cell_measurement_theta_max      29.4813
_cell_measurement_temperature    150

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.095
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_max          0.400

_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    1.227

# Sheldrick geometric approximatio 0.86 0.89
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            20371
_reflns_number_total             9784
_diffrn_reflns_av_R_equivalents  0.062
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 9784
# Theoretical number of reflections is about 22958


_diffrn_reflns_theta_min         3.548
_diffrn_reflns_theta_max         29.585
_diffrn_measured_fraction_theta_max 0.853

_diffrn_reflns_theta_full        26.331
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       17
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              0
_reflns_limit_k_max              26
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -2.18
_refine_diff_density_max         2.35


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


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         9784
_refine_ls_number_restraints     0
_refine_ls_number_parameters     388
_oxford_refine_ls_R_factor_ref   0.0888
_refine_ls_wR_factor_ref         0.1729
_refine_ls_goodness_of_fit_ref   0.9784
_refine_ls_shift/su_max          0.0013562
_refine_ls_shift/su_mean         1.8561907


# The values computed from all data
_oxford_reflns_number_all        9784
_refine_ls_R_factor_all          0.0888
_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                6722
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_gt          0.1284

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
247. 372. 176. 41.2
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
C1 C 1.2774(6) 0.7593(4) 0.6187(4) 0.0428 1.0000 Uani . . . . . . .
C2 C 1.2502(8) 0.7954(5) 0.5444(5) 0.0635 1.0000 Uani . . . . . . .
C3 C 1.3762(7) 0.7918(6) 0.6730(6) 0.0686 1.0000 Uani . . . . . . .
C4 C 0.9998(6) 0.5186(3) 0.7093(4) 0.0357 1.0000 Uani . . . . . . .
C5 C 1.0584(7) 0.4754(4) 0.6595(5) 0.0483 1.0000 Uani . . . . . . .
C6 C 1.0623(7) 0.5163(4) 0.7897(4) 0.0490 1.0000 Uani . . . . . . .
C7 C 0.7384(6) 0.8046(4) 0.7445(4) 0.0395 1.0000 Uani . . . . . . .
C8 C 0.8165(9) 0.7939(6) 0.8196(5) 0.0669 1.0000 Uani . . . . . . .
C9 C 0.6603(7) 0.8647(4) 0.7444(5) 0.0503 1.0000 Uani . . . . . . .
C10 C 1.0243(6) 0.9016(3) 0.6704(4) 0.0367 1.0000 Uani . . . . . . .
C11 C 1.0924(8) 0.9488(4) 0.6301(6) 0.0566 1.0000 Uani . . . . . . .
C12 C 1.0853(8) 0.8890(5) 0.7500(5) 0.0582 1.0000 Uani . . . . . . .
C13 C 0.7049(7) 0.9082(4) 0.5396(5) 0.0508 1.0000 Uani . . . . . . .
C14 C 0.7610(9) 0.9586(5) 0.4966(6) 0.0683 1.0000 Uani . . . . . . .
C15 C 0.5763(7) 0.8990(5) 0.5075(7) 0.0677 1.0000 Uani . . . . . . .
C16 C 0.8812(7) 0.7726(4) 0.4295(4) 0.0434 1.0000 Uani . . . . . . .
C17 C 0.8696(9) 0.7095(5) 0.3828(5) 0.0663 1.0000 Uani . . . . . . .
C18 C 0.9631(9) 0.8238(6) 0.4095(6) 0.0720 1.0000 Uani . . . . . . .
C19 C 0.6078(5) 0.7154(3) 0.5617(4) 0.0340 1.0000 Uani . . . . . . .
C20 C 0.5904(7) 0.7143(4) 0.4775(4) 0.0485 1.0000 Uani . . . . . . .
C21 C 0.5376(6) 0.6608(4) 0.5911(5) 0.0449 1.0000 Uani . . . . . . .
C22 C 0.7021(8) 0.6079(5) 0.7769(5) 0.0583 1.0000 Uani . . . . . . .
C23 C 0.7865(11) 0.6031(6) 0.8509(5) 0.0869 1.0000 Uani . . . . . . .
C24 C 0.6212(9) 0.5493(5) 0.7608(7) 0.0811 1.0000 Uani . . . . . . .
C25 C 0.7630(6) 0.5131(3) 0.5249(4) 0.0388 1.0000 Uani . . . . . . .
C26 C 0.7098(9) 0.4582(5) 0.5635(5) 0.0640 1.0000 Uani . . . . . . .
C27 C 0.6881(8) 0.5309(4) 0.4500(4) 0.0541 1.0000 Uani . . . . . . .
O1 O 1.1778(4) 0.7550(2) 0.6510(3) 0.0398 1.0000 Uani . . . . . . .
O2 O 0.9871(3) 0.5874(2) 0.6824(2) 0.0284 1.0000 Uani . . . . . . .
O3 O 0.9414(3) 0.7043(2) 0.6426(2) 0.0254 1.0000 Uani . . . . . . .
O4 O 0.8080(4) 0.8152(2) 0.6902(3) 0.0360 1.0000 Uani . . . . . . .
O5 O 1.0050(4) 0.8385(2) 0.6294(2) 0.0309 1.0000 Uani . . . . . . .
O6 O 0.7660(4) 0.8466(2) 0.5433(3) 0.0369 1.0000 Uani . . . . . . .
O7 O 0.9116(4) 0.7539(2) 0.5072(2) 0.0379 1.0000 Uani . . . . . . .
O8 O 0.7322(3) 0.7096(2) 0.5942(2) 0.0283 1.0000 Uani . . . . . . .
O9 O 0.7652(4) 0.6177(3) 0.7197(3) 0.0446 1.0000 Uani . . . . . . .
O10 O 0.7807(4) 0.5707(2) 0.5716(3) 0.0440 1.0000 Uani . . . . . . .
Sn1 Sn 1.10821(3) 0.66497(2) 0.67511(2) 0.0275 1.0000 Uani . . . . . . .
Ti2 Ti 0.82956(9) 0.63155(5) 0.64141(6) 0.0259 1.0000 Uani . . . . . . .
Ti1 Ti 0.84816(9) 0.78564(5) 0.60573(6) 0.0269 1.0000 Uani . . . . . . .
Cl3 Cl 1.09470(15) 0.63040(9) 0.54398(9) 0.0385 1.0000 Uani . . . . . . .
Cl2 Cl 1.10761(15) 0.69669(9) 0.80142(9) 0.0404 1.0000 Uani . . . . . . .
Cl1 Cl 1.28998(14) 0.60533(10) 0.71048(10) 0.0435 1.0000 Uani . . . . . . .
H11 H 1.3020 0.7134 0.6094 0.0520 1.0000 Uiso R . . . . . .
H23 H 1.1913 0.7704 0.5102 0.0950 1.0000 Uiso R . . . . . .
H22 H 1.2203 0.8398 0.5512 0.0950 1.0000 Uiso R . . . . . .
H21 H 1.3210 0.7991 0.5239 0.0950 1.0000 Uiso R . . . . . .
H31 H 1.4000 0.7633 0.7161 0.1040 1.0000 Uiso R . . . . . .
H32 H 1.3500 0.8344 0.6890 0.1039 1.0000 Uiso R . . . . . .
H33 H 1.4427 0.7991 0.6490 0.1040 1.0000 Uiso R . . . . . .
H41 H 0.9196 0.5010 0.7066 0.0430 1.0000 Uiso R . . . . . .
H51 H 1.0142 0.4771 0.6088 0.0718 1.0000 Uiso R . . . . . .
H52 H 1.1372 0.4913 0.6601 0.0720 1.0000 Uiso R . . . . . .
H53 H 1.0619 0.4297 0.6772 0.0720 1.0000 Uiso R . . . . . .
H61 H 1.0239 0.5457 0.8192 0.0729 1.0000 Uiso R . . . . . .
H62 H 1.1429 0.5301 0.7934 0.0730 1.0000 Uiso R . . . . . .
H63 H 1.0599 0.4710 0.8078 0.0729 1.0000 Uiso R . . . . . .
H71 H 0.6888 0.7648 0.7307 0.0480 1.0000 Uiso R . . . . . .
H81 H 0.8704 0.7577 0.8164 0.1010 1.0000 Uiso R . . . . . .
H82 H 0.8603 0.8344 0.8346 0.1009 1.0000 Uiso R . . . . . .
H83 H 0.7691 0.7830 0.8558 0.1009 1.0000 Uiso R . . . . . .
H91 H 0.6090 0.8690 0.6960 0.0760 1.0000 Uiso R . . . . . .
H92 H 0.7087 0.9044 0.7550 0.0760 1.0000 Uiso R . . . . . .
H93 H 0.6136 0.8591 0.7823 0.0759 1.0000 Uiso R . . . . . .
H101 H 0.9468 0.9214 0.6709 0.0439 1.0000 Uiso R . . . . . .
H111 H 1.0528 0.9534 0.5786 0.0848 1.0000 Uiso R . . . . . .
H112 H 1.0978 0.9919 0.6543 0.0849 1.0000 Uiso R . . . . . .
H113 H 1.1704 0.9312 0.6320 0.0849 1.0000 Uiso R . . . . . .
H123 H 1.0444 0.8548 0.7720 0.0880 1.0000 Uiso R . . . . . .
H122 H 1.0864 0.9295 0.7786 0.0878 1.0000 Uiso R . . . . . .
H121 H 1.1651 0.8748 0.7513 0.0880 1.0000 Uiso R . . . . . .
H131 H 0.7117 0.9250 0.5913 0.0611 1.0000 Uiso R . . . . . .
H143 H 0.8431 0.9641 0.5191 0.1040 1.0000 Uiso R . . . . . .
H142 H 0.7211 1.0011 0.4961 0.1040 1.0000 Uiso R . . . . . .
H141 H 0.7545 0.9431 0.4458 0.1040 1.0000 Uiso R . . . . . .
H151 H 0.5410 0.8703 0.5395 0.1010 1.0000 Uiso R . . . . . .
H152 H 0.5374 0.9418 0.5036 0.1009 1.0000 Uiso R . . . . . .
H153 H 0.5670 0.8792 0.4586 0.1011 1.0000 Uiso R . . . . . .
H161 H 0.8032 0.7936 0.4225 0.0519 1.0000 Uiso R . . . . . .
H171 H 0.8237 0.6770 0.4037 0.0981 1.0000 Uiso R . . . . . .
H172 H 0.9469 0.6915 0.3830 0.0979 1.0000 Uiso R . . . . . .
H173 H 0.8318 0.7198 0.3321 0.0979 1.0000 Uiso R . . . . . .
H181 H 0.9682 0.8611 0.4433 0.1069 1.0000 Uiso R . . . . . .
H182 H 1.0402 0.8045 0.4130 0.1070 1.0000 Uiso R . . . . . .
H183 H 0.9346 0.8389 0.3590 0.1070 1.0000 Uiso R . . . . . .
H191 H 0.5800 0.7588 0.5768 0.0418 1.0000 Uiso R . . . . . .
H201 H 0.6367 0.7490 0.4607 0.0730 1.0000 Uiso R . . . . . .
H202 H 0.5084 0.7216 0.4564 0.0731 1.0000 Uiso R . . . . . .
H203 H 0.6139 0.6714 0.4616 0.0730 1.0000 Uiso R . . . . . .
H211 H 0.5401 0.6672 0.6438 0.0669 1.0000 Uiso R . . . . . .
H212 H 0.4572 0.6627 0.5647 0.0670 1.0000 Uiso R . . . . . .
H213 H 0.5696 0.6174 0.5830 0.0670 1.0000 Uiso R . . . . . .
H221 H 0.6528 0.6481 0.7789 0.0700 1.0000 Uiso R . . . . . .
H231 H 0.8380 0.6414 0.8567 0.1310 1.0000 Uiso R . . . . . .
H232 H 0.7434 0.6021 0.8910 0.1309 1.0000 Uiso R . . . . . .
H233 H 0.8321 0.5626 0.8517 0.1310 1.0000 Uiso R . . . . . .
H243 H 0.5713 0.5546 0.7122 0.1220 1.0000 Uiso R . . . . . .
H242 H 0.5734 0.5463 0.7985 0.1220 1.0000 Uiso R . . . . . .
H241 H 0.6672 0.5090 0.7614 0.1220 1.0000 Uiso R . . . . . .
H251 H 0.8401 0.4978 0.5162 0.0469 1.0000 Uiso R . . . . . .
H263 H 0.7621 0.4466 0.6096 0.0960 1.0000 Uiso R . . . . . .
H262 H 0.6355 0.4729 0.5740 0.0959 1.0000 Uiso R . . . . . .
H261 H 0.6971 0.4195 0.5313 0.0960 1.0000 Uiso R . . . . . .
H271 H 0.7243 0.5675 0.4280 0.0810 1.0000 Uiso R . . . . . .
H272 H 0.6106 0.5444 0.4565 0.0809 1.0000 Uiso R . . . . . .
H273 H 0.6812 0.4926 0.4173 0.0810 1.0000 Uiso R . . . . . .
H5 H 1.0652 0.8157 0.6358 0.0469 1.0000 Uiso R . . . . . .
H7 H 0.9529 0.7195 0.5123 0.0572 1.0000 Uiso R . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.7334(16)
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 . 1.507(12) yes
C1 . C3 . 1.501(11) yes
C1 . O1 . 1.393(8) yes
C1 . H11 . 0.979 no
C2 . H23 . 0.964 no
C2 . H22 . 0.963 no
C2 . H21 . 0.964 no
C3 . H31 . 0.963 no
C3 . H32 . 0.963 no
C3 . H33 . 0.965 no
C4 . C5 . 1.502(10) yes
C4 . C6 . 1.497(10) yes
C4 . O2 . 1.449(7) yes
C4 . H41 . 0.981 no
C5 . H51 . 0.961 no
C5 . H52 . 0.961 no
C5 . H53 . 0.962 no
C6 . H61 . 0.959 no
C6 . H62 . 0.960 no
C6 . H63 . 0.961 no
C7 . C8 . 1.497(11) yes
C7 . C9 . 1.496(10) yes
C7 . O4 . 1.405(8) yes
C7 . H71 . 0.980 no
C8 . H81 . 0.960 no
C8 . H82 . 0.961 no
C8 . H83 . 0.959 no
C9 . H91 . 0.963 no
C9 . H92 . 0.963 no
C9 . H93 . 0.960 no
C10 . C11 . 1.502(10) yes
C10 . C12 . 1.500(11) yes
C10 . O5 . 1.453(7) yes
C10 . H101 . 0.979 no
C11 . H111 . 0.961 no
C11 . H112 . 0.961 no
C11 . H113 . 0.960 no
C12 . H123 . 0.959 no
C12 . H122 . 0.958 no
C12 . H121 . 0.959 no
C13 . C14 . 1.493(12) yes
C13 . C15 . 1.495(12) yes
C13 . O6 . 1.406(8) yes
C13 . H131 . 0.987 no
C14 . H143 . 0.962 no
C14 . H142 . 0.961 no
C14 . H141 . 0.961 no
C15 . H151 . 0.960 no
C15 . H152 . 0.958 no
C15 . H153 . 0.960 no
C16 . C17 . 1.506(11) yes
C16 . C18 . 1.481(11) yes
C16 . O7 . 1.436(8) yes
C16 . H161 . 0.977 no
C17 . H171 . 0.961 no
C17 . H172 . 0.961 no
C17 . H173 . 0.960 no
C18 . H181 . 0.959 no
C18 . H182 . 0.960 no
C18 . H183 . 0.960 no
C19 . C20 . 1.504(10) yes
C19 . C21 . 1.513(10) yes
C19 . O8 . 1.447(7) yes
C19 . H191 . 0.979 no
C20 . H201 . 0.958 no
C20 . H202 . 0.960 no
C20 . H203 . 0.957 no
C21 . H211 . 0.960 no
C21 . H212 . 0.959 no
C21 . H213 . 0.960 no
C22 . C23 . 1.499(14) yes
C22 . C24 . 1.486(13) yes
C22 . O9 . 1.396(9) yes
C22 . H221 . 0.986 no
C23 . H231 . 0.959 no
C23 . H232 . 0.961 no
C23 . H233 . 0.960 no
C24 . H243 . 0.961 no
C24 . H242 . 0.961 no
C24 . H241 . 0.961 no
C25 . C26 . 1.493(11) yes
C25 . C27 . 1.505(10) yes
C25 . O10 . 1.416(7) yes
C25 . H251 . 0.982 no
C26 . H263 . 0.959 no
C26 . H262 . 0.961 no
C26 . H261 . 0.959 no
C27 . H271 . 0.962 no
C27 . H272 . 0.963 no
C27 . H273 . 0.960 no
O1 . Sn1 . 2.044(5) yes
O2 . Sn1 . 2.103(4) yes
O2 . Ti2 . 2.025(4) yes
O3 . Sn1 . 2.054(4) yes
O3 . Ti2 . 1.935(4) yes
O3 . Ti1 . 1.985(4) yes
O4 . Ti1 . 1.787(5) yes
O5 . Ti1 . 2.064(4) yes
O5 . H5 . 0.819 no
O6 . Ti1 . 1.799(4) yes
O7 . Ti1 . 2.156(5) yes
O7 . H7 . 0.827 no
O8 . Ti2 . 2.007(4) yes
O8 . Ti1 . 2.002(4) yes
O9 . Ti2 . 1.750(5) yes
O10 . Ti2 . 1.763(5) yes
Sn1 . Cl3 . 2.4546(16) yes
Sn1 . Cl2 . 2.3809(16) yes
Sn1 . Cl1 . 2.3857(17) 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 . C3 . 112.4(8) yes
C2 . C1 . O1 . 111.3(6) yes
C3 . C1 . O1 . 109.5(6) yes
C2 . C1 . H11 . 107.9 no
C3 . C1 . H11 . 107.8 no
O1 . C1 . H11 . 107.9 no
C1 . C2 . H23 . 109.1 no
C1 . C2 . H22 . 109.7 no
H23 . C2 . H22 . 109.3 no
C1 . C2 . H21 . 109.7 no
H23 . C2 . H21 . 109.6 no
H22 . C2 . H21 . 109.5 no
C1 . C3 . H31 . 109.8 no
C1 . C3 . H32 . 109.6 no
H31 . C3 . H32 . 109.1 no
C1 . C3 . H33 . 109.7 no
H31 . C3 . H33 . 109.3 no
H32 . C3 . H33 . 109.4 no
C5 . C4 . C6 . 112.4(6) yes
C5 . C4 . O2 . 111.3(6) yes
C6 . C4 . O2 . 110.9(5) yes
C5 . C4 . H41 . 107.2 no
C6 . C4 . H41 . 107.9 no
O2 . C4 . H41 . 106.7 no
C4 . C5 . H51 . 109.9 no
C4 . C5 . H52 . 110.0 no
H51 . C5 . H52 . 108.9 no
C4 . C5 . H53 . 109.4 no
H51 . C5 . H53 . 109.4 no
H52 . C5 . H53 . 109.3 no
C4 . C6 . H61 . 109.8 no
C4 . C6 . H62 . 109.5 no
H61 . C6 . H62 . 109.5 no
C4 . C6 . H63 . 108.9 no
H61 . C6 . H63 . 109.4 no
H62 . C6 . H63 . 109.8 no
C8 . C7 . C9 . 111.7(7) yes
C8 . C7 . O4 . 109.7(6) yes
C9 . C7 . O4 . 107.9(6) yes
C8 . C7 . H71 . 109.6 no
C9 . C7 . H71 . 108.9 no
O4 . C7 . H71 . 109.0 no
C7 . C8 . H81 . 109.4 no
C7 . C8 . H82 . 109.1 no
H81 . C8 . H82 . 109.5 no
C7 . C8 . H83 . 109.5 no
H81 . C8 . H83 . 109.7 no
H82 . C8 . H83 . 109.6 no
C7 . C9 . H91 . 109.5 no
C7 . C9 . H92 . 109.2 no
H91 . C9 . H92 . 109.8 no
C7 . C9 . H93 . 109.2 no
H91 . C9 . H93 . 109.4 no
H92 . C9 . H93 . 109.8 no
C11 . C10 . C12 . 112.5(7) yes
C11 . C10 . O5 . 109.4(6) yes
C12 . C10 . O5 . 110.2(6) yes
C11 . C10 . H101 . 108.7 no
C12 . C10 . H101 . 108.4 no
O5 . C10 . H101 . 107.7 no
C10 . C11 . H111 . 109.8 no
C10 . C11 . H112 . 109.0 no
H111 . C11 . H112 . 109.6 no
C10 . C11 . H113 . 109.4 no
H111 . C11 . H113 . 109.6 no
H112 . C11 . H113 . 109.4 no
C10 . C12 . H123 . 110.2 no
C10 . C12 . H122 . 109.7 no
H123 . C12 . H122 . 108.9 no
C10 . C12 . H121 . 109.9 no
H123 . C12 . H121 . 109.2 no
H122 . C12 . H121 . 108.9 no
C14 . C13 . C15 . 112.2(7) yes
C14 . C13 . O6 . 110.1(7) yes
C15 . C13 . O6 . 111.3(7) yes
C14 . C13 . H131 . 107.9 no
C15 . C13 . H131 . 107.4 no
O6 . C13 . H131 . 107.7 no
C13 . C14 . H143 . 110.4 no
C13 . C14 . H142 . 109.7 no
H143 . C14 . H142 . 109.5 no
C13 . C14 . H141 . 109.1 no
H143 . C14 . H141 . 109.2 no
H142 . C14 . H141 . 109.0 no
C13 . C15 . H151 . 110.1 no
C13 . C15 . H152 . 109.7 no
H151 . C15 . H152 . 108.9 no
C13 . C15 . H153 . 109.5 no
H151 . C15 . H153 . 109.4 no
H152 . C15 . H153 . 109.3 no
C17 . C16 . C18 . 115.0(8) yes
C17 . C16 . O7 . 108.4(6) yes
C18 . C16 . O7 . 112.1(7) yes
C17 . C16 . H161 . 107.7 no
C18 . C16 . H161 . 106.9 no
O7 . C16 . H161 . 106.3 no
C16 . C17 . H171 . 109.4 no
C16 . C17 . H172 . 109.2 no
H171 . C17 . H172 . 109.3 no
C16 . C17 . H173 . 109.7 no
H171 . C17 . H173 . 109.9 no
H172 . C17 . H173 . 109.3 no
C16 . C18 . H181 . 109.6 no
C16 . C18 . H182 . 109.8 no
H181 . C18 . H182 . 109.2 no
C16 . C18 . H183 . 109.5 no
H181 . C18 . H183 . 109.6 no
H182 . C18 . H183 . 109.2 no
C20 . C19 . C21 . 112.1(6) yes
C20 . C19 . O8 . 109.8(5) yes
C21 . C19 . O8 . 110.9(5) yes
C20 . C19 . H191 . 108.2 no
C21 . C19 . H191 . 107.8 no
O8 . C19 . H191 . 108.0 no
C19 . C20 . H201 . 110.0 no
C19 . C20 . H202 . 109.1 no
H201 . C20 . H202 . 109.6 no
C19 . C20 . H203 . 109.2 no
H201 . C20 . H203 . 109.7 no
H202 . C20 . H203 . 109.2 no
C19 . C21 . H211 . 110.1 no
C19 . C21 . H212 . 109.1 no
H211 . C21 . H212 . 109.2 no
C19 . C21 . H213 . 109.9 no
H211 . C21 . H213 . 109.6 no
H212 . C21 . H213 . 108.9 no
C23 . C22 . C24 . 113.5(9) yes
C23 . C22 . O9 . 109.5(8) yes
C24 . C22 . O9 . 111.3(8) yes
C23 . C22 . H221 . 107.3 no
C24 . C22 . H221 . 107.3 no
O9 . C22 . H221 . 107.6 no
C22 . C23 . H231 . 109.1 no
C22 . C23 . H232 . 109.8 no
H231 . C23 . H232 . 109.5 no
C22 . C23 . H233 . 109.0 no
H231 . C23 . H233 . 109.8 no
H232 . C23 . H233 . 109.5 no
C22 . C24 . H243 . 109.6 no
C22 . C24 . H242 . 109.5 no
H243 . C24 . H242 . 109.8 no
C22 . C24 . H241 . 109.1 no
H243 . C24 . H241 . 109.3 no
H242 . C24 . H241 . 109.5 no
C26 . C25 . C27 . 112.4(7) yes
C26 . C25 . O10 . 109.4(6) yes
C27 . C25 . O10 . 110.0(6) yes
C26 . C25 . H251 . 108.6 no
C27 . C25 . H251 . 107.8 no
O10 . C25 . H251 . 108.5 no
C25 . C26 . H263 . 109.8 no
C25 . C26 . H262 . 109.6 no
H263 . C26 . H262 . 109.5 no
C25 . C26 . H261 . 109.0 no
H263 . C26 . H261 . 109.7 no
H262 . C26 . H261 . 109.2 no
C25 . C27 . H271 . 109.4 no
C25 . C27 . H272 . 109.7 no
H271 . C27 . H272 . 109.4 no
C25 . C27 . H273 . 109.5 no
H271 . C27 . H273 . 109.5 no
H272 . C27 . H273 . 109.3 no
C1 . O1 . Sn1 . 122.4(4) yes
C4 . O2 . Sn1 . 133.5(4) yes
C4 . O2 . Ti2 . 123.9(4) yes
Sn1 . O2 . Ti2 . 102.65(18) yes
Sn1 . O3 . Ti2 . 107.74(19) yes
Sn1 . O3 . Ti1 . 145.3(2) yes
Ti2 . O3 . Ti1 . 106.76(18) yes
C7 . O4 . Ti1 . 146.6(4) yes
C10 . O5 . Ti1 . 125.9(4) yes
C10 . O5 . H5 . 111.4 no
Ti1 . O5 . H5 . 115.7 no
C13 . O6 . Ti1 . 144.5(5) yes
C16 . O7 . Ti1 . 133.0(4) yes
C16 . O7 . H7 . 110.3 no
Ti1 . O7 . H7 . 115.6 no
C19 . O8 . Ti2 . 131.6(4) yes
C19 . O8 . Ti1 . 125.0(4) yes
Ti2 . O8 . Ti1 . 103.42(18) yes
C22 . O9 . Ti2 . 173.8(5) yes
C25 . O10 . Ti2 . 167.0(5) yes
O2 . Sn1 . O3 . 72.52(16) yes
O2 . Sn1 . O1 . 161.71(18) yes
O3 . Sn1 . O1 . 89.48(18) yes
O2 . Sn1 . Cl3 . 86.53(13) yes
O3 . Sn1 . Cl3 . 87.14(12) yes
O1 . Sn1 . Cl3 . 89.41(14) yes
O2 . Sn1 . Cl2 . 90.33(13) yes
O3 . Sn1 . Cl2 . 89.79(12) yes
O1 . Sn1 . Cl2 . 92.89(14) yes
Cl3 . Sn1 . Cl2 . 176.15(6) yes
O2 . Sn1 . Cl1 . 100.32(12) yes
O3 . Sn1 . Cl1 . 172.56(12) yes
O1 . Sn1 . Cl1 . 97.53(15) yes
Cl3 . Sn1 . Cl1 . 90.43(6) yes
Cl2 . Sn1 . Cl1 . 92.33(6) yes
O2 . Ti2 . O8 . 151.59(17) yes
O2 . Ti2 . O3 . 76.75(16) yes
O8 . Ti2 . O3 . 75.16(16) yes
O2 . Ti2 . O10 . 96.0(2) yes
O8 . Ti2 . O10 . 98.6(2) yes
O3 . Ti2 . O10 . 129.8(2) yes
O2 . Ti2 . O9 . 97.3(2) yes
O8 . Ti2 . O9 . 100.2(2) yes
O3 . Ti2 . O9 . 119.8(2) yes
O10 . Ti2 . O9 . 110.4(3) yes
O7 . Ti1 . O5 . 84.02(18) yes
O7 . Ti1 . O8 . 91.21(18) yes
O5 . Ti1 . O8 . 161.26(17) yes
O7 . Ti1 . O3 . 77.98(17) yes
O5 . Ti1 . O3 . 87.09(17) yes
O8 . Ti1 . O3 . 74.18(16) yes
O7 . Ti1 . O6 . 84.1(2) yes
O5 . Ti1 . O6 . 96.9(2) yes
O8 . Ti1 . O6 . 100.6(2) yes
O3 . Ti1 . O6 . 161.1(2) yes
O7 . Ti1 . O4 . 175.0(2) yes
O5 . Ti1 . O4 . 91.04(19) yes
O8 . Ti1 . O4 . 93.3(2) yes
O3 . Ti1 . O4 . 101.1(2) yes
O6 . Ti1 . O4 . 97.3(2) 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
O5 . H5 . O1 . 170 0.82 1.75 2.566(12) yes
####################################################################### 
# 
# 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_SMR226b
_database_code_depnum_ccdc_archive 'CCDC 759077'
_audit_update_record             
;
2009-12-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'SMR226b.cif'

_audit_creation_date             09-11-20
_audit_creation_method           CRYSTALS_ver_12.87

_oxford_structure_analysis_title 'smr226b in P n m a'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   19.382(2)
_cell_length_b                   14.234(2)
_cell_length_c                   9.515(1)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2625.0(5)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P n m a '
_symmetry_space_group_name_Hall  '-P 2ac 2n'
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
x,-y+1/2,z
-x,y+1/2,-z
-x+1/2,-y,z+1/2
x+1/2,y,-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'
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'
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'
Nb -2.0727 0.6215 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957
3.7559 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C9 H12 Cl6 Nb0.75 O4.50 Sn0.75
# Dc = 2.85 Fooo = 1296.00 Mu = 33.39 M = 563.60
# Found Formula = C7.50 H17.50 Cl2 Nb0.50 O2.50 Sn0.50
# Dc = 1.64 FOOO = 1296.00 Mu = 18.15 M = 324.42

_chemical_formula_sum            'C15 H35 Cl4 Nb O5 Sn '
_chemical_formula_moiety         'C15 H35 Cl4 Nb O5 Sn '
_chemical_compound_source        ?
_chemical_formula_weight         648.85


_cell_measurement_reflns_used    5366
_cell_measurement_theta_min      3.5425
_cell_measurement_theta_max      29.4874
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.1889
_exptl_crystal_size_mid          0.1430
_exptl_crystal_size_min          0.0769

_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1296
_exptl_absorpt_coefficient_mu    1.815

# Sheldrick geometric approximatio 1.00 1.00
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            16727
_reflns_number_total             3411
_diffrn_reflns_av_R_equivalents  0.063
# Number of reflections without Friedels Law is 5809
# Number of reflections with Friedels Law is 3411
# Theoretical number of reflections is about 3657


_diffrn_reflns_theta_min         3.552
_diffrn_reflns_theta_max         29.499
_diffrn_measured_fraction_theta_max 0.899

_diffrn_reflns_theta_full        26.254
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              0
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -3.52
_refine_diff_density_max         2.57


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


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         3411
_refine_ls_number_restraints     1
_refine_ls_number_parameters     137
_oxford_refine_ls_R_factor_ref   0.0793
_refine_ls_wR_factor_ref         0.1069
_refine_ls_goodness_of_fit_ref   1.0476
_refine_ls_shift/su_max          0.0020789


# The values computed from all data
_oxford_reflns_number_all        3411
_refine_ls_R_factor_all          0.0793
_refine_ls_wR_factor_all         0.1069

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2012
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_gt          0.0623

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
78.3 94.6 36.8 4.64
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
O3 O 0.4302(3) 0.2500 0.4845(7) 0.0262 1.0000 Uani S T . . . . .
C2 C 0.2833(5) 0.5066(5) 0.5465(8) 0.0427 1.0000 Uani . . . . . . .
H111 H 0.3576 0.5012 0.3120 0.0592 1.0000 Uiso R . . . . . .
C4 C 0.4016(4) 0.4222(5) 0.8219(7) 0.0295 1.0000 Uani . . . . . . .
C5 C 0.4123(4) 0.3787(6) 0.9647(8) 0.0421 1.0000 Uani . . . . . . .
C6 C 0.4625(4) 0.4776(6) 0.7708(9) 0.0457 1.0000 Uani . . . . . . .
C9 C 0.5043(6) 0.250000(10) 0.2839(12) 0.0468 1.0000 Uani S T . . . . .
H123 H 0.3724 0.3425 0.9870 0.0819 1.0000 Uiso R . . . . . .
H231 H 0.3249 0.5105 0.6003 0.0587 1.0000 Uiso R . . . . . .
Sn1 Sn 0.20310(3) 0.2500 0.50223(8) 0.0246 1.0000 Uani S T . . . . .
Nb1 Nb 0.36080(4) 0.2500 0.61347(9) 0.0207 1.0000 Uani S T . . . . .
Cl1 Cl 0.23987(13) 0.2500 0.7587(3) 0.0316 1.0000 Uani S T . . . . .
Cl3 Cl 0.12312(9) 0.12787(14) 0.5395(2) 0.0417 1.0000 Uani . . . . . . .
Cl2 Cl 0.19994(15) 0.2500 0.2550(3) 0.0427 1.0000 Uani S T . . . . .
O2 O 0.3890(2) 0.3479(3) 0.7227(5) 0.0293 1.0000 Uani . . . . . . .
O1 O 0.2907(2) 0.3369(3) 0.5043(5) 0.0231 1.0000 Uani . . . . . . .
H172 H 0.4702 0.5307 0.8331 0.0571 1.0000 Uiso R . . . . . .
H101 H 0.2524 0.4326 0.3745 0.0401 1.0000 Uiso R . . . . . .
H173 H 0.4534 0.4993 0.6766 0.0571 1.0000 Uiso R . . . . . .
H112 H 0.3959 0.4328 0.4145 0.0591 1.0000 Uiso R . . . . . .
H113 H 0.3578 0.3918 0.2814 0.0589 1.0000 Uiso R . . . . . .
H121 H 0.4183 0.4262 1.0344 0.0822 1.0000 Uiso R . . . . . .
H122 H 0.4528 0.3411 0.9576 0.0820 1.0000 Uiso R . . . . . .
H232 H 0.2750 0.5648 0.4975 0.0592 1.0000 Uiso R . . . . . .
C1 C 0.2919(4) 0.4300(5) 0.4394(7) 0.0286 1.0000 Uani . . . . . . .
H171 H 0.5016 0.4366 0.7705 0.0569 1.0000 Uiso R . . . . . .
H233 H 0.2447 0.4921 0.6058 0.0588 1.0000 Uiso R . . . . . .
H102 H 0.5066 0.3418 0.4522 0.0529 0.5000 Uiso R . . . . . .
C3 C 0.3570(4) 0.4397(6) 0.3531(9) 0.0470 1.0000 Uani . . . . . . .
C11 C 0.5499(8) 0.2198(15) 0.5255(18) 0.0636 0.5000 Uani . . . . . . .
C10 C 0.4994(6) 0.2754(11) 0.4399(14) 0.0383 0.5000 Uani . . . . . . .
H91 H 0.4718 0.2862 0.2323 0.0567 0.5000 Uiso R . . . . . .
H92 H 0.5495 0.2629 0.2504 0.0567 0.5000 Uiso R . . . . . .
H93 H 0.4944 0.1851 0.2722 0.0567 0.5000 Uiso R . . . . . .
H114 H 0.5454 0.2377 0.6213 0.0556 0.5000 Uiso R . . . . . .
H115 H 0.5955 0.2324 0.4944 0.0556 0.5000 Uiso R . . . . . .
H116 H 0.5405 0.1546 0.5162 0.0556 0.5000 Uiso R . . . . . .
H41 H 0.3624 0.4621 0.8256 0.0371 1.0000 Uiso R . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.5004(8)
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
O3 . C10 5_555 1.453(13) yes
O3 . Nb1 . 1.820(6) yes
O3 . C10 . 1.453(13) yes
C2 . H231 . 0.957 no
C2 . H232 . 0.964 no
C2 . C1 . 1.502(9) yes
C2 . H233 . 0.959 no
H111 . C3 . 0.959 no
C4 . C5 . 1.507(10) yes
C4 . C6 . 1.501(10) yes
C4 . O2 . 1.438(8) yes
C4 . H41 . 0.950 no
C5 . H123 . 0.953 no
C5 . H121 . 0.955 no
C5 . H122 . 0.953 no
C6 . H172 . 0.971 no
C6 . H173 . 0.965 no
C6 . H171 . 0.958 no
C9 . C10 5_555 1.530(17) yes
C9 . H91 5_555 0.950 no
C9 . H92 5_555 0.950 no
C9 . H93 5_555 0.950 no
C9 . C10 . 1.530(17) yes
C9 . H91 . 0.950 no
C9 . H92 . 0.950 no
C9 . H93 . 0.950 no
Sn1 . O1 5_555 2.100(4) yes
Sn1 . Cl3 5_555 2.3559(19) yes
Sn1 . Cl1 . 2.542(3) yes
Sn1 . Cl3 . 2.3559(19) yes
Sn1 . Cl2 . 2.353(3) yes
Sn1 . O1 . 2.100(4) yes
Nb1 . O1 5_555 2.110(4) yes
Nb1 . O2 5_555 1.822(5) yes
Nb1 . Cl1 . 2.721(3) yes
Nb1 . O2 . 1.822(5) yes
Nb1 . O1 . 2.110(4) yes
O1 . C1 . 1.463(7) yes
H101 . C1 . 0.984 no
H112 . C3 . 0.960 no
H113 . C3 . 0.966 no
C1 . C3 . 1.512(10) yes
H102 . C10 . 0.963 no
C11 . H114 5_555 1.098 no
C11 . H115 5_555 1.155 no
C11 . C10 5_555 1.275(19) yes
C11 . C11 5_555 0.86(4) yes
C11 . C10 . 1.50(2) yes
C11 . H114 . 0.950 no
C11 . H115 . 0.950 no
C11 . H116 . 0.950 no
H91 . H93 5_555 0.710 no
H92 . H92 5_555 0.366 no
H114 . H114 5_555 0.352 no
H115 . H115 5_555 0.502 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
C10 5_555 O3 . Nb1 . 151.6(7) yes
C10 5_555 O3 . C10 . 28.8(13) yes
Nb1 . O3 . C10 . 151.6(7) yes
H231 . C2 . H232 . 110.4 no
H231 . C2 . C1 . 108.2 no
H232 . C2 . C1 . 108.3 no
H231 . C2 . H233 . 110.8 no
H232 . C2 . H233 . 109.8 no
C1 . C2 . H233 . 109.3 no
C5 . C4 . C6 . 113.6(7) yes
C5 . C4 . O2 . 108.3(6) yes
C6 . C4 . O2 . 107.9(6) yes
C5 . C4 . H41 . 108.8 no
C6 . C4 . H41 . 109.0 no
O2 . C4 . H41 . 109.1 no
C4 . C5 . H123 . 108.2 no
C4 . C5 . H121 . 110.6 no
H123 . C5 . H121 . 109.1 no
C4 . C5 . H122 . 106.3 no
H123 . C5 . H122 . 112.4 no
H121 . C5 . H122 . 110.3 no
C4 . C6 . H172 . 109.4 no
C4 . C6 . H173 . 109.0 no
H172 . C6 . H173 . 110.3 no
C4 . C6 . H171 . 107.6 no
H172 . C6 . H171 . 110.7 no
H173 . C6 . H171 . 109.7 no
C10 5_555 C9 . H91 5_555 109.4 no
C10 5_555 C9 . H92 5_555 109.7 no
H91 5_555 C9 . H92 5_555 109.5 no
C10 5_555 C9 . H93 5_555 109.3 no
H91 5_555 C9 . H93 5_555 109.5 no
H92 5_555 C9 . H93 5_555 109.5 no
C10 5_555 C9 . C10 . 27.3(12) yes
H91 5_555 C9 . C10 . 126.0 no
H92 5_555 C9 . C10 . 115.3 no
H93 5_555 C9 . C10 . 82.7 no
C10 5_555 C9 . H91 . 126.0 no
H91 5_555 C9 . H91 . 65.7 no
H92 5_555 C9 . H91 . 122.8 no
H93 5_555 C9 . H91 . 43.9 no
C10 . C9 . H91 . 109.4 no
C10 5_555 C9 . H92 . 115.3 no
H91 5_555 C9 . H92 . 122.8 no
H92 5_555 C9 . H92 . 22.2 no
H93 5_555 C9 . H92 . 87.6 no
C10 . C9 . H92 . 109.7 no
C10 5_555 C9 . H93 . 82.7 no
H91 5_555 C9 . H93 . 43.9 no
H92 5_555 C9 . H93 . 87.6 no
H93 5_555 C9 . H93 . 153.1 no
C10 . C9 . H93 . 109.3 no
H91 . C9 . H92 . 109.5 no
H91 . C9 . H93 . 109.5 no
H92 . C9 . H93 . 109.5 no
O1 5_555 Sn1 . Cl3 5_555 164.75(13) yes
O1 5_555 Sn1 . Cl1 . 76.36(14) yes
Cl3 5_555 Sn1 . Cl1 . 92.30(7) yes
O1 5_555 Sn1 . Cl3 . 95.51(12) yes
Cl3 5_555 Sn1 . Cl3 . 95.10(10) yes
Cl1 . Sn1 . Cl3 . 92.30(8) yes
O1 5_555 Sn1 . Cl2 . 91.75(15) yes
Cl3 5_555 Sn1 . Cl2 . 97.65(8) yes
Cl1 . Sn1 . Cl2 . 165.21(10) yes
Cl3 . Sn1 . Cl2 . 97.65(8) yes
O1 5_555 Sn1 . O1 . 72.1(2) yes
Cl3 5_555 Sn1 . O1 . 95.51(12) yes
Cl1 . Sn1 . O1 . 76.36(15) yes
Cl3 . Sn1 . O1 . 164.75(13) yes
Cl2 . Sn1 . O1 . 91.75(15) yes
O1 5_555 Nb1 . O2 5_555 91.48(19) yes
O1 5_555 Nb1 . O3 . 98.3(2) yes
O2 5_555 Nb1 . O3 . 99.4(2) yes
O1 5_555 Nb1 . Cl1 . 72.25(13) yes
O2 5_555 Nb1 . Cl1 . 88.21(15) yes
O3 . Nb1 . Cl1 . 168.1(2) yes
O1 5_555 Nb1 . O2 . 157.19(19) yes
O2 5_555 Nb1 . O2 . 99.8(3) yes
O3 . Nb1 . O2 . 99.4(2) yes
Cl1 . Nb1 . O2 . 88.21(16) yes
O1 5_555 Nb1 . O1 . 71.7(2) yes
O2 5_555 Nb1 . O1 . 157.19(18) yes
O3 . Nb1 . O1 . 98.3(2) yes
Cl1 . Nb1 . O1 . 72.25(13) yes
O2 . Nb1 . O1 . 91.48(19) yes
Nb1 . Cl1 . Sn1 . 75.76(8) yes
C4 . O2 . Nb1 . 170.9(4) yes
Sn1 . O1 . Nb1 . 100.39(17) yes
Sn1 . O1 . C1 . 122.8(4) yes
Nb1 . O1 . C1 . 136.8(4) yes
C2 . C1 . O1 . 111.7(5) yes
C2 . C1 . H101 . 108.1 no
O1 . C1 . H101 . 106.7 no
C2 . C1 . C3 . 113.3(7) yes
O1 . C1 . C3 . 109.0(6) yes
H101 . C1 . C3 . 107.8 no
C1 . C3 . H113 . 109.4 no
C1 . C3 . H112 . 108.5 no
H113 . C3 . H112 . 110.2 no
C1 . C3 . H111 . 108.4 no
H113 . C3 . H111 . 110.9 no
H112 . C3 . H111 . 109.4 no
H114 5_555 C11 . H115 5_555 87.0 no
H114 5_555 C11 . C10 5_555 116.1 no
H115 5_555 C11 . C10 5_555 113.1 no
H114 5_555 C11 . C11 5_555 56.5 no
H115 5_555 C11 . C11 5_555 53.9 no
C10 5_555 C11 . C11 5_555 86.9(13) yes
H114 5_555 C11 . C10 . 96.2 no
H115 5_555 C11 . C10 . 92.8 no
C10 5_555 C11 . C10 . 28.8(13) yes
C11 5_555 C11 . C10 . 58.1(9) yes
H114 5_555 C11 . H114 . 18.0 no
H115 5_555 C11 . H114 . 99.1 no
C10 5_555 C11 . H114 . 121.9 no
C11 5_555 C11 . H114 . 74.5 no
C10 . C11 . H114 . 108.7 no
H114 5_555 C11 . H115 . 103.2 no
H115 5_555 C11 . H115 . 25.3 no
C10 5_555 C11 . H115 . 120.4 no
C11 5_555 C11 . H115 . 79.1 no
C10 . C11 . H115 . 109.8 no
H114 5_555 C11 . H116 . 127.0 no
H115 5_555 C11 . H116 . 134.3 no
C10 5_555 C11 . H116 . 81.1 no
C11 5_555 C11 . H116 . 167.7 no
C10 . C11 . H116 . 109.9 no
H114 . C11 . H115 . 109.5 no
H114 . C11 . H116 . 109.5 no
H115 . C11 . H116 . 109.5 no
C9 . C10 . C11 . 111.3(12) yes
C9 . C10 . O3 . 106.4(10) yes
C11 . C10 . O3 . 108.2(11) yes
C9 . C10 . H102 . 109.9 no
C11 . C10 . H102 . 110.9 no
O3 . C10 . H102 . 110.0 no
C9 . C10 . C11 5_555 125.8(13) yes
C11 . C10 . C11 5_555 35.0(18) yes
O3 . C10 . C11 5_555 122.3(13) yes
H102 . C10 . C11 5_555 76.0 no
H93 5_555 H91 . C9 . 68.1 no
C9 . H92 . H92 5_555 78.9 no
H91 5_555 H93 . C9 . 68.1 no
C11 5_555 H114 . C11 . 49.0 no
C11 5_555 H114 . H114 5_555 56.5 no
C11 . H114 . H114 5_555 105.5 no
C11 5_555 H115 . H115 5_555 53.9 no
C11 5_555 H115 . C11 . 47.0 no
H115 5_555 H115 . C11 . 100.9 no
####################################################################### 
# 
# 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_SMR227
_database_code_depnum_ccdc_archive 'CCDC 759078'
_audit_update_record             
;
2009-12-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'SMR227.cif'

_audit_creation_date             09-12-01
_audit_creation_method           CRYSTALS_ver_12.87

_oxford_structure_analysis_title 'smr227 in P 1 21/n 1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.9442(7)
_cell_length_b                   14.6160(10)
_cell_length_c                   18.675(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.107(8)
_cell_angle_gamma                90
_cell_volume                     2680.1(4)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Nb -2.0727 0.6215 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957
3.7559 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C20 H48.75 Cl5 Nb1.25 O7.50 Sn1.25
# Dc = 2.11 Fooo = 1368.00 Mu = 22.30 M = 851.11
# Found Formula = C16 H39 Cl4 Nb1 O6 Sn1
# Dc = 1.69 FOOO = 1368.00 Mu = 17.84 M = 680.89

_chemical_formula_sum            'C16 H39 Cl4 Nb1 O6 Sn1'
_chemical_formula_moiety         'C16 H39 Cl4 Nb1 O6 Sn1'
_chemical_compound_source        ?
_chemical_formula_weight         680.89


_cell_measurement_reflns_used    5691
_cell_measurement_theta_min      3.5022
_cell_measurement_theta_max      29.5275
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.254
_exptl_crystal_size_mid          0.406
_exptl_crystal_size_max          0.507

_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1368
_exptl_absorpt_coefficient_mu    1.784

# Sheldrick geometric approximatio 1.00 1.00
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_T_max  0.716
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            13308
_reflns_number_total             6374
_diffrn_reflns_av_R_equivalents  0.033
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 6374
# Theoretical number of reflections is about 14999


_diffrn_reflns_theta_min         3.546
_diffrn_reflns_theta_max         29.544
_diffrn_measured_fraction_theta_max 0.850

_diffrn_reflns_theta_full        26.294
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -2.09
_refine_diff_density_max         2.27


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


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         6374
_refine_ls_number_restraints     0
_refine_ls_number_parameters     253
_oxford_refine_ls_R_factor_ref   0.0836
_refine_ls_wR_factor_ref         0.1838
_refine_ls_goodness_of_fit_ref   1.0282
_refine_ls_shift/su_max          0.0005253
_refine_ls_shift/su_mean         3.6051214


# The values computed from all data
_oxford_reflns_number_all        6374
_refine_ls_R_factor_all          0.0836
_refine_ls_wR_factor_all         0.1838

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4194
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_gt          0.1669

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method= Modified Sheldrick
w=1/[σ²(F²) + ( 0.12P)² + 0.00P]
,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 atomsattached to an atom.

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
C1 C 0.6974(9) 0.3243(5) 0.7515(5) 0.0822 1.0000 Uani . . . . . . .
C2 C 0.7691(10) 0.2829(9) 0.8192(5) 0.1179 1.0000 Uani . . . . . . .
C3 C 0.6308(8) 0.1098(6) 0.5231(4) 0.0732 1.0000 Uani . . . . . . .
C4 C 0.5586(11) 0.1504(9) 0.4550(5) 0.1153 1.0000 Uani . . . . . . .
C5 C 0.6831(13) 0.4438(7) 0.5328(7) 0.1227 1.0000 Uani . . . . . . .
C6 C 0.719(2) 0.5230(8) 0.5707(9) 0.2190 1.0000 Uani . . . . . . .
C7 C 0.700(2) 0.4349(12) 0.4600(8) 0.2360 1.0000 Uani . . . . . . .
C8 C 1.0764(13) 0.3553(11) 0.7027(10) 0.1662 1.0000 Uani . . . . . . .
C9 C 1.1326(16) 0.3576(14) 0.7653(11) 0.2342 1.0000 Uani . . . . . . .
C10 C 1.1009(13) 0.4403(9) 0.6577(10) 0.1577 1.0000 Uani . . . . . . .
C11 C 0.9481(17) 0.2210(11) 0.4741(8) 0.1535 1.0000 Uani . . . . . . .
C12 C 1.0586(14) 0.2827(15) 0.4752(7) 0.1911 1.0000 Uani . . . . . . .
C13 C 0.983(3) 0.1395(17) 0.4487(12) 0.2777 1.0000 Uani . . . . . . .
C14 C 1.0205(9) 0.0948(8) 0.6815(8) 0.1186 1.0000 Uani . . . . . . .
C15 C 1.0552(14) 0.0738(14) 0.7611(10) 0.2068 1.0000 Uani . . . . . . .
C16 C 1.022(2) 0.0074(13) 0.6445(18) 0.2873 1.0000 Uani . . . . . . .
Sn1 Sn 0.51291(3) 0.18128(3) 0.65849(2) 0.0475 1.0000 Uani . . . . . . .
Nb1 Nb 0.81513(5) 0.26060(4) 0.61458(3) 0.0478 1.0000 Uani . . . . . . .
Cl4 Cl 0.63243(18) 0.04475(12) 0.70836(13) 0.0815 1.0000 Uani . . . . . . .
Cl3 Cl 0.33704(19) 0.09010(18) 0.59292(16) 0.1025 1.0000 Uani . . . . . . .
Cl1 Cl 0.41113(18) 0.31832(14) 0.60483(15) 0.0914 1.0000 Uani . . . . . . .
Cl2 Cl 0.4148(2) 0.19976(17) 0.76464(13) 0.0857 1.0000 Uani . . . . . . .
O1 O 0.6906(4) 0.2574(3) 0.6952(2) 0.0446 1.0000 Uani . . . . . . .
O4 O 0.9580(4) 0.3140(3) 0.6728(3) 0.0672 1.0000 Uani . . . . . . .
O5 O 0.8931(5) 0.2259(4) 0.5374(3) 0.0800 1.0000 Uani . . . . . . .
O3 O 0.7316(5) 0.3646(4) 0.5737(4) 0.0889 1.0000 Uani . . . . . . .
O2 O 0.6458(4) 0.1759(3) 0.5810(2) 0.0494 1.0000 Uani . . . . . . .
O6 O 0.8920(4) 0.1329(3) 0.6650(3) 0.0733 1.0000 Uani . . . . . . .
H11 H 0.7469 0.3774 0.7386 0.0910 1.0000 Uiso R . . . . . .
H12 H 0.6058 0.3424 0.7580 0.0910 1.0000 Uiso R . . . . . .
H23 H 0.7732 0.3277 0.8570 0.1730 1.0000 Uiso R . . . . . .
H22 H 0.8600 0.2659 0.8134 0.1729 1.0000 Uiso R . . . . . .
H21 H 0.7219 0.2297 0.8320 0.1730 1.0000 Uiso R . . . . . .
H31 H 0.7216 0.0901 0.5155 0.0889 1.0000 Uiso R . . . . . .
H32 H 0.5796 0.0576 0.5364 0.0890 1.0000 Uiso R . . . . . .
H41 H 0.5549 0.1070 0.4161 0.1799 1.0000 Uiso R . . . . . .
H42 H 0.6077 0.2040 0.4437 0.1799 1.0000 Uiso R . . . . . .
H43 H 0.4677 0.1670 0.4612 0.1799 1.0000 Uiso R . . . . . .
H51 H 0.5839 0.4420 0.5321 0.1582 1.0000 Uiso R . . . . . .
H63 H 0.7018 0.5163 0.6197 0.3019 1.0000 Uiso R . . . . . .
H62 H 0.8143 0.5312 0.5695 0.3020 1.0000 Uiso R . . . . . .
H61 H 0.6677 0.5734 0.5475 0.3020 1.0000 Uiso R . . . . . .
H71 H 0.6817 0.3729 0.4433 0.3051 1.0000 Uiso R . . . . . .
H72 H 0.7916 0.4524 0.4559 0.3050 1.0000 Uiso R . . . . . .
H73 H 0.6354 0.4761 0.4325 0.3051 1.0000 Uiso R . . . . . .
H91 H 1.1435 0.2947 0.7807 0.2841 1.0000 Uiso R . . . . . .
H93 H 1.2181 0.3905 0.7753 0.2841 1.0000 Uiso R . . . . . .
H92 H 1.0623 0.3873 0.7870 0.2841 1.0000 Uiso R . . . . . .
H103 H 1.0744 0.4377 0.6061 0.2630 1.0000 Uiso R . . . . . .
H101 H 1.1960 0.4542 0.6694 0.2631 1.0000 Uiso R . . . . . .
H102 H 1.0482 0.4857 0.6781 0.2631 1.0000 Uiso R . . . . . .
H111 H 0.8748 0.2406 0.4348 0.1641 1.0000 Uiso R . . . . . .
H123 H 1.0371 0.3455 0.4840 0.2669 1.0000 Uiso R . . . . . .
H121 H 1.1259 0.2597 0.5132 0.2671 1.0000 Uiso R . . . . . .
H122 H 1.0916 0.2778 0.4298 0.2671 1.0000 Uiso R . . . . . .
H131 H 0.9123 0.0939 0.4456 0.2971 1.0000 Uiso R . . . . . .
H132 H 1.0565 0.1248 0.4879 0.2971 1.0000 Uiso R . . . . . .
H133 H 1.0181 0.1437 0.4033 0.2972 1.0000 Uiso R . . . . . .
H141 H 1.0887 0.1363 0.6666 0.1472 1.0000 Uiso R . . . . . .
H152 H 1.0604 0.1288 0.7896 0.2809 1.0000 Uiso R . . . . . .
H151 H 1.1411 0.0429 0.7678 0.2810 1.0000 Uiso R . . . . . .
H153 H 0.9866 0.0340 0.7743 0.2810 1.0000 Uiso R . . . . . .
H162 H 0.9760 0.0150 0.5946 0.2970 1.0000 Uiso R . . . . . .
H163 H 1.1149 -0.0126 0.6453 0.2971 1.0000 Uiso R . . . . . .
H161 H 0.9729 -0.0367 0.6696 0.2972 1.0000 Uiso R . . . . . .
H81 H 1.1422 0.3136 0.6850 0.1662 1.0000 Uiso R . . . . . .
H6 H 0.8336 0.1058 0.6833 0.1083 1.0000 Uiso R . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.75(4)
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 . 1.478(14) yes
C1 . O1 . 1.430(8) yes
C1 . H11 . 0.970 no
C1 . H12 . 0.974 no
C2 . H23 . 0.959 no
C2 . H22 . 0.960 no
C2 . H21 . 0.959 no
C3 . C4 . 1.481(12) yes
C3 . O2 . 1.441(8) yes
C3 . H31 . 0.979 no
C3 . H32 . 0.971 no
C4 . H41 . 0.961 no
C4 . H42 . 0.964 no
C4 . H43 . 0.960 no
C5 . C6 . 1.375(17) yes
C5 . C7 . 1.401(18) yes
C5 . O3 . 1.428(10) yes
C5 . H51 . 0.985 no
C6 . H63 . 0.961 no
C6 . H62 . 0.962 no
C6 . H61 . 0.958 no
C7 . H71 . 0.966 no
C7 . H72 . 0.965 no
C7 . H73 . 0.964 no
C8 . C9 . 1.22(2) yes
C8 . C10 . 1.54(2) yes
C8 . O4 . 1.361(11) yes
C8 . H81 . 0.988 no
C9 . H91 . 0.964 no
C9 . H93 . 0.968 no
C9 . H92 . 0.965 no
C10 . H103 . 0.960 no
C10 . H101 . 0.958 no
C10 . H102 . 0.960 no
C11 . C12 . 1.419(19) yes
C11 . C13 . 1.35(2) yes
C11 . O5 . 1.380(11) yes
C11 . H111 . 0.991 no
C12 . H123 . 0.963 no
C12 . H121 . 0.957 no
C12 . H122 . 0.959 no
C13 . H131 . 0.967 no
C13 . H132 . 0.970 no
C13 . H133 . 0.966 no
C14 . C15 . 1.504(19) yes
C14 . C16 . 1.45(3) yes
C14 . O6 . 1.383(9) yes
C14 . H141 . 0.983 no
C15 . H152 . 0.961 no
C15 . H151 . 0.956 no
C15 . H153 . 0.957 no
C16 . H162 . 0.975 no
C16 . H163 . 0.971 no
C16 . H161 . 0.970 no
Sn1 . Nb1 . 3.4393(6) yes
Sn1 . Cl4 . 2.4315(17) yes
Sn1 . Cl3 . 2.378(2) yes
Sn1 . Cl1 . 2.3915(18) yes
Sn1 . Cl2 . 2.359(2) yes
Sn1 . O1 . 2.109(4) yes
Sn1 . O2 . 2.109(4) yes
Nb1 . O1 . 2.095(4) yes
Nb1 . O4 . 1.822(4) yes
Nb1 . O5 . 1.814(5) yes
Nb1 . O3 . 1.839(5) yes
Nb1 . O2 . 2.104(4) yes
Nb1 . O6 . 2.174(4) yes
O6 . H6 . 0.822 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . O1 . 108.0(7) yes
C2 . C1 . H11 . 110.2 no
O1 . C1 . H11 . 109.3 no
C2 . C1 . H12 . 109.8 no
O1 . C1 . H12 . 109.9 no
H11 . C1 . H12 . 109.6 no
C1 . C2 . H23 . 108.0 no
C1 . C2 . H22 . 110.2 no
H23 . C2 . H22 . 109.2 no
C1 . C2 . H21 . 110.9 no
H23 . C2 . H21 . 109.6 no
H22 . C2 . H21 . 109.0 no
C4 . C3 . O2 . 110.8(8) yes
C4 . C3 . H31 . 109.1 no
O2 . C3 . H31 . 108.6 no
C4 . C3 . H32 . 109.4 no
O2 . C3 . H32 . 109.3 no
H31 . C3 . H32 . 109.7 no
C3 . C4 . H41 . 109.9 no
C3 . C4 . H42 . 108.6 no
H41 . C4 . H42 . 109.3 no
C3 . C4 . H43 . 109.6 no
H41 . C4 . H43 . 109.5 no
H42 . C4 . H43 . 109.9 no
C6 . C5 . C7 . 121.1(13) yes
C6 . C5 . O3 . 111.7(11) yes
C7 . C5 . O3 . 111.3(11) yes
C6 . C5 . H51 . 101.8 no
C7 . C5 . H51 . 104.8 no
O3 . C5 . H51 . 103.8 no
C5 . C6 . H63 . 109.5 no
C5 . C6 . H62 . 105.5 no
H63 . C6 . H62 . 110.9 no
C5 . C6 . H61 . 109.9 no
H63 . C6 . H61 . 110.6 no
H62 . C6 . H61 . 110.4 no
C5 . C7 . H71 . 110.9 no
C5 . C7 . H72 . 108.1 no
H71 . C7 . H72 . 110.6 no
C5 . C7 . H73 . 106.9 no
H71 . C7 . H73 . 109.9 no
H72 . C7 . H73 . 110.4 no
C9 . C8 . C10 . 114.5(16) yes
C9 . C8 . O4 . 130.0(19) yes
C10 . C8 . O4 . 109.6(12) yes
C9 . C8 . H81 . 96.3 no
C10 . C8 . H81 . 98.3 no
O4 . C8 . H81 . 99.5 no
C8 . C9 . H91 . 105.9 no
C8 . C9 . H93 . 117.1 no
H91 . C9 . H93 . 111.3 no
C8 . C9 . H92 . 99.3 no
H91 . C9 . H92 . 111.0 no
H93 . C9 . H92 . 111.6 no
C8 . C10 . H103 . 118.3 no
C8 . C10 . H101 . 106.4 no
H103 . C10 . H101 . 110.0 no
C8 . C10 . H102 . 101.4 no
H103 . C10 . H102 . 110.2 no
H101 . C10 . H102 . 110.1 no
C12 . C11 . C13 . 108.7(16) yes
C12 . C11 . O5 . 111.5(11) yes
C13 . C11 . O5 . 120.5(15) yes
C12 . C11 . H111 . 107.7 no
C13 . C11 . H111 . 101.3 no
O5 . C11 . H111 . 106.0 no
C11 . C12 . H123 . 114.6 no
C11 . C12 . H121 . 103.6 no
H123 . C12 . H121 . 110.8 no
C11 . C12 . H122 . 108.3 no
H123 . C12 . H122 . 109.8 no
H121 . C12 . H122 . 109.5 no
C11 . C13 . H131 . 113.6 no
C11 . C13 . H132 . 97.8 no
H131 . C13 . H132 . 110.3 no
C11 . C13 . H133 . 113.7 no
H131 . C13 . H133 . 110.5 no
H132 . C13 . H133 . 110.3 no
C15 . C14 . C16 . 105.8(14) yes
C15 . C14 . O6 . 111.3(10) yes
C16 . C14 . O6 . 108.9(13) yes
C15 . C14 . H141 . 110.2 no
C16 . C14 . H141 . 110.5 no
O6 . C14 . H141 . 110.0 no
C14 . C15 . H152 . 111.1 no
C14 . C15 . H151 . 106.6 no
H152 . C15 . H151 . 110.7 no
C14 . C15 . H153 . 108.4 no
H152 . C15 . H153 . 110.2 no
H151 . C15 . H153 . 109.8 no
C14 . C16 . H162 . 108.5 no
C14 . C16 . H163 . 109.7 no
H162 . C16 . H163 . 110.3 no
C14 . C16 . H161 . 108.2 no
H162 . C16 . H161 . 110.2 no
H163 . C16 . H161 . 109.9 no
Nb1 . Sn1 . Cl4 . 88.59(4) yes
Nb1 . Sn1 . Cl3 . 131.70(7) yes
Cl4 . Sn1 . Cl3 . 90.71(9) yes
Nb1 . Sn1 . Cl1 . 86.88(5) yes
Cl4 . Sn1 . Cl1 . 175.33(6) yes
Cl3 . Sn1 . Cl1 . 91.47(9) yes
Nb1 . Sn1 . Cl2 . 130.91(6) yes
Cl4 . Sn1 . Cl2 . 90.81(8) yes
Cl3 . Sn1 . Cl2 . 97.39(8) yes
Cl1 . Sn1 . Cl2 . 93.00(9) yes
Nb1 . Sn1 . O1 . 34.98(11) yes
Cl4 . Sn1 . O1 . 88.56(12) yes
Cl3 . Sn1 . O1 . 166.67(12) yes
Cl1 . Sn1 . O1 . 88.37(12) yes
Cl2 . Sn1 . O1 . 95.92(12) yes
Nb1 . Sn1 . O2 . 35.24(11) yes
Cl4 . Sn1 . O2 . 84.88(12) yes
Cl3 . Sn1 . O2 . 96.63(13) yes
Cl1 . Sn1 . O2 . 90.76(12) yes
Cl2 . Sn1 . O2 . 165.38(13) yes
O1 . Sn1 . O2 . 70.05(15) yes
Sn1 . Nb1 . O1 . 35.24(10) yes
Sn1 . Nb1 . O4 . 129.06(16) yes
O1 . Nb1 . O4 . 94.25(19) yes
Sn1 . Nb1 . O5 . 126.52(17) yes
O1 . Nb1 . O5 . 160.1(2) yes
O4 . Nb1 . O5 . 101.7(2) yes
Sn1 . Nb1 . O3 . 91.32(16) yes
O1 . Nb1 . O3 . 92.1(2) yes
O4 . Nb1 . O3 . 98.8(2) yes
O5 . Nb1 . O3 . 97.1(3) yes
Sn1 . Nb1 . O2 . 35.33(12) yes
O1 . Nb1 . O2 . 70.40(16) yes
O4 . Nb1 . O2 . 160.2(2) yes
O5 . Nb1 . O2 . 91.3(2) yes
O3 . Nb1 . O2 . 94.3(2) yes
Sn1 . Nb1 . O6 . 82.42(12) yes
O1 . Nb1 . O6 . 82.96(17) yes
O4 . Nb1 . O6 . 85.5(2) yes
O5 . Nb1 . O6 . 86.5(2) yes
O3 . Nb1 . O6 . 173.73(19) yes
O2 . Nb1 . O6 . 80.43(17) yes
C1 . O1 . Sn1 . 122.6(4) yes
C1 . O1 . Nb1 . 123.3(4) yes
Sn1 . O1 . Nb1 . 109.78(17) yes
C8 . O4 . Nb1 . 167.5(9) yes
C11 . O5 . Nb1 . 166.4(8) yes
C5 . O3 . Nb1 . 169.7(7) yes
C3 . O2 . Sn1 . 122.6(4) yes
C3 . O2 . Nb1 . 126.9(4) yes
Sn1 . O2 . Nb1 . 109.44(18) yes
C14 . O6 . Nb1 . 133.8(5) yes
C14 . O6 . H6 . 113.7 no
Nb1 . O6 . H6 . 111.8 no


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

data_1
_database_code_depnum_ccdc_archive 'CCDC 772661'
_audit_update_record             
;
2010-04-09 deposited with the CCDC.
2015-03-02 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.
;
_refine_special_details          
;
?
;
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a                   10.3378(8)
_cell_length_b                   11.3589(8)
_cell_length_c                   19.9780(10)
_cell_angle_alpha                88.599(6)
_cell_angle_beta                 75.838(6)
_cell_angle_gamma                66.319(7)
_cell_volume                     2075.9(3)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
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'
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'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C24 H56 Cl4 O8 Sn1 Ti2
# Dc = 1.33 Fooo = 904.00 Mu = 12.63 M = 829.00
# Found Formula = C27 H65 Cl3 O10 Sn1 Ti2
# Dc = 1.39 FOOO = 904.00 Mu = 12.08 M = 870.65

_chemical_formula_sum            'C27 H65 Cl3 O10 Sn1 Ti2'
_chemical_formula_moiety         'C27 H65 Cl3 O10 Sn1 Ti2'
_chemical_compound_source        ?
_chemical_formula_weight         870.65


_cell_measurement_reflns_used    8961
_cell_measurement_theta_min      3.3730
_cell_measurement_theta_max      29.4903
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.205
_exptl_crystal_size_mid          0.429
_exptl_crystal_size_max          0.560

_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    1.208

# Sheldrick geometric approximatio 0.60 0.78
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_detector_area_resol_mean 10.4685

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            17109
_reflns_number_total             9701
_diffrn_reflns_av_R_equivalents  0.045
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 9701
# Theoretical number of reflections is about 23256


_diffrn_reflns_theta_min         3.380
_diffrn_reflns_theta_max         29.554
_diffrn_measured_fraction_theta_max 0.833

_diffrn_reflns_theta_full        26.303
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -15
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              27

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -2.17
_refine_diff_density_max         2.21


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


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         9701
_refine_ls_number_restraints     0
_refine_ls_number_parameters     388
_oxford_refine_ls_R_factor_ref   0.0657
_refine_ls_wR_factor_ref         0.1195
_refine_ls_goodness_of_fit_ref   1.0041
_refine_ls_shift/su_max          0.0004838
_refine_ls_shift/su_mean         0.0000517


# The values computed from all data
_oxford_reflns_number_all        9701
_refine_ls_R_factor_all          0.0657
_refine_ls_wR_factor_all         0.1195

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7833
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_gt          0.1001

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
0.222E+04 0.336E+04 0.179E+04 507.
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
C1 C 0.4479(6) 0.6611(5) 0.7003(3) 0.0307 1.0000 Uani . . . . . . .
C2 C 0.3308(8) 0.6906(6) 0.6615(4) 0.0507 1.0000 Uani . . . . . . .
C3 C 0.5596(8) 0.7140(6) 0.6678(4) 0.0519 1.0000 Uani . . . . . . .
C4 C 0.4009(5) 0.2920(5) 0.9280(2) 0.0250 1.0000 Uani . . . . . . .
C5 C 0.3547(6) 0.4031(5) 0.9804(3) 0.0324 1.0000 Uani . . . . . . .
C6 C 0.2707(6) 0.2783(6) 0.9117(3) 0.0382 1.0000 Uani . . . . . . .
C7 C 0.7575(6) 0.2344(5) 0.9784(3) 0.0328 1.0000 Uani . . . . . . .
C8 C 0.7173(8) 0.1464(8) 1.0284(3) 0.0549 1.0000 Uani . . . . . . .
C9 C 0.9063(7) 0.2307(7) 0.9766(3) 0.0479 1.0000 Uani . . . . . . .
C10 C 0.6800(8) -0.0812(6) 0.8369(3) 0.0450 1.0000 Uani . . . . . . .
C11 C 0.5421(10) -0.0752(8) 0.8235(5) 0.0708 1.0000 Uani . . . . . . .
C12 C 0.7011(9) -0.1260(8) 0.9061(4) 0.0671 1.0000 Uani . . . . . . .
C13 C 1.0545(5) 0.0348(5) 0.7685(3) 0.0300 1.0000 Uani . . . . . . .
C14 C 1.1427(6) 0.0973(6) 0.7906(3) 0.0445 1.0000 Uani . . . . . . .
C15 C 1.0397(7) -0.0702(6) 0.8139(3) 0.0448 1.0000 Uani . . . . . . .
C16 C 0.8530(8) -0.0134(6) 0.6453(3) 0.0468 1.0000 Uani . . . . . . .
C17 C 0.7105(8) -0.0011(8) 0.6350(5) 0.0691 1.0000 Uani . . . . . . .
C18 C 0.9814(8) -0.1117(6) 0.5947(4) 0.0573 1.0000 Uani . . . . . . .
C19 C 1.1680(7) 0.1545(6) 0.5827(3) 0.0441 1.0000 Uani . . . . . . .
C20 C 1.1897(9) 0.2528(8) 0.5357(4) 0.0774 1.0000 Uani . . . . . . .
C21 C 1.3047(8) 0.0719(9) 0.6023(5) 0.0805 1.0000 Uani . . . . . . .
C22 C 0.7580(7) 0.3403(6) 0.5550(3) 0.0373 1.0000 Uani . . . . . . .
C23 C 0.6193(8) 0.3243(8) 0.5556(4) 0.0563 1.0000 Uani . . . . . . .
C24 C 0.7758(9) 0.4438(7) 0.5100(3) 0.0570 1.0000 Uani . . . . . . .
C25 C 0.9743(6) 0.4505(6) 0.7387(3) 0.0391 1.0000 Uani . . . . . . .
C26 C 0.9578(9) 0.4916(10) 0.8128(5) 0.0799 1.0000 Uani . . . . . . .
C27 C 0.9657(9) 0.5536(8) 0.6906(5) 0.0805 1.0000 Uani . . . . . . .
O1 O 0.6793(3) 0.2933(3) 0.75745(16) 0.0207 1.0000 Uani . . . . . . .
O2 O 0.5197(4) 0.5266(3) 0.70266(17) 0.0271 1.0000 Uani . . . . . . .
O3 O 0.4988(3) 0.3029(3) 0.86458(16) 0.0219 1.0000 Uani . . . . . . .
O4 O 0.7551(4) 0.2005(4) 0.91062(18) 0.0331 1.0000 Uani . . . . . . .
O5 O 0.6885(4) 0.0388(3) 0.8280(2) 0.0345 1.0000 Uani . . . . . . .
O6 O 0.9115(3) 0.1332(3) 0.76756(17) 0.0231 1.0000 Uani . . . . . . .
O7 O 0.8645(4) 0.1071(3) 0.63977(18) 0.0308 1.0000 Uani . . . . . . .
O8 O 1.0526(4) 0.2156(4) 0.64208(19) 0.0325 1.0000 Uani . . . . . . .
O9 O 0.7598(4) 0.3697(3) 0.62540(17) 0.0274 1.0000 Uani . . . . . . .
O10 O 0.8655(4) 0.4023(3) 0.73798(19) 0.0299 1.0000 Uani . . . . . . .
Sn1 Sn 0.47119(3) 0.43486(3) 0.787836(16) 0.0199 1.0000 Uani . . . . . . .
Ti1 Ti 0.71199(9) 0.18257(8) 0.83279(4) 0.0201 1.0000 Uani . . . . . . .
Ti2 Ti 0.87036(9) 0.23581(8) 0.68658(4) 0.0216 1.0000 Uani . . . . . . .
Cl3 Cl 0.56959(14) 0.55012(12) 0.85066(6) 0.0290 1.0000 Uani . . . . . . .
Cl1 Cl 0.37649(14) 0.31981(13) 0.72866(7) 0.0330 1.0000 Uani . . . . . . .
Cl2 Cl 0.23281(13) 0.59241(12) 0.84071(6) 0.0294 1.0000 Uani . . . . . . .
H11 H 0.3999 0.6992 0.7480 0.0367 1.0000 Uiso R . . . . . .
H23 H 0.2709 0.6449 0.6809 0.0749 1.0000 Uiso R . . . . . .
H22 H 0.2714 0.7815 0.6668 0.0751 1.0000 Uiso R . . . . . .
H21 H 0.3765 0.6629 0.6130 0.0750 1.0000 Uiso R . . . . . .
H31 H 0.6319 0.6928 0.6949 0.0779 1.0000 Uiso R . . . . . .
H32 H 0.5100 0.8073 0.6680 0.0779 1.0000 Uiso R . . . . . .
H33 H 0.6070 0.6763 0.6206 0.0778 1.0000 Uiso R . . . . . .
H41 H 0.4556 0.2124 0.9475 0.0300 1.0000 Uiso R . . . . . .
H51 H 0.4388 0.4133 0.9871 0.0481 1.0000 Uiso R . . . . . .
H52 H 0.3021 0.3873 1.0245 0.0480 1.0000 Uiso R . . . . . .
H53 H 0.2923 0.4818 0.9656 0.0479 1.0000 Uiso R . . . . . .
H61 H 0.3040 0.2179 0.8720 0.0590 1.0000 Uiso R . . . . . .
H62 H 0.2202 0.2484 0.9504 0.0591 1.0000 Uiso R . . . . . .
H63 H 0.2044 0.3609 0.9020 0.0590 1.0000 Uiso R . . . . . .
H71 H 0.6804 0.3216 0.9925 0.0401 1.0000 Uiso R . . . . . .
H81 H 0.6198 0.1555 1.0301 0.0820 1.0000 Uiso R . . . . . .
H82 H 0.7222 0.1678 1.0739 0.0820 1.0000 Uiso R . . . . . .
H83 H 0.7847 0.0588 1.0127 0.0819 1.0000 Uiso R . . . . . .
H101 H 0.7619 -0.1428 0.8020 0.0673 1.0000 Uiso R . . . . . .
H131 H 1.1045 -0.0041 0.7211 0.0368 1.0000 Uiso R . . . . . .
H143 H 1.1541 0.1597 0.7581 0.0680 1.0000 Uiso R . . . . . .
H142 H 1.0940 0.1398 0.8364 0.0678 1.0000 Uiso R . . . . . .
H141 H 1.2366 0.0312 0.7905 0.0681 1.0000 Uiso R . . . . . .
H151 H 0.9950 -0.1152 0.7933 0.0689 1.0000 Uiso R . . . . . .
H152 H 0.9785 -0.0316 0.8597 0.0690 1.0000 Uiso R . . . . . .
H153 H 1.1347 -0.1301 0.8180 0.0691 1.0000 Uiso R . . . . . .
H161 H 0.8574 -0.0391 0.6925 0.0561 1.0000 Uiso R . . . . . .
H171 H 0.6316 0.0589 0.6706 0.1051 1.0000 Uiso R . . . . . .
H172 H 0.7054 -0.0841 0.6360 0.1050 1.0000 Uiso R . . . . . .
H173 H 0.7022 0.0309 0.5905 0.1049 1.0000 Uiso R . . . . . .
H181 H 1.0699 -0.1240 0.6072 0.0870 1.0000 Uiso R . . . . . .
H182 H 0.9709 -0.1923 0.5951 0.0869 1.0000 Uiso R . . . . . .
H183 H 0.9847 -0.0811 0.5492 0.0872 1.0000 Uiso R . . . . . .
H191 H 1.1404 0.0982 0.5577 0.0530 1.0000 Uiso R . . . . . .
H201 H 1.0968 0.3130 0.5296 0.1162 1.0000 Uiso R . . . . . .
H202 H 1.2340 0.2981 0.5565 0.1159 1.0000 Uiso R . . . . . .
H203 H 1.2536 0.2101 0.4914 0.1161 1.0000 Uiso R . . . . . .
H211 H 1.2864 0.0135 0.6354 0.1180 1.0000 Uiso R . . . . . .
H212 H 1.3391 0.1264 0.6220 0.1181 1.0000 Uiso R . . . . . .
H213 H 1.3776 0.0238 0.5614 0.1180 1.0000 Uiso R . . . . . .
H221 H 0.8404 0.2578 0.5361 0.0438 1.0000 Uiso R . . . . . .
H231 H 0.6040 0.2676 0.5908 0.0839 1.0000 Uiso R . . . . . .
H232 H 0.5384 0.4090 0.5661 0.0840 1.0000 Uiso R . . . . . .
H233 H 0.6291 0.2876 0.5102 0.0839 1.0000 Uiso R . . . . . .
H243 H 0.8625 0.4542 0.5132 0.0867 1.0000 Uiso R . . . . . .
H242 H 0.6913 0.5239 0.5249 0.0871 1.0000 Uiso R . . . . . .
H241 H 0.7861 0.4191 0.4626 0.0868 1.0000 Uiso R . . . . . .
H251 H 1.0720 0.3807 0.7227 0.0471 1.0000 Uiso R . . . . . .
H263 H 0.9478 0.4254 0.8424 0.1231 1.0000 Uiso R . . . . . .
H262 H 1.0423 0.5049 0.8155 0.1229 1.0000 Uiso R . . . . . .
H261 H 0.8726 0.5709 0.8269 0.1230 1.0000 Uiso R . . . . . .
H271 H 0.9598 0.5268 0.6466 0.1220 1.0000 Uiso R . . . . . .
H272 H 1.0514 0.5707 0.6845 0.1220 1.0000 Uiso R . . . . . .
H273 H 0.8804 0.6302 0.7100 0.1220 1.0000 Uiso R . . . . . .
H10 H 0.7846 0.4412 0.7678 0.0357 1.0000 Uiso R . . . . . .
H9 H 0.7122 0.4474 0.6426 0.0328 1.0000 Uiso R . . . . . .
H91 H 0.9273 0.2876 0.9444 0.0578 1.0000 Uiso R . . . . . .
H92 H 0.9066 0.2568 1.0214 0.0578 1.0000 Uiso R . . . . . .
H93 H 0.9785 0.1454 0.9630 0.0578 1.0000 Uiso R . . . . . .
H111 H 0.5365 -0.0466 0.7788 0.0846 1.0000 Uiso R . . . . . .
H112 H 0.4612 -0.0163 0.8575 0.0846 1.0000 Uiso R . . . . . .
H113 H 0.5405 -0.1582 0.8258 0.0846 1.0000 Uiso R . . . . . .
H121 H 0.7912 -0.1279 0.9108 0.0802 1.0000 Uiso R . . . . . .
H122 H 0.6231 -0.0681 0.9416 0.0802 1.0000 Uiso R . . . . . .
H123 H 0.7025 -0.2100 0.9099 0.0802 1.0000 Uiso R . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.06(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 . 1.516(8) yes
C1 . C3 . 1.513(8) yes
C1 . O2 . 1.410(6) yes
C1 . H11 . 0.980 no
C2 . H23 . 0.966 no
C2 . H22 . 0.959 no
C2 . H21 . 0.967 no
C3 . H31 . 0.978 no
C3 . H32 . 0.974 no
C3 . H33 . 0.968 no
C4 . C5 . 1.500(7) yes
C4 . C6 . 1.525(7) yes
C4 . O3 . 1.453(5) yes
C4 . H41 . 0.984 no
C5 . H51 . 0.963 no
C5 . H52 . 0.970 no
C5 . H53 . 0.959 no
C6 . H61 . 0.960 no
C6 . H62 . 0.958 no
C6 . H63 . 0.963 no
C7 . C8 . 1.501(8) yes
C7 . C9 . 1.514(8) yes
C7 . O4 . 1.426(6) yes
C7 . H71 . 0.982 no
C8 . H81 . 0.963 no
C8 . H82 . 0.964 no
C8 . H83 . 0.962 no
C9 . H91 . 0.950 no
C9 . H92 . 0.950 no
C9 . H93 . 0.950 no
C10 . C11 . 1.488(10) yes
C10 . C12 . 1.498(9) yes
C10 . O5 . 1.405(6) yes
C10 . H101 . 0.975 no
C11 . H111 . 0.950 no
C11 . H112 . 0.950 no
C11 . H113 . 0.950 no
C12 . H121 . 0.950 no
C12 . H122 . 0.950 no
C12 . H123 . 0.950 no
C13 . C14 . 1.503(8) yes
C13 . C15 . 1.515(7) yes
C13 . O6 . 1.456(6) yes
C13 . H131 . 0.978 no
C14 . H143 . 0.972 no
C14 . H142 . 0.962 no
C14 . H141 . 0.960 no
C15 . H151 . 0.967 no
C15 . H152 . 0.971 no
C15 . H153 . 0.967 no
C16 . C17 . 1.487(10) yes
C16 . C18 . 1.497(9) yes
C16 . O7 . 1.419(6) yes
C16 . H161 . 0.988 no
C17 . H171 . 0.963 no
C17 . H172 . 0.965 no
C17 . H173 . 0.962 no
C18 . H181 . 0.963 no
C18 . H182 . 0.964 no
C18 . H183 . 0.963 no
C19 . C20 . 1.492(9) yes
C19 . C21 . 1.489(10) yes
C19 . O8 . 1.412(6) yes
C19 . H191 . 0.986 no
C20 . H201 . 0.965 no
C20 . H202 . 0.968 no
C20 . H203 . 0.965 no
C21 . H211 . 0.965 no
C21 . H212 . 0.961 no
C21 . H213 . 0.960 no
C22 . C23 . 1.513(9) yes
C22 . C24 . 1.505(8) yes
C22 . O9 . 1.460(6) yes
C22 . H221 . 0.982 no
C23 . H231 . 0.969 no
C23 . H232 . 0.973 no
C23 . H233 . 0.974 no
C24 . H243 . 0.967 no
C24 . H242 . 0.963 no
C24 . H241 . 0.962 no
C25 . C26 . 1.512(10) yes
C25 . C27 . 1.486(10) yes
C25 . O10 . 1.438(6) yes
C25 . H251 . 0.980 no
C26 . H263 . 0.967 no
C26 . H262 . 0.958 no
C26 . H261 . 0.960 no
C27 . H271 . 0.959 no
C27 . H272 . 0.960 no
C27 . H273 . 0.958 no
O1 . Sn1 . 2.053(3) yes
O1 . Ti1 . 1.943(3) yes
O1 . Ti2 . 1.993(3) yes
O2 . Sn1 . 2.037(3) yes
O3 . Sn1 . 2.106(3) yes
O3 . Ti1 . 2.017(3) yes
O4 . Ti1 . 1.756(4) yes
O5 . Ti1 . 1.753(4) yes
O6 . Ti1 . 2.014(3) yes
O6 . Ti2 . 2.001(3) yes
O7 . Ti2 . 1.784(4) yes
O8 . Ti2 . 1.799(4) yes
O9 . Ti2 . 2.076(3) yes
O9 . H9 . 0.850 no
O10 . Ti2 . 2.151(3) yes
O10 . H10 . 0.850 no
Sn1 . Ti1 . 3.2331(9) yes
Sn1 . Cl3 . 2.4696(13) yes
Sn1 . Cl1 . 2.3944(13) yes
Sn1 . Cl2 . 2.3806(12) yes
Ti1 . Ti2 . 3.1538(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 . C3 . 112.4(5) yes
C2 . C1 . O2 . 110.0(5) yes
C3 . C1 . O2 . 109.2(5) yes
C2 . C1 . H11 . 108.0 no
C3 . C1 . H11 . 109.5 no
O2 . C1 . H11 . 107.7 no
C1 . C2 . H23 . 108.4 no
C1 . C2 . H22 . 109.7 no
H23 . C2 . H22 . 109.5 no
C1 . C2 . H21 . 109.3 no
H23 . C2 . H21 . 110.3 no
H22 . C2 . H21 . 109.6 no
C1 . C3 . H31 . 109.0 no
C1 . C3 . H32 . 108.8 no
H31 . C3 . H32 . 109.8 no
C1 . C3 . H33 . 109.5 no
H31 . C3 . H33 . 110.0 no
H32 . C3 . H33 . 109.7 no
C5 . C4 . C6 . 112.3(4) yes
C5 . C4 . O3 . 111.3(4) yes
C6 . C4 . O3 . 110.0(4) yes
C5 . C4 . H41 . 108.0 no
C6 . C4 . H41 . 107.9 no
O3 . C4 . H41 . 107.1 no
C4 . C5 . H51 . 110.5 no
C4 . C5 . H52 . 109.8 no
H51 . C5 . H52 . 108.2 no
C4 . C5 . H53 . 110.8 no
H51 . C5 . H53 . 108.8 no
H52 . C5 . H53 . 108.7 no
C4 . C6 . H61 . 109.7 no
C4 . C6 . H62 . 110.3 no
H61 . C6 . H62 . 109.3 no
C4 . C6 . H63 . 109.4 no
H61 . C6 . H63 . 109.2 no
H62 . C6 . H63 . 108.9 no
C8 . C7 . C9 . 112.4(5) yes
C8 . C7 . O4 . 109.9(5) yes
C9 . C7 . O4 . 109.5(4) yes
C8 . C7 . H71 . 106.9 no
C9 . C7 . H71 . 111.3 no
O4 . C7 . H71 . 106.7 no
C7 . C8 . H81 . 109.7 no
C7 . C8 . H82 . 109.6 no
H81 . C8 . H82 . 109.8 no
C7 . C8 . H83 . 108.6 no
H81 . C8 . H83 . 109.1 no
H82 . C8 . H83 . 110.0 no
C7 . C9 . H91 . 109.5 no
C7 . C9 . H92 . 109.4 no
H91 . C9 . H92 . 109.5 no
C7 . C9 . H93 . 109.4 no
H91 . C9 . H93 . 109.5 no
H92 . C9 . H93 . 109.5 no
C11 . C10 . C12 . 114.0(6) yes
C11 . C10 . O5 . 110.0(6) yes
C12 . C10 . O5 . 110.9(6) yes
C11 . C10 . H101 . 108.2 no
C12 . C10 . H101 . 106.8 no
O5 . C10 . H101 . 106.5 no
C10 . C11 . H111 . 109.3 no
C10 . C11 . H112 . 109.3 no
H111 . C11 . H112 . 109.5 no
C10 . C11 . H113 . 109.8 no
H111 . C11 . H113 . 109.5 no
H112 . C11 . H113 . 109.5 no
C10 . C12 . H121 . 109.3 no
C10 . C12 . H122 . 109.3 no
H121 . C12 . H122 . 109.5 no
C10 . C12 . H123 . 109.8 no
H121 . C12 . H123 . 109.5 no
H122 . C12 . H123 . 109.5 no
C14 . C13 . C15 . 112.7(5) yes
C14 . C13 . O6 . 109.4(4) yes
C15 . C13 . O6 . 110.9(4) yes
C14 . C13 . H131 . 107.8 no
C15 . C13 . H131 . 108.2 no
O6 . C13 . H131 . 107.6 no
C13 . C14 . H143 . 109.3 no
C13 . C14 . H142 . 109.9 no
H143 . C14 . H142 . 109.8 no
C13 . C14 . H141 . 108.2 no
H143 . C14 . H141 . 110.0 no
H142 . C14 . H141 . 109.7 no
C13 . C15 . H151 . 108.9 no
C13 . C15 . H152 . 109.3 no
H151 . C15 . H152 . 109.6 no
C13 . C15 . H153 . 110.1 no
H151 . C15 . H153 . 109.8 no
H152 . C15 . H153 . 109.0 no
C17 . C16 . C18 . 113.0(6) yes
C17 . C16 . O7 . 110.4(6) yes
C18 . C16 . O7 . 108.6(5) yes
C17 . C16 . H161 . 108.5 no
C18 . C16 . H161 . 108.4 no
O7 . C16 . H161 . 107.8 no
C16 . C17 . H171 . 109.8 no
C16 . C17 . H172 . 110.3 no
H171 . C17 . H172 . 110.1 no
C16 . C17 . H173 . 108.8 no
H171 . C17 . H173 . 109.0 no
H172 . C17 . H173 . 108.8 no
C16 . C18 . H181 . 109.6 no
C16 . C18 . H182 . 109.6 no
H181 . C18 . H182 . 109.5 no
C16 . C18 . H183 . 108.6 no
H181 . C18 . H183 . 109.9 no
H182 . C18 . H183 . 109.6 no
C20 . C19 . C21 . 111.6(6) yes
C20 . C19 . O8 . 110.1(5) yes
C21 . C19 . O8 . 111.0(6) yes
C20 . C19 . H191 . 108.1 no
C21 . C19 . H191 . 107.8 no
O8 . C19 . H191 . 108.1 no
C19 . C20 . H201 . 109.8 no
C19 . C20 . H202 . 108.4 no
H201 . C20 . H202 . 109.9 no
C19 . C20 . H203 . 109.3 no
H201 . C20 . H203 . 109.7 no
H202 . C20 . H203 . 109.7 no
C19 . C21 . H211 . 110.3 no
C19 . C21 . H212 . 108.8 no
H211 . C21 . H212 . 109.9 no
C19 . C21 . H213 . 109.1 no
H211 . C21 . H213 . 109.9 no
H212 . C21 . H213 . 108.8 no
C23 . C22 . C24 . 112.2(6) yes
C23 . C22 . O9 . 110.2(5) yes
C24 . C22 . O9 . 109.8(5) yes
C23 . C22 . H221 . 107.2 no
C24 . C22 . H221 . 108.5 no
O9 . C22 . H221 . 108.9 no
C22 . C23 . H231 . 109.3 no
C22 . C23 . H232 . 108.1 no
H231 . C23 . H232 . 110.0 no
C22 . C23 . H233 . 108.8 no
H231 . C23 . H233 . 110.2 no
H232 . C23 . H233 . 110.3 no
C22 . C24 . H243 . 109.4 no
C22 . C24 . H242 . 109.8 no
H243 . C24 . H242 . 109.8 no
C22 . C24 . H241 . 109.5 no
H243 . C24 . H241 . 109.0 no
H242 . C24 . H241 . 109.3 no
C26 . C25 . C27 . 114.2(7) yes
C26 . C25 . O10 . 108.4(5) yes
C27 . C25 . O10 . 110.8(5) yes
C26 . C25 . H251 . 106.7 no
C27 . C25 . H251 . 107.1 no
O10 . C25 . H251 . 109.6 no
C25 . C26 . H263 . 109.6 no
C25 . C26 . H262 . 109.2 no
H263 . C26 . H262 . 110.0 no
C25 . C26 . H261 . 108.7 no
H263 . C26 . H261 . 110.0 no
H262 . C26 . H261 . 109.3 no
C25 . C27 . H271 . 110.1 no
C25 . C27 . H272 . 108.9 no
H271 . C27 . H272 . 109.8 no
C25 . C27 . H273 . 109.2 no
H271 . C27 . H273 . 109.3 no
H272 . C27 . H273 . 109.6 no
Sn1 . O1 . Ti1 . 107.99(15) yes
Sn1 . O1 . Ti2 . 144.85(16) yes
Ti1 . O1 . Ti2 . 106.50(14) yes
C1 . O2 . Sn1 . 122.3(3) yes
C4 . O3 . Sn1 . 133.1(3) yes
C4 . O3 . Ti1 . 123.6(3) yes
Sn1 . O3 . Ti1 . 103.27(14) yes
C7 . O4 . Ti1 . 167.5(3) yes
C10 . O5 . Ti1 . 168.0(4) yes
C13 . O6 . Ti1 . 132.1(3) yes
C13 . O6 . Ti2 . 123.8(3) yes
Ti1 . O6 . Ti2 . 103.54(14) yes
C16 . O7 . Ti2 . 144.5(4) yes
C19 . O8 . Ti2 . 143.5(4) yes
C22 . O9 . Ti2 . 124.8(3) yes
C22 . O9 . H9 . 117.6 no
Ti2 . O9 . H9 . 117.6 no
C25 . O10 . Ti2 . 133.6(3) yes
C25 . O10 . H10 . 114.4 no
Ti2 . O10 . H10 . 111.4 no
O3 . Sn1 . O1 . 71.93(12) yes
O3 . Sn1 . O2 . 160.31(13) yes
O1 . Sn1 . O2 . 88.71(13) yes
O3 . Sn1 . Ti1 . 37.38(9) yes
O1 . Sn1 . Ti1 . 34.86(8) yes
O2 . Sn1 . Ti1 . 122.98(10) yes
O3 . Sn1 . Cl3 . 87.11(10) yes
O1 . Sn1 . Cl3 . 87.33(10) yes
O2 . Sn1 . Cl3 . 88.43(10) yes
Ti1 . Sn1 . Cl3 . 82.99(3) yes
O3 . Sn1 . Cl1 . 91.69(10) yes
O1 . Sn1 . Cl1 . 92.28(10) yes
O2 . Sn1 . Cl1 . 92.69(11) yes
Ti1 . Sn1 . Cl1 . 96.04(4) yes
Cl3 . Sn1 . Cl1 . 178.80(5) yes
O3 . Sn1 . Cl2 . 100.34(9) yes
O1 . Sn1 . Cl2 . 171.21(9) yes
O2 . Sn1 . Cl2 . 98.68(10) yes
Ti1 . Sn1 . Cl2 . 136.92(4) yes
Cl3 . Sn1 . Cl2 . 88.13(5) yes
Cl1 . Sn1 . Cl2 . 92.12(5) yes
Sn1 . Ti1 . O3 . 39.36(9) yes
Sn1 . Ti1 . O6 . 111.38(9) yes
O3 . Ti1 . O6 . 150.63(13) yes
Sn1 . Ti1 . O1 . 37.15(9) yes
O3 . Ti1 . O1 . 76.17(13) yes
O6 . Ti1 . O1 . 75.10(13) yes
Sn1 . Ti1 . O4 . 116.71(13) yes
O3 . Ti1 . O4 . 95.92(15) yes
O6 . Ti1 . O4 . 98.77(16) yes
O1 . Ti1 . O4 . 132.13(17) yes
Sn1 . Ti1 . O5 . 116.12(13) yes
O3 . Ti1 . O5 . 97.47(16) yes
O6 . Ti1 . O5 . 101.04(16) yes
O1 . Ti1 . O5 . 117.53(17) yes
O4 . Ti1 . O5 . 110.28(19) yes
Sn1 . Ti1 . Ti2 . 74.29(2) yes
O3 . Ti1 . Ti2 . 113.47(9) yes
O6 . Ti1 . Ti2 . 38.07(9) yes
O1 . Ti1 . Ti2 . 37.30(9) yes
O4 . Ti1 . Ti2 . 124.46(13) yes
O5 . Ti1 . Ti2 . 111.08(13) yes
Ti1 . Ti2 . O10 . 86.80(10) yes
Ti1 . Ti2 . O9 . 122.75(10) yes
O10 . Ti2 . O9 . 83.71(14) yes
Ti1 . Ti2 . O6 . 38.38(9) yes
O10 . Ti2 . O6 . 91.13(14) yes
O9 . Ti2 . O6 . 160.94(14) yes
Ti1 . Ti2 . O1 . 36.21(9) yes
O10 . Ti2 . O1 . 78.68(14) yes
O9 . Ti2 . O1 . 86.67(13) yes
O6 . Ti2 . O1 . 74.32(13) yes
Ti1 . Ti2 . O8 . 137.01(13) yes
O10 . Ti2 . O8 . 83.60(16) yes
O9 . Ti2 . O8 . 97.70(16) yes
O6 . Ti2 . O8 . 99.94(15) yes
O1 . Ti2 . O8 . 161.18(17) yes
Ti1 . Ti2 . O7 . 95.41(12) yes
O10 . Ti2 . O7 . 175.05(16) yes
O9 . Ti2 . O7 . 91.38(16) yes
O6 . Ti2 . O7 . 93.35(15) yes
O1 . Ti2 . O7 . 100.52(16) yes
O8 . Ti2 . O7 . 97.68(18) 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
O9 . H9 . O2 . 129 0.85 1.91 2.535(11) yes
####################################################################### 
# 
# 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_smr268b
_database_code_depnum_ccdc_archive 'CCDC 802189'
_audit_update_record             
;
2010-11-25 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'smr268b.cif'

_audit_creation_date             10-11-19
_audit_creation_method           CRYSTALS_ver_14.11

_oxford_structure_analysis_title 'smr268b in C 2/c'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.3200(10)
_cell_length_b                   19.198(2)
_cell_length_c                   14.026(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.880(10)
_cell_angle_gamma                90
_cell_volume                     2413.8(5)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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'
Nb -2.0727 0.6215 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957
3.7559 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C18 H30 Cl6 Nb1.50 O9 Sn1.50
# Dc = 2.53 Fooo = 1244.00 Mu = 29.57 M = 460.27
# Found Formula = C12 H32 Cl4 Nb1 O6 Sn1
# Dc = 1.72 FOOO = 1244.00 Mu = 19.73 M = 312.89

_chemical_formula_sum            'C12 H32 Cl4 Nb1 O6 Sn1'
_chemical_formula_moiety         'C12 H32 Cl4 Nb1 O6 Sn1'
_chemical_compound_source        ?
_chemical_formula_weight         625.79


_cell_measurement_reflns_used    4908
_cell_measurement_theta_min      3.4073
_cell_measurement_theta_max      29.5459
_cell_measurement_temperature    110

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.211
_exptl_crystal_size_mid          0.386
_exptl_crystal_size_max          0.494

_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             1244
_exptl_absorpt_coefficient_mu    1.973

# Sheldrick geometric approximatio 0.47 0.66
_exptl_absorpt_correction_T_min  0.62353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_detector_area_resol_mean 10.4685

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_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      110
_diffrn_reflns_number            10336
_reflns_number_total             3001
_diffrn_reflns_av_R_equivalents  0.065
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 3001
# Theoretical number of reflections is about 6795


_diffrn_reflns_theta_min         3.414
_diffrn_reflns_theta_max         29.610
_diffrn_measured_fraction_theta_max 0.884

_diffrn_reflns_theta_full        26.353
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              26
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

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

_refine_diff_density_min         -2.69
_refine_diff_density_max         2.21


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


# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         3001
_refine_ls_number_restraints     0
_refine_ls_number_parameters     128
_oxford_refine_ls_R_factor_ref   0.0978
_refine_ls_wR_factor_ref         0.1759
_refine_ls_goodness_of_fit_ref   0.9174
_refine_ls_shift/su_max          0.0002955
_refine_ls_shift/su_mean         0.0000299


# The values computed from all data
_oxford_reflns_number_all        3001
_refine_ls_R_factor_all          0.0978
_refine_ls_wR_factor_all         0.1759

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2209
_refine_ls_R_factor_gt           0.0746
_refine_ls_wR_factor_gt          0.1444

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
0.267E+04 0.436E+04 0.256E+04 986. 210.
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Sn1 Sn 1.0000 0.58765(5) 0.7500 0.0520 1.0000 Uani S T . . . .
Cl2 Cl 0.7802(3) 0.58321(15) 0.61095(15) 0.0708 1.0000 Uani . . . . . .
Cl3 Cl 1.1110(3) 0.66828(15) 0.66433(18) 0.0775 1.0000 Uani . . . . . .
O1 O 1.0740(6) 0.4974(3) 0.6923(4) 0.0533 1.0000 Uani . . . . . .
O2 O 0.8201(9) 0.4130(5) 0.6291(6) 0.0931 1.0000 Uani . . . . . .
C4 C 0.582(4) 0.369(2) 0.579(3) 0.1455 0.5000 Uani . . . 1 2 .
C7 C 0.650(3) 0.4022(14) 0.5800(19) 0.0746 0.5000 Uani . . . 1 1 .
O3 O 1.0941(11) 0.3494(4) 0.6867(7) 0.0983 1.0000 Uani . . . . . .
C1 C 1.1515(9) 0.4985(5) 0.6150(6) 0.0582 1.0000 Uani . . . . . .
C2 C 1.3163(10) 0.5027(7) 0.6620(7) 0.0790 1.0000 Uani . . . . . .
C3 C 0.737(3) 0.3582(18) 0.581(2) 0.1164 0.5000 Uani . . . 1 2 .
C8 C 0.640(3) 0.3437(17) 0.5151(19) 0.1094 0.5000 Uani . . . 1 1 .
Nb1 Nb 1.0000 0.40888(8) 0.7500 0.0954 1.0000 Uani S T . . . .
H71 H 0.5984 0.3926 0.6300 0.0900 0.5000 Uiso R . . 1 1 .
H72 H 0.6076 0.4433 0.5426 0.0900 0.5000 Uiso R . . 1 1 .
H11 H 1.1173 0.5387 0.5725 0.0699 1.0000 Uiso R . . . . .
H12 H 1.1283 0.4558 0.5760 0.0699 1.0000 Uiso R . . . . .
H23 H 1.3673 0.5080 0.6116 0.1190 1.0000 Uiso R . . . . .
H22 H 1.3369 0.5418 0.7065 0.1189 1.0000 Uiso R . . . . .
H21 H 1.3484 0.4603 0.6984 0.1189 1.0000 Uiso R . . . . .
H31 H 0.7719 0.3153 0.6158 0.1390 0.5000 Uiso R . . 1 2 .
H32 H 0.7450 0.3550 0.5134 0.1390 0.5000 Uiso R . . 1 2 .
H83 H 0.5388 0.3275 0.4944 0.1610 0.5000 Uiso R . . 1 1 .
H82 H 0.7038 0.3070 0.5497 0.1609 0.5000 Uiso R . . 1 1 .
H81 H 0.6716 0.3573 0.4580 0.1610 0.5000 Uiso R . . 1 1 .
C9 C 1.123(3) 0.2907(11) 0.6282(14) 0.1908 1.0000 Uani . . . . . .
C10 C 1.280(3) 0.3010(11) 0.6286(14) 0.2008 1.0000 Uani . . . . . .
H91 H 1.1060 0.2457 0.6570 0.2120 1.0000 Uiso R . . 2 2 .
H92 H 1.0597 0.2938 0.5608 0.2120 1.0000 Uiso R . . 2 2 .
H103 H 1.3119 0.2616 0.5969 0.3090 1.0000 Uiso R . . 2 2 .
H102 H 1.3403 0.3040 0.6961 0.3090 1.0000 Uiso R . . 2 2 .
H101 H 1.2927 0.3430 0.5942 0.3090 1.0000 Uiso R . . 2 2 .
H2 H 0.7893 0.4532 0.6200 0.1400 0.5000 Uiso R . . . . .
H41 H 0.5244 0.3306 0.5460 0.1723 0.5000 Uiso R . . 1 2 .
H42 H 0.5736 0.3720 0.6446 0.1723 0.5000 Uiso R . . 1 2 .
H43 H 0.5477 0.4106 0.5441 0.1723 0.5000 Uiso R . . 1 2 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.94(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 . O1 5_756 2.106(6) yes
Sn1 . Cl2 5_756 2.413(2) yes
Sn1 . Cl3 5_756 2.364(3) yes
Sn1 . Cl2 . 2.413(2) yes
Sn1 . Cl3 . 2.364(3) yes
Sn1 . O1 . 2.106(6) yes
O1 . C1 . 1.458(9) yes
O1 . Nb1 . 2.080(6) yes
O2 . C7 . 1.56(3) yes
O2 . Nb1 . 2.034(8) yes
O2 . H2 . 0.822 no
O2 . C3 . 1.37(3) yes
O2 . Nb1 . 2.034(8) yes
O2 . H2 . 0.822 no
C4 . C3 . 1.44(4) yes
C4 . H41 . 0.950 no
C4 . H42 . 0.950 no
C4 . H43 . 0.950 no
C7 . C8 . 1.43(4) yes
C7 . H71 . 0.972 no
C7 . H72 . 0.970 no
O3 . Nb1 . 1.813(8) yes
O3 . C9 . 1.462(16) yes
C1 . C2 . 1.499(12) yes
C1 . H11 . 0.974 no
C1 . H12 . 0.976 no
C2 . H23 . 0.959 no
C2 . H22 . 0.961 no
C2 . H21 . 0.964 no
C3 . H31 . 0.970 no
C3 . H32 . 0.972 no
C8 . H83 . 0.961 no
C8 . H82 . 0.962 no
C8 . H81 . 0.962 no
C9 . C10 . 1.48(3) yes
C9 . H91 . 0.984 no
C9 . H92 . 0.971 no
C10 . H103 . 0.963 no
C10 . H102 . 0.961 no
C10 . H101 . 0.963 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 5_756 Sn1 . Cl2 5_756 87.43(16) yes
O1 5_756 Sn1 . Cl3 5_756 96.22(17) yes
Cl2 5_756 Sn1 . Cl3 5_756 90.29(10) yes
O1 5_756 Sn1 . Cl2 . 89.24(16) yes
Cl2 5_756 Sn1 . Cl2 . 175.95(15) yes
Cl3 5_756 Sn1 . Cl2 . 92.36(9) yes
O1 5_756 Sn1 . Cl3 . 165.58(18) yes
Cl2 5_756 Sn1 . Cl3 . 92.36(9) yes
Cl3 5_756 Sn1 . Cl3 . 98.20(14) yes
Cl2 . Sn1 . Cl3 . 90.29(10) yes
O1 5_756 Sn1 . O1 . 69.4(3) yes
Cl2 5_756 Sn1 . O1 . 89.24(16) yes
Cl3 5_756 Sn1 . O1 . 165.58(18) yes
Cl2 . Sn1 . O1 . 87.43(16) yes
Cl3 . Sn1 . O1 . 96.22(17) yes
Sn1 . O1 . C1 . 123.7(5) yes
Sn1 . O1 . Nb1 . 110.1(2) yes
C1 . O1 . Nb1 . 125.8(5) yes
C7 . O2 . Nb1 . 150.4(11) yes
C7 . O2 . H2 . 77.7 no
Nb1 . O2 . H2 . 109.8 no
C3 . O2 . Nb1 . 127.5(15) yes
C3 . O2 . H2 . 121.1 no
Nb1 . O2 . H2 . 109.8 no
C3 . C4 . H41 . 109.5 no
C3 . C4 . H42 . 109.9 no
H41 . C4 . H42 . 109.5 no
C3 . C4 . H43 . 109.0 no
H41 . C4 . H43 . 109.5 no
H42 . C4 . H43 . 109.5 no
O2 . C7 . C8 . 105(2) yes
O2 . C7 . H71 . 110.6 no
C8 . C7 . H71 . 110.6 no
O2 . C7 . H72 . 110.4 no
C8 . C7 . H72 . 110.3 no
H71 . C7 . H72 . 109.4 no
Nb1 . O3 . C9 . 161.5(13) yes
O1 . C1 . C2 . 109.3(6) yes
O1 . C1 . H11 . 108.7 no
C2 . C1 . H11 . 110.5 no
O1 . C1 . H12 . 109.1 no
C2 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.7 no
C1 . C2 . H23 . 109.7 no
C1 . C2 . H22 . 109.1 no
H23 . C2 . H22 . 110.1 no
C1 . C2 . H21 . 108.7 no
H23 . C2 . H21 . 109.6 no
H22 . C2 . H21 . 109.7 no
C4 . C3 . O2 . 109(3) yes
C4 . C3 . H31 . 109.1 no
O2 . C3 . H31 . 109.4 no
C4 . C3 . H32 . 109.6 no
O2 . C3 . H32 . 110.0 no
H31 . C3 . H32 . 109.5 no
C7 . C8 . H83 . 109.5 no
C7 . C8 . H82 . 109.2 no
H83 . C8 . H82 . 109.6 no
C7 . C8 . H81 . 109.5 no
H83 . C8 . H81 . 109.5 no
H82 . C8 . H81 . 109.5 no
O1 . Nb1 . O1 5_756 70.4(3) yes
O1 . Nb1 . O2 . 86.0(3) yes
O1 5_756 Nb1 . O2 . 90.4(3) yes
O1 . Nb1 . O2 5_756 90.4(3) yes
O1 5_756 Nb1 . O2 5_756 86.0(3) yes
O2 . Nb1 . O2 5_756 175.6(5) yes
O1 . Nb1 . O3 . 93.9(3) yes
O1 5_756 Nb1 . O3 . 164.0(3) yes
O2 . Nb1 . O3 . 90.9(4) yes
O2 5_756 Nb1 . O3 . 91.9(4) yes
O1 . Nb1 . O3 5_756 164.0(3) yes
O1 5_756 Nb1 . O3 5_756 93.9(3) yes
O2 . Nb1 . O3 5_756 91.9(4) yes
O2 5_756 Nb1 . O3 5_756 90.9(4) yes
O3 . Nb1 . O3 5_756 102.0(6) yes
O3 . C9 . C10 . 103.3(18) yes
O3 . C9 . H91 . 111.8 no
C10 . C9 . H91 . 112.9 no
O3 . C9 . H92 . 109.9 no
C10 . C9 . H92 . 109.5 no
H91 . C9 . H92 . 109.3 no
C9 . C10 . H103 . 108.8 no
C9 . C10 . H102 . 108.7 no
H103 . C10 . H102 . 109.4 no
C9 . C10 . H101 . 111.5 no
H103 . C10 . H101 . 109.4 no
H102 . C10 . H101 . 109.0 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/11/10 at 14:26:27
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE O ( 2,X'S) H ( 2,X'S)
RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) H ( 43,X'S)
RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S)
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S)
RIDE C ( 2,X'S) H ( 23,X'S) H ( 22,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE C ( 8,X'S) H ( 83,X'S) H ( 82,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S)
RIDE C ( 10,X'S) H ( 103,X'S) H ( 102,X'S) H ( 101,X'S)
END
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/11/10 at 14:26:27
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;


