# 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_final
_database_code_depnum_ccdc_archive 'CCDC 1421298'
_audit_update_record             
;
2015-09-30 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C82 H112 N2 Nb2 O6 P6, (C6 H6)'
_chemical_formula_sum            'C88 H118 N2 Nb2 O6 P6'
_chemical_formula_weight         1749.6787


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4029(7)
_cell_length_b                   13.7294(10)
_cell_length_c                   16.3434(12)
_cell_angle_alpha                94.9290(10)
_cell_angle_beta                 93.6830(10)
_cell_angle_gamma                95.8840(10)
_cell_volume                     2307.1(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       shard
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_F_000             880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.400
_shelx_estimated_absorpt_T_min   0.946
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6618
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_absorpt_special_details   ;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            57444
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_av_R_equivalents  0.1072
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.862
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11436
_reflns_number_gt                8015
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2009)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0234P)²+1.5512P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11436
_refine_ls_number_parameters     563
_refine_ls_number_restraints     986
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0829
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      0.981
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.15396(2) 0.65299(2) 0.22028(2) 0.01302(7) Uani 1 1 d . U . . .
P1 P 0.14323(7) 0.65796(5) 0.06346(5) 0.01919(17) Uani 1 1 d . U . . .
P2 P 0.05488(7) 0.50439(5) 0.06161(5) 0.01783(16) Uani 1 1 d . U . . .
P3 P -0.04065(7) 0.62730(5) 0.11716(5) 0.01811(16) Uani 1 1 d . U . . .
O1 O 0.02397(17) 0.62041(13) 0.29835(11) 0.0145(4) Uani 1 1 d . U . . .
O2 O 0.22743(17) 0.53468(12) 0.23800(11) 0.0139(4) Uani 1 1 d . U . . .
O3 O 0.15753(18) 0.79007(13) 0.24807(12) 0.0179(4) Uani 1 1 d . U . . .
N1 N 0.3748(2) 0.69990(16) 0.19243(14) 0.0159(5) Uani 1 1 d . U . . .
C11 C -0.1738(3) 0.6634(2) 0.34917(17) 0.0181(6) Uani 1 1 d . U . . .
C12 C -0.1031(3) 0.5930(2) 0.30999(16) 0.0152(6) Uani 1 1 d . U . . .
C121 C -0.1110(3) 0.7668(2) 0.3784(2) 0.0255(7) Uani 1 1 d . U . . .
H121 H -0.0175 0.7701 0.3667 0.031 Uiso 1 1 calc R U . . .
C122 C -0.1707(4) 0.8444(3) 0.3331(3) 0.0492(11) Uani 1 1 d . U . . .
H12A H -0.1669 0.8292 0.2737 0.074 Uiso 1 1 calc R U . . .
H12B H -0.1226 0.9089 0.3503 0.074 Uiso 1 1 calc R U . . .
H12C H -0.2612 0.8454 0.3461 0.074 Uiso 1 1 calc R U . . .
C123 C -0.1174(4) 0.7888(3) 0.4719(2) 0.0492(10) Uani 1 1 d . U . . .
H12D H -0.0726 0.8543 0.4895 0.074 Uiso 1 1 calc R U . . .
H12E H -0.0755 0.7394 0.5007 0.074 Uiso 1 1 calc R U . . .
H12F H -0.2082 0.7867 0.4850 0.074 Uiso 1 1 calc R U . . .
C13 C -0.3024(3) 0.6362(2) 0.36293(18) 0.0224(6) Uani 1 1 d . U . . .
H13 H -0.3516 0.6834 0.3882 0.027 Uiso 1 1 calc R U . . .
C14 C -0.3602(3) 0.5412(2) 0.34039(18) 0.0239(7) Uani 1 1 d . U . . .
H14 H -0.4482 0.5236 0.3502 0.029 Uiso 1 1 calc R U . . .
C15 C -0.2890(3) 0.4729(2) 0.30371(17) 0.0208(6) Uani 1 1 d . U . . .
H15 H -0.3290 0.4078 0.2890 0.025 Uiso 1 1 calc R U . . .
C16 C -0.1599(3) 0.4962(2) 0.28743(17) 0.0170(6) Uani 1 1 d . U . . .
C161 C -0.0870(3) 0.4162(2) 0.24801(17) 0.0186(6) Uani 1 1 d . U . . .
H161 H -0.0033 0.4482 0.2312 0.022 Uiso 1 1 calc R U . . .
C162 C -0.1633(3) 0.3637(2) 0.17032(18) 0.0262(7) Uani 1 1 d . U . . .
H16A H -0.2426 0.3271 0.1857 0.039 Uiso 1 1 calc R U . . .
H16B H -0.1100 0.3181 0.1426 0.039 Uiso 1 1 calc R U . . .
H16C H -0.1861 0.4125 0.1331 0.039 Uiso 1 1 calc R U . . .
C163 C -0.0548(3) 0.3409(2) 0.30903(19) 0.0262(7) Uani 1 1 d . U . . .
H16D H -0.0007 0.3746 0.3565 0.039 Uiso 1 1 calc R U . . .
H16E H -0.0078 0.2906 0.2816 0.039 Uiso 1 1 calc R U . . .
H16F H -0.1353 0.3097 0.3278 0.039 Uiso 1 1 calc R U . . .
C21 C 0.2738(2) 0.46393(19) 0.28261(17) 0.0148(6) Uani 1 1 d . U . . .
C22 C 0.3114(3) 0.3796(2) 0.23839(18) 0.0192(6) Uani 1 1 d . U . . .
C221 C 0.3060(3) 0.3671(2) 0.14558(18) 0.0219(6) Uani 1 1 d . U . . .
H221 H 0.2764 0.4281 0.1248 0.026 Uiso 1 1 calc R U . . .
C222 C 0.2078(3) 0.2801(2) 0.1104(2) 0.0316(8) Uani 1 1 d . U . . .
H22A H 0.2347 0.2191 0.1296 0.047 Uiso 1 1 calc R U . . .
H22B H 0.2041 0.2755 0.0501 0.047 Uiso 1 1 calc R U . . .
H22C H 0.1220 0.2902 0.1289 0.047 Uiso 1 1 calc R U . . .
C223 C 0.4407(3) 0.3551(2) 0.1146(2) 0.0323(8) Uani 1 1 d . U . . .
H22D H 0.5014 0.4122 0.1361 0.049 Uiso 1 1 calc R U . . .
H22E H 0.4348 0.3500 0.0543 0.049 Uiso 1 1 calc R U . . .
H22F H 0.4717 0.2953 0.1338 0.049 Uiso 1 1 calc R U . . .
C23 C 0.3554(3) 0.3067(2) 0.2844(2) 0.0256(7) Uani 1 1 d . U . . .
H23 H 0.3824 0.2496 0.2565 0.031 Uiso 1 1 calc R U . . .
C24 C 0.3604(3) 0.3158(2) 0.3692(2) 0.0274(7) Uani 1 1 d . U . . .
H24 H 0.3869 0.2640 0.3990 0.033 Uiso 1 1 calc R U . . .
C25 C 0.3270(3) 0.4003(2) 0.41078(19) 0.0213(6) Uani 1 1 d . U . . .
H25 H 0.3326 0.4063 0.4693 0.026 Uiso 1 1 calc R U . . .
C26 C 0.2852(3) 0.47723(19) 0.36907(17) 0.0161(6) Uani 1 1 d . U . . .
C261 C 0.2585(3) 0.5705(2) 0.41789(17) 0.0174(6) Uani 1 1 d . U . . .
H261 H 0.2388 0.6190 0.3778 0.021 Uiso 1 1 calc R U . . .
C262 C 0.1407(3) 0.5543(2) 0.46914(19) 0.0259(7) Uani 1 1 d . U . . .
H26A H 0.0640 0.5291 0.4326 0.039 Uiso 1 1 calc R U . . .
H26B H 0.1258 0.6169 0.4986 0.039 Uiso 1 1 calc R U . . .
H26C H 0.1573 0.5068 0.5089 0.039 Uiso 1 1 calc R U . . .
C263 C 0.3771(3) 0.6156(2) 0.47398(18) 0.0239(7) Uani 1 1 d . U . . .
H26D H 0.4018 0.5679 0.5118 0.036 Uiso 1 1 calc R U . . .
H26E H 0.3560 0.6750 0.5057 0.036 Uiso 1 1 calc R U . . .
H26F H 0.4493 0.6327 0.4403 0.036 Uiso 1 1 calc R U . . .
C31 C 0.1543(3) 0.88706(19) 0.27520(19) 0.0201(6) Uani 1 1 d . U . . .
C32 C 0.0866(3) 0.9455(2) 0.2242(2) 0.0250(7) Uani 1 1 d . U . . .
C321 C 0.0210(3) 0.9027(2) 0.1417(2) 0.0321(8) Uani 1 1 d . U . . .
H321 H -0.0006 0.8306 0.1449 0.039 Uiso 1 1 calc R U . . .
C322 C -0.1058(4) 0.9454(2) 0.1200(2) 0.0425(9) Uani 1 1 d . U . . .
H32A H -0.1602 0.9432 0.1668 0.064 Uiso 1 1 calc R U . . .
H32B H -0.1518 0.9066 0.0718 0.064 Uiso 1 1 calc R U . . .
H32C H -0.0867 1.0137 0.1076 0.064 Uiso 1 1 calc R U . . .
C323 C 0.1117(4) 0.9151(3) 0.0726(2) 0.0479(10) Uani 1 1 d . U . . .
H32D H 0.1312 0.9852 0.0658 0.072 Uiso 1 1 calc R U . . .
H32E H 0.0698 0.8811 0.0211 0.072 Uiso 1 1 calc R U . . .
H32F H 0.1923 0.8870 0.0864 0.072 Uiso 1 1 calc R U . . .
C33 C 0.0851(3) 1.0446(2) 0.2520(2) 0.0312(8) Uani 1 1 d . U . . .
H33 H 0.0398 1.0858 0.2192 0.037 Uiso 1 1 calc R U . . .
C34 C 0.1483(3) 1.0834(2) 0.3262(2) 0.0351(8) Uani 1 1 d . U . . .
H34 H 0.1475 1.1511 0.3436 0.042 Uiso 1 1 calc R U . . .
C35 C 0.2123(3) 1.0248(2) 0.3750(2) 0.0370(8) Uani 1 1 d . U . . .
H35 H 0.2542 1.0526 0.4263 0.044 Uiso 1 1 calc R U . . .
C36 C 0.2174(3) 0.9252(2) 0.3511(2) 0.0275(7) Uani 1 1 d . U . . .
C361 C 0.2881(3) 0.8619(2) 0.4073(2) 0.0370(8) Uani 1 1 d . U . . .
H361 H 0.2594 0.7915 0.3878 0.044 Uiso 1 1 calc R U . . .
C362 C 0.2554(4) 0.8783(3) 0.4968(2) 0.0517(11) Uani 1 1 d . U . . .
H36A H 0.2875 0.9457 0.5187 0.078 Uiso 1 1 calc R U . . .
H36B H 0.2966 0.8318 0.5294 0.078 Uiso 1 1 calc R U . . .
H36C H 0.1613 0.8680 0.4997 0.078 Uiso 1 1 calc R U . . .
C363 C 0.4345(4) 0.8788(3) 0.4012(3) 0.0572(12) Uani 1 1 d . U . . .
H36D H 0.4549 0.8607 0.3446 0.086 Uiso 1 1 calc R U . . .
H36E H 0.4779 0.8384 0.4386 0.086 Uiso 1 1 calc R U . . .
H36F H 0.4647 0.9484 0.4166 0.086 Uiso 1 1 calc R U . . .
C41 C 0.4165(3) 0.7910(2) 0.1766(2) 0.0312(8) Uani 1 1 d . U . . .
H41 H 0.3593 0.8403 0.1832 0.037 Uiso 1 1 calc R U . . .
C42 C 0.5386(3) 0.8178(2) 0.1511(2) 0.0407(9) Uani 1 1 d . U . . .
H42 H 0.5636 0.8838 0.1405 0.049 Uiso 1 1 calc R U . . .
C43 C 0.6231(3) 0.7478(2) 0.14142(19) 0.0267(7) Uani 1 1 d . U . . .
H43 H 0.7069 0.7639 0.1232 0.032 Uiso 1 1 calc R U . . .
C44 C 0.5833(3) 0.6545(2) 0.1587(2) 0.0293(7) Uani 1 1 d . U . . .
H44 H 0.6400 0.6046 0.1537 0.035 Uiso 1 1 calc R U . . .
C45 C 0.4596(3) 0.6332(2) 0.1834(2) 0.0259(7) Uani 1 1 d . U . . .
H45 H 0.4333 0.5676 0.1947 0.031 Uiso 1 1 calc R U . . .
C1S C -0.5771(8) 1.0575(6) 0.1770(7) 0.051(2) Uani 0.621(11) 1 d D U P A 1
H1S H -0.6590 1.0369 0.1961 0.061 Uiso 0.621(11) 1 calc R U P A 1
C2S C -0.5663(8) 1.0648(6) 0.0953(7) 0.060(2) Uani 0.621(11) 1 d D U P A 1
H2S H -0.6398 1.0478 0.0573 0.072 Uiso 0.621(11) 1 calc R U P A 1
C3S C -0.4525(7) 1.0958(5) 0.0690(6) 0.055(2) Uani 0.621(11) 1 d D U P A 1
H3S H -0.4461 1.1023 0.0120 0.066 Uiso 0.621(11) 1 calc R U P A 1
C4S C -0.3432(8) 1.1187(7) 0.1224(6) 0.048(2) Uani 0.621(11) 1 d D U P A 1
H4S H -0.2636 1.1415 0.1014 0.058 Uiso 0.621(11) 1 calc R U P A 1
C5S C -0.3472(9) 1.1094(7) 0.2039(7) 0.063(3) Uani 0.621(11) 1 d D U P A 1
H5S H -0.2708 1.1220 0.2399 0.076 Uiso 0.621(11) 1 calc R U P A 1
C6S C -0.4684(9) 1.0801(6) 0.2339(7) 0.062(2) Uani 0.621(11) 1 d D U P A 1
H6S H -0.4762 1.0758 0.2911 0.074 Uiso 0.621(11) 1 calc R U P A 1
C1T C -0.5268(14) 1.0769(10) 0.1367(9) 0.053(3) Uani 0.379(11) 1 d D U P A 2
H1T H -0.5958 1.0699 0.0949 0.064 Uiso 0.379(11) 1 calc R U P A 2
C2T C -0.5503(15) 1.0599(10) 0.2165(9) 0.044(3) Uani 0.379(11) 1 d D U P A 2
H2T H -0.6363 1.0390 0.2287 0.053 Uiso 0.379(11) 1 calc R U P A 2
C3T C -0.4567(13) 1.0718(10) 0.2773(9) 0.056(3) Uani 0.379(11) 1 d D U P A 2
H3T H -0.4760 1.0596 0.3318 0.067 Uiso 0.379(11) 1 calc R U P A 2
C4T C -0.3352(12) 1.1013(8) 0.2608(10) 0.060(3) Uani 0.379(11) 1 d D U P A 2
H4T H -0.2689 1.1097 0.3043 0.072 Uiso 0.379(11) 1 calc R U P A 2
C5T C -0.3037(13) 1.1194(10) 0.1840(10) 0.051(3) Uani 0.379(11) 1 d D U P A 2
H5T H -0.2166 1.1423 0.1757 0.062 Uiso 0.379(11) 1 calc R U P A 2
C6T C -0.3948(15) 1.1056(12) 0.1174(10) 0.057(4) Uani 0.379(11) 1 d D U P A 2
H6T H -0.3724 1.1142 0.0628 0.068 Uiso 0.379(11) 1 calc R U P A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O3 1.8938(18) . ?
Nb1 O2 1.9008(17) . ?
Nb1 O1 1.9627(18) . ?
Nb1 N1 2.404(2) . ?
Nb1 P3 2.5253(8) . ?
Nb1 P1 2.5653(8) . ?
P1 P3 2.1727(11) . ?
P1 P2 2.2089(10) . ?
P2 P3 2.2035(11) . ?
P2 P2 2.2381(15) 2_565 ?
O1 C12 1.367(3) . ?
O2 C21 1.371(3) . ?
O3 C31 1.371(3) . ?
N1 C41 1.333(3) . ?
N1 C45 1.341(4) . ?
C11 C13 1.389(4) . ?
C11 C12 1.409(4) . ?
C11 C121 1.524(4) . ?
C12 C16 1.407(4) . ?
C121 C122 1.510(4) . ?
C121 C123 1.539(5) . ?
C13 C14 1.387(4) . ?
C14 C15 1.375(4) . ?
C15 C16 1.396(4) . ?
C16 C161 1.519(4) . ?
C161 C162 1.535(4) . ?
C161 C163 1.543(4) . ?
C21 C26 1.405(4) . ?
C21 C22 1.415(4) . ?
C22 C23 1.398(4) . ?
C22 C221 1.509(4) . ?
C221 C222 1.535(4) . ?
C221 C223 1.541(4) . ?
C23 C24 1.379(4) . ?
C24 C25 1.381(4) . ?
C25 C26 1.396(4) . ?
C26 C261 1.510(4) . ?
C261 C263 1.532(4) . ?
C261 C262 1.536(4) . ?
C31 C36 1.399(4) . ?
C31 C32 1.411(4) . ?
C32 C33 1.398(4) . ?
C32 C321 1.515(4) . ?
C321 C323 1.527(5) . ?
C321 C322 1.530(5) . ?
C33 C34 1.380(5) . ?
C34 C35 1.370(5) . ?
C35 C36 1.397(4) . ?
C36 C361 1.524(5) . ?
C361 C362 1.526(5) . ?
C361 C363 1.529(5) . ?
C41 C42 1.387(4) . ?
C42 C43 1.373(4) . ?
C43 C44 1.364(4) . ?
C44 C45 1.384(4) . ?
C1S C2S 1.359(10) . ?
C1S C6S 1.408(11) . ?
C2S C3S 1.327(9) . ?
C3S C4S 1.380(10) . ?
C4S C5S 1.352(11) . ?
C5S C6S 1.414(10) . ?
C1T C2T 1.379(13) . ?
C1T C6T 1.451(16) . ?
C2T C3T 1.333(13) . ?
C3T C4T 1.339(14) . ?
C4T C5T 1.353(13) . ?
C5T C6T 1.384(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Nb1 O2 147.76(8) . . ?
O3 Nb1 O1 93.12(8) . . ?
O2 Nb1 O1 89.63(7) . . ?
O3 Nb1 N1 82.08(8) . . ?
O2 Nb1 N1 79.79(7) . . ?
O1 Nb1 N1 150.24(8) . . ?
O3 Nb1 P3 99.18(6) . . ?
O2 Nb1 P3 113.03(6) . . ?
O1 Nb1 P3 83.08(6) . . ?
N1 Nb1 P3 126.67(6) . . ?
O3 Nb1 P1 97.06(6) . . ?
O2 Nb1 P1 104.17(6) . . ?
O1 Nb1 P1 133.48(6) . . ?
N1 Nb1 P1 76.26(6) . . ?
P3 Nb1 P1 50.52(2) . . ?
P3 P1 P2 60.38(3) . . ?
P3 P1 Nb1 63.78(3) . . ?
P2 P1 Nb1 83.95(3) . . ?
P3 P2 P1 59.00(3) . . ?
P3 P2 P2 95.50(5) . 2_565 ?
P1 P2 P2 97.20(5) . 2_565 ?
P1 P3 P2 60.62(3) . . ?
P1 P3 Nb1 65.69(3) . . ?
P2 P3 Nb1 85.01(3) . . ?
C12 O1 Nb1 147.37(17) . . ?
C21 O2 Nb1 156.77(17) . . ?
C31 O3 Nb1 174.27(18) . . ?
C41 N1 C45 116.0(2) . . ?
C41 N1 Nb1 122.24(19) . . ?
C45 N1 Nb1 121.41(18) . . ?
C13 C11 C12 118.6(3) . . ?
C13 C11 C121 120.0(3) . . ?
C12 C11 C121 121.3(2) . . ?
O1 C12 C16 121.1(2) . . ?
O1 C12 C11 117.9(2) . . ?
C16 C12 C11 120.9(2) . . ?
C122 C121 C11 112.2(3) . . ?
C122 C121 C123 110.2(3) . . ?
C11 C121 C123 111.1(3) . . ?
C14 C13 C11 121.2(3) . . ?
C15 C14 C13 119.4(3) . . ?
C14 C15 C16 122.0(3) . . ?
C15 C16 C12 117.8(3) . . ?
C15 C16 C161 118.9(2) . . ?
C12 C16 C161 123.2(2) . . ?
C16 C161 C162 111.2(2) . . ?
C16 C161 C163 111.7(2) . . ?
C162 C161 C163 110.3(2) . . ?
O2 C21 C26 120.2(2) . . ?
O2 C21 C22 117.6(2) . . ?
C26 C21 C22 122.2(2) . . ?
C23 C22 C21 117.2(3) . . ?
C23 C22 C221 120.3(3) . . ?
C21 C22 C221 122.5(2) . . ?
C22 C221 C222 111.4(2) . . ?
C22 C221 C223 111.4(2) . . ?
C222 C221 C223 110.5(2) . . ?
C24 C23 C22 121.6(3) . . ?
C23 C24 C25 119.9(3) . . ?
C24 C25 C26 121.7(3) . . ?
C25 C26 C21 117.3(3) . . ?
C25 C26 C261 119.2(3) . . ?
C21 C26 C261 123.4(2) . . ?
C26 C261 C263 111.5(2) . . ?
C26 C261 C262 112.3(2) . . ?
C263 C261 C262 109.8(2) . . ?
O3 C31 C36 120.0(3) . . ?
O3 C31 C32 117.9(3) . . ?
C36 C31 C32 122.1(3) . . ?
C33 C32 C31 117.5(3) . . ?
C33 C32 C321 121.5(3) . . ?
C31 C32 C321 121.0(3) . . ?
C32 C321 C323 111.4(3) . . ?
C32 C321 C322 113.3(3) . . ?
C323 C321 C322 109.8(3) . . ?
C34 C33 C32 121.0(3) . . ?
C35 C34 C33 120.4(3) . . ?
C34 C35 C36 121.6(3) . . ?
C35 C36 C31 117.5(3) . . ?
C35 C36 C361 120.2(3) . . ?
C31 C36 C361 122.3(3) . . ?
C36 C361 C362 112.6(3) . . ?
C36 C361 C363 111.0(3) . . ?
C362 C361 C363 110.3(3) . . ?
N1 C41 C42 123.7(3) . . ?
C43 C42 C41 119.1(3) . . ?
C44 C43 C42 118.2(3) . . ?
C43 C44 C45 119.4(3) . . ?
N1 C45 C44 123.6(3) . . ?
C2S C1S C6S 120.9(7) . . ?
C3S C2S C1S 119.5(8) . . ?
C2S C3S C4S 121.7(8) . . ?
C5S C4S C3S 121.3(7) . . ?
C4S C5S C6S 118.1(9) . . ?
C1S C6S C5S 118.4(8) . . ?
C2T C1T C6T 118.9(11) . . ?
C3T C2T C1T 122.4(12) . . ?
C2T C3T C4T 119.2(11) . . ?
C3T C4T C5T 122.2(12) . . ?
C4T C5T C6T 121.8(12) . . ?
C5T C6T C1T 115.3(12) . . ?

_refine_diff_density_max         0.877
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.100

####################################################################### 
# 
# 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_10113
_database_code_depnum_ccdc_archive 'CCDC 1421299'
_audit_update_record             
;
2015-08-28 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ONbODipp3Py
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H64 N Nb O5'
_chemical_formula_weight         791.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pna2(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   18.4033(17)
_cell_length_b                   23.170(2)
_cell_length_c                   10.0258(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4275.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9908
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      23.09

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1688
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8416
_exptl_absorpt_correction_T_max  0.9683
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 'Siemens three-circle diffractometer, Bruker APEX CCD' 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            67735
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         27.10
_reflns_number_total             9407
_reflns_number_gt                7423
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0354P)²+2.1559P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         9407
_refine_ls_number_parameters     481
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.0901
_refine_ls_wR_factor_gt          0.0801
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb -0.311505(13) 0.037229(10) -0.11320(4) 0.02548(7) Uani 1 1 d . . .
N1 N -0.36282(14) 0.03769(11) -0.3263(3) 0.0309(6) Uani 1 1 d . . .
O1 O -0.36961(13) -0.01675(10) -0.0680(2) 0.0405(7) Uani 1 1 d . . .
O1S O -0.0744(2) 0.2326(2) 0.5218(5) 0.129(2) Uani 1 1 d . . .
C1S C -0.0597(3) 0.2913(3) 0.5493(6) 0.0931(19) Uani 1 1 d . . .
H1S1 H -0.0759 0.3013 0.6406 0.112 Uiso 1 1 calc R . .
H1S2 H -0.0856 0.3165 0.4852 0.112 Uiso 1 1 calc R . .
O2 O -0.36194(10) 0.10910(8) -0.1035(3) 0.0381(5) Uani 1 1 d . . .
C2S C 0.0207(3) 0.2995(2) 0.5366(7) 0.0868(18) Uani 1 1 d . . .
H2S1 H 0.0323 0.3326 0.4780 0.104 Uiso 1 1 calc R . .
H2S2 H 0.0435 0.3056 0.6249 0.104 Uiso 1 1 calc R . .
O3 O -0.23117(11) 0.00902(9) -0.2160(2) 0.0286(5) Uani 1 1 d . . .
C3S C 0.0446(3) 0.2443(2) 0.4763(8) 0.109(2) Uani 1 1 d . . .
H3S1 H 0.0618 0.2510 0.3839 0.131 Uiso 1 1 calc R . .
H3S2 H 0.0852 0.2278 0.5286 0.131 Uiso 1 1 calc R . .
O4 O -0.25379(14) 0.04931(9) 0.0429(2) 0.0386(6) Uani 1 1 d . . .
C4S C -0.0095(3) 0.2093(3) 0.4758(10) 0.176(5) Uani 1 1 d . . .
H4S1 H 0.0029 0.1755 0.5318 0.211 Uiso 1 1 calc R . .
H4S2 H -0.0170 0.1952 0.3836 0.211 Uiso 1 1 calc R . .
C10 C -0.32542(19) 0.03581(15) -0.4402(4) 0.0381(8) Uani 1 1 d . . .
H10 H -0.2740 0.0330 -0.4363 0.046 Uiso 1 1 calc R . .
C11 C -0.3587(2) 0.03782(16) -0.5633(4) 0.0512(10) Uani 1 1 d . . .
H11 H -0.3306 0.0377 -0.6428 0.061 Uiso 1 1 calc R . .
C12 C -0.4326(3) 0.03997(17) -0.5689(5) 0.0629(15) Uani 1 1 d . . .
H12 H -0.4566 0.0403 -0.6529 0.076 Uiso 1 1 calc R . .
C13 C -0.4721(2) 0.04159(18) -0.4541(6) 0.0647(14) Uani 1 1 d . . .
H13 H -0.5237 0.0432 -0.4567 0.078 Uiso 1 1 calc R . .
C14 C -0.43595(19) 0.04088(15) -0.3351(5) 0.0461(10) Uani 1 1 d . . .
H14 H -0.4635 0.0427 -0.2551 0.055 Uiso 1 1 calc R . .
C20 C -0.38242(15) 0.16522(11) -0.1032(4) 0.0275(6) Uani 1 1 d . . .
C21 C -0.45000(18) 0.17908(14) -0.0462(3) 0.0323(7) Uani 1 1 d . . .
C22 C -0.4704(2) 0.23710(15) -0.0442(4) 0.0479(10) Uani 1 1 d . . .
H22 H -0.5154 0.2480 -0.0053 0.057 Uiso 1 1 calc R . .
C23 C -0.42543(19) 0.27896(14) -0.0987(6) 0.0563(11) Uani 1 1 d . . .
H23 H -0.4406 0.3181 -0.0996 0.068 Uiso 1 1 calc R . .
C24 C -0.35928(19) 0.26421(14) -0.1513(4) 0.0444(11) Uani 1 1 d . . .
H24 H -0.3287 0.2937 -0.1859 0.053 Uiso 1 1 calc R . .
C25 C -0.33563(18) 0.20707(14) -0.1553(3) 0.0321(8) Uani 1 1 d . . .
C30 C -0.16869(17) -0.02319(14) -0.2237(3) 0.0263(7) Uani 1 1 d . . .
C31 C -0.17304(17) -0.08085(14) -0.2616(4) 0.0310(7) Uani 1 1 d . . .
C32 C -0.10860(19) -0.11252(15) -0.2672(4) 0.0389(8) Uani 1 1 d . . .
H32 H -0.1102 -0.1523 -0.2903 0.047 Uiso 1 1 calc R . .
C33 C -0.0422(2) -0.08667(18) -0.2396(4) 0.0445(10) Uani 1 1 d . . .
H33 H 0.0012 -0.1087 -0.2448 0.053 Uiso 1 1 calc R . .
C34 C -0.03918(19) -0.02952(17) -0.2048(4) 0.0415(9) Uani 1 1 d . . .
H34 H 0.0067 -0.0123 -0.1872 0.050 Uiso 1 1 calc R . .
C35 C -0.10185(17) 0.00385(15) -0.1947(4) 0.0326(8) Uani 1 1 d . . .
C40 C -0.2181(2) 0.04368(14) 0.1604(3) 0.0333(8) Uani 1 1 d . . .
C41 C -0.19847(17) -0.01127(14) 0.2068(3) 0.0302(7) Uani 1 1 d . . .
C42 C -0.16435(18) -0.01481(16) 0.3311(4) 0.0354(8) Uani 1 1 d . . .
H42 H -0.1521 -0.0517 0.3660 0.042 Uiso 1 1 calc R . .
C43 C -0.14793(17) 0.03419(16) 0.4050(5) 0.0396(9) Uani 1 1 d . . .
H43 H -0.1248 0.0309 0.4893 0.047 Uiso 1 1 calc R . .
C44 C -0.16563(19) 0.08792(17) 0.3542(4) 0.0428(10) Uani 1 1 d . . .
H44 H -0.1540 0.1214 0.4045 0.051 Uiso 1 1 calc R . .
C45 C -0.19986(19) 0.09422(15) 0.2321(4) 0.0377(8) Uani 1 1 d . . .
C211 C -0.50052(18) 0.13289(15) 0.0081(4) 0.0398(9) Uani 1 1 d . . .
H211 H -0.4731 0.0956 0.0082 0.048 Uiso 1 1 calc R . .
C212 C -0.5235(2) 0.1452(2) 0.1518(4) 0.0582(12) Uani 1 1 d . . .
H21A H -0.4802 0.1507 0.2072 0.087 Uiso 1 1 calc R . .
H21B H -0.5517 0.1125 0.1860 0.087 Uiso 1 1 calc R . .
H21C H -0.5533 0.1802 0.1543 0.087 Uiso 1 1 calc R . .
C213 C -0.56619(19) 0.12543(17) -0.0843(5) 0.0589(15) Uani 1 1 d . . .
H21D H -0.5940 0.1615 -0.0872 0.088 Uiso 1 1 calc R . .
H21E H -0.5972 0.0943 -0.0504 0.088 Uiso 1 1 calc R . .
H21F H -0.5494 0.1157 -0.1742 0.088 Uiso 1 1 calc R . .
C251 C -0.26363(19) 0.19184(15) -0.2200(4) 0.0371(8) Uani 1 1 d . . .
H251 H -0.2505 0.1520 -0.1904 0.045 Uiso 1 1 calc R . .
C252 C -0.2703(3) 0.1907(2) -0.3707(4) 0.0595(12) Uani 1 1 d . . .
H25A H -0.3089 0.1638 -0.3965 0.089 Uiso 1 1 calc R . .
H25B H -0.2242 0.1780 -0.4098 0.089 Uiso 1 1 calc R . .
H25C H -0.2822 0.2294 -0.4032 0.089 Uiso 1 1 calc R . .
C253 C -0.2017(2) 0.23208(18) -0.1768(5) 0.0507(10) Uani 1 1 d . . .
H25D H -0.2108 0.2710 -0.2110 0.076 Uiso 1 1 calc R . .
H25E H -0.1556 0.2177 -0.2126 0.076 Uiso 1 1 calc R . .
H25F H -0.1991 0.2332 -0.0792 0.076 Uiso 1 1 calc R . .
C311 C -0.24572(19) -0.10936(15) -0.2950(4) 0.0415(9) Uani 1 1 d . . .
H311 H -0.2822 -0.0779 -0.3079 0.050 Uiso 1 1 calc R . .
C312 C -0.2727(2) -0.14727(19) -0.1822(4) 0.0557(12) Uani 1 1 d . . .
H31A H -0.3189 -0.1650 -0.2077 0.083 Uiso 1 1 calc R . .
H31B H -0.2797 -0.1238 -0.1020 0.083 Uiso 1 1 calc R . .
H31C H -0.2368 -0.1775 -0.1640 0.083 Uiso 1 1 calc R . .
C313 C -0.2426(3) -0.1438(2) -0.4230(4) 0.0710(15) Uani 1 1 d . . .
H31D H -0.2079 -0.1756 -0.4128 0.107 Uiso 1 1 calc R . .
H31E H -0.2269 -0.1187 -0.4962 0.107 Uiso 1 1 calc R . .
H31F H -0.2908 -0.1594 -0.4429 0.107 Uiso 1 1 calc R . .
C351 C -0.0973(2) 0.06720(16) -0.1577(4) 0.0466(11) Uani 1 1 d . . .
H351 H -0.1478 0.0808 -0.1387 0.056 Uiso 1 1 calc R . .
C352 C -0.0682(3) 0.10317(18) -0.2715(5) 0.0728(15) Uani 1 1 d . . .
H35A H -0.0194 0.0896 -0.2955 0.109 Uiso 1 1 calc R . .
H35B H -0.0657 0.1437 -0.2440 0.109 Uiso 1 1 calc R . .
H35C H -0.1005 0.0995 -0.3487 0.109 Uiso 1 1 calc R . .
C353 C -0.0523(3) 0.0769(2) -0.0319(5) 0.0623(13) Uani 1 1 d . . .
H35D H -0.0706 0.0520 0.0397 0.093 Uiso 1 1 calc R . .
H35E H -0.0562 0.1174 -0.0045 0.093 Uiso 1 1 calc R . .
H35F H -0.0014 0.0675 -0.0500 0.093 Uiso 1 1 calc R . .
C411 C -0.21532(18) -0.06525(15) 0.1264(4) 0.0334(8) Uani 1 1 d . . .
H411 H -0.2297 -0.0526 0.0347 0.040 Uiso 1 1 calc R . .
C412 C -0.2801(2) -0.09726(17) 0.1868(4) 0.0464(10) Uani 1 1 d . . .
H41A H -0.2687 -0.1084 0.2788 0.070 Uiso 1 1 calc R . .
H41B H -0.2903 -0.1319 0.1341 0.070 Uiso 1 1 calc R . .
H41C H -0.3228 -0.0720 0.1863 0.070 Uiso 1 1 calc R . .
C413 C -0.1486(2) -0.10389(16) 0.1125(4) 0.0453(10) Uani 1 1 d . . .
H41D H -0.1095 -0.0824 0.0685 0.068 Uiso 1 1 calc R . .
H41E H -0.1611 -0.1379 0.0589 0.068 Uiso 1 1 calc R . .
H41F H -0.1325 -0.1162 0.2011 0.068 Uiso 1 1 calc R . .
C451 C -0.2211(2) 0.15303(16) 0.1751(4) 0.0491(10) Uani 1 1 d . . .
H451 H -0.2218 0.1493 0.0757 0.059 Uiso 1 1 calc R . .
C452 C -0.2973(2) 0.16955(18) 0.2191(4) 0.0584(12) Uani 1 1 d . . .
H45A H -0.3314 0.1390 0.1935 0.088 Uiso 1 1 calc R . .
H45B H -0.3115 0.2058 0.1760 0.088 Uiso 1 1 calc R . .
H45C H -0.2982 0.1745 0.3162 0.088 Uiso 1 1 calc R . .
C453 C -0.1659(3) 0.20021(17) 0.2105(5) 0.0656(13) Uani 1 1 d . . .
H45D H -0.1790 0.2361 0.1648 0.098 Uiso 1 1 calc R . .
H45E H -0.1172 0.1881 0.1822 0.098 Uiso 1 1 calc R . .
H45F H -0.1661 0.2066 0.3071 0.098 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O1 1.707(2) . ?
Nb1 O2 1.9090(18) . ?
Nb1 O4 1.912(3) . ?
Nb1 O3 1.917(2) . ?
Nb1 N1 2.336(3) . ?
N1 C10 1.334(5) . ?
N1 C14 1.351(4) . ?
O1S C4S 1.390(6) . ?
O1S C1S 1.413(7) . ?
C1S C2S 1.496(7) . ?
O2 C20 1.354(3) . ?
C2S C3S 1.482(7) . ?
O3 C30 1.373(4) . ?
C3S C4S 1.285(7) . ?
O4 C40 1.354(4) . ?
C10 C11 1.379(5) . ?
C11 C12 1.362(6) . ?
C12 C13 1.362(7) . ?
C13 C14 1.366(6) . ?
C20 C25 1.398(4) . ?
C20 C21 1.406(4) . ?
C21 C22 1.396(5) . ?
C21 C211 1.519(5) . ?
C22 C23 1.387(5) . ?
C23 C24 1.370(5) . ?
C24 C25 1.394(4) . ?
C25 C251 1.517(5) . ?
C30 C31 1.391(4) . ?
C30 C35 1.411(4) . ?
C31 C32 1.396(4) . ?
C31 C311 1.529(5) . ?
C32 C33 1.388(5) . ?
C33 C34 1.370(5) . ?
C34 C35 1.392(5) . ?
C35 C351 1.516(5) . ?
C40 C41 1.403(5) . ?
C40 C45 1.415(5) . ?
C41 C42 1.398(5) . ?
C41 C411 1.520(5) . ?
C42 C43 1.389(5) . ?
C43 C44 1.384(5) . ?
C44 C45 1.384(5) . ?
C45 C451 1.529(5) . ?
C211 C212 1.527(6) . ?
C211 C213 1.533(5) . ?
C251 C252 1.516(6) . ?
C251 C253 1.535(5) . ?
C311 C313 1.513(6) . ?
C311 C312 1.515(6) . ?
C351 C352 1.511(6) . ?
C351 C353 1.525(6) . ?
C411 C413 1.525(5) . ?
C411 C412 1.529(5) . ?
C451 C452 1.519(6) . ?
C451 C453 1.535(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 O2 108.73(10) . . ?
O1 Nb1 O4 103.77(11) . . ?
O2 Nb1 O4 95.79(12) . . ?
O1 Nb1 O3 112.10(10) . . ?
O2 Nb1 O3 134.39(11) . . ?
O4 Nb1 O3 93.54(10) . . ?
O1 Nb1 N1 89.59(11) . . ?
O2 Nb1 N1 81.13(12) . . ?
O4 Nb1 N1 166.55(10) . . ?
O3 Nb1 N1 79.71(9) . . ?
C10 N1 C14 117.4(3) . . ?
C10 N1 Nb1 125.0(2) . . ?
C14 N1 Nb1 117.6(3) . . ?
C4S O1S C1S 105.9(4) . . ?
O1S C1S C2S 107.2(4) . . ?
C20 O2 Nb1 166.75(19) . . ?
C3S C2S C1S 102.7(5) . . ?
C30 O3 Nb1 149.5(2) . . ?
C4S C3S C2S 108.4(5) . . ?
C40 O4 Nb1 165.2(2) . . ?
C3S C4S O1S 114.8(6) . . ?
N1 C10 C11 122.4(3) . . ?
C12 C11 C10 118.8(4) . . ?
C11 C12 C13 119.9(4) . . ?
C12 C13 C14 118.5(4) . . ?
N1 C14 C13 122.9(4) . . ?
O2 C20 C25 119.6(3) . . ?
O2 C20 C21 117.8(3) . . ?
C25 C20 C21 122.6(3) . . ?
C22 C21 C20 117.6(3) . . ?
C22 C21 C211 120.6(3) . . ?
C20 C21 C211 121.8(3) . . ?
C23 C22 C21 120.5(3) . . ?
C24 C23 C22 120.5(3) . . ?
C23 C24 C25 121.7(3) . . ?
C24 C25 C20 117.1(3) . . ?
C24 C25 C251 120.4(3) . . ?
C20 C25 C251 122.4(3) . . ?
O3 C30 C31 119.3(3) . . ?
O3 C30 C35 118.5(3) . . ?
C31 C30 C35 122.2(3) . . ?
C30 C31 C32 117.8(3) . . ?
C30 C31 C311 121.7(3) . . ?
C32 C31 C311 120.5(3) . . ?
C33 C32 C31 120.8(3) . . ?
C34 C33 C32 120.2(3) . . ?
C33 C34 C35 121.4(3) . . ?
C34 C35 C30 117.4(3) . . ?
C34 C35 C351 120.6(3) . . ?
C30 C35 C351 121.9(3) . . ?
O4 C40 C41 120.1(3) . . ?
O4 C40 C45 118.5(3) . . ?
C41 C40 C45 121.4(3) . . ?
C42 C41 C40 117.7(3) . . ?
C42 C41 C411 121.1(3) . . ?
C40 C41 C411 121.2(3) . . ?
C43 C42 C41 121.7(3) . . ?
C44 C43 C42 119.2(4) . . ?
C43 C44 C45 121.8(4) . . ?
C44 C45 C40 118.0(3) . . ?
C44 C45 C451 122.8(3) . . ?
C40 C45 C451 119.1(3) . . ?
C21 C211 C212 112.1(3) . . ?
C21 C211 C213 110.2(3) . . ?
C212 C211 C213 111.9(3) . . ?
C252 C251 C25 111.1(3) . . ?
C252 C251 C253 110.6(3) . . ?
C25 C251 C253 112.8(3) . . ?
C313 C311 C312 109.9(3) . . ?
C313 C311 C31 112.3(3) . . ?
C312 C311 C31 111.9(3) . . ?
C352 C351 C35 111.6(3) . . ?
C352 C351 C353 110.5(3) . . ?
C35 C351 C353 112.0(3) . . ?
C41 C411 C413 111.5(3) . . ?
C41 C411 C412 110.4(3) . . ?
C413 C411 C412 112.2(3) . . ?
C452 C451 C45 110.6(3) . . ?
C452 C451 C453 111.4(3) . . ?
C45 C451 C453 112.2(4) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_D8_10142_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1421300'
_audit_update_record             
;
2015-08-28 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H53 N2 Nb O2 P3'
_chemical_formula_weight         815.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.1121 2.4826 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.0102(10)
_cell_length_b                   16.5289(12)
_cell_length_c                   18.0957(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.662(4)
_cell_angle_gamma                90
_cell_volume                     4186.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_F_000             1708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.707
_shelx_estimated_absorpt_T_min   0.524
_shelx_estimated_absorpt_T_max   0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5870
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 'Bruker D8 three-circle diffractometer, Bruker APEX CCD' 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube, graphite'
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            87281
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.623
_diffrn_reflns_theta_max         70.215
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             7782
_reflns_number_gt                6190
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 'Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
' 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0605P)²+0.9292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7782
_refine_ls_number_parameters     495
_refine_ls_number_restraints     276
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0923
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.58866(2) 0.68028(2) 0.86567(2) 0.02003(8) Uani 1 1 d . . . . .
P1 P 0.57710(7) 0.61517(5) 0.98974(4) 0.03333(19) Uani 1 1 d . . . . .
P2 P 0.51796(6) 0.73648(5) 0.98207(4) 0.02875(17) Uani 1 1 d . . . . .
P3 P 0.67140(6) 0.71863(5) 0.98774(4) 0.03066(18) Uani 1 1 d . . . . .
O1 O 0.70590(14) 0.66631(12) 0.81281(12) 0.0248(4) Uani 1 1 d . . . . .
O2 O 0.46921(14) 0.69569(12) 0.80660(11) 0.0226(4) Uani 1 1 d . . . . .
N3 N 0.56239(18) 0.54880(15) 0.82267(15) 0.0264(5) Uani 1 1 d . . . . .
N4 N 0.61399(18) 0.81696(14) 0.84760(14) 0.0250(5) Uani 1 1 d . . . . .
C11 C 0.7882(2) 0.67209(17) 0.77760(17) 0.0250(6) Uani 1 1 d . . . . .
C12 C 0.8750(2) 0.64723(18) 0.81371(17) 0.0264(6) Uani 1 1 d . . . . .
C13 C 0.9582(2) 0.65083(18) 0.77436(18) 0.0291(7) Uani 1 1 d . . . . .
H13 H 1.0169 0.6337 0.7976 0.035 Uiso 1 1 calc R U . . .
C14 C 0.9570(2) 0.67889(19) 0.70215(19) 0.0321(7) Uani 1 1 d . . . . .
H14 H 1.0146 0.6815 0.6766 0.039 Uiso 1 1 calc R U . . .
C15 C 0.8718(2) 0.70299(18) 0.66742(18) 0.0301(7) Uani 1 1 d . . . . .
H15 H 0.8715 0.7219 0.6178 0.036 Uiso 1 1 calc R U . . .
C16 C 0.7863(2) 0.70012(17) 0.70361(18) 0.0267(6) Uani 1 1 d . . . . .
C21 C 0.3766(2) 0.71633(18) 0.79415(16) 0.0239(6) Uani 1 1 d . . . . .
C22 C 0.3517(2) 0.76890(18) 0.73469(17) 0.0258(6) Uani 1 1 d . . . . .
C23 C 0.2560(2) 0.78976(19) 0.72266(19) 0.0315(7) Uani 1 1 d . . . . .
H23 H 0.2379 0.8249 0.6829 0.038 Uiso 1 1 calc R U . . .
C24 C 0.1866(2) 0.7603(2) 0.7675(2) 0.0359(8) Uani 1 1 d . . . . .
H24 H 0.1219 0.7768 0.7597 0.043 Uiso 1 1 calc R U . . .
C25 C 0.2118(2) 0.7067(2) 0.8236(2) 0.0338(7) Uani 1 1 d . . . . .
H25 H 0.1635 0.6862 0.8536 0.041 Uiso 1 1 calc R U . . .
C26 C 0.3059(2) 0.68187(18) 0.83748(17) 0.0265(6) Uani 1 1 d . . . . .
C31 C 0.5606(2) 0.47857(19) 0.8597(2) 0.0330(7) Uani 1 1 d . . . . .
H31 H 0.5691 0.4798 0.9121 0.040 Uiso 1 1 calc R U . . .
C32 C 0.5470(3) 0.4043(2) 0.8253(2) 0.0401(8) Uani 1 1 d . . . . .
H32 H 0.5459 0.3560 0.8537 0.048 Uiso 1 1 calc R U . . .
C33 C 0.5351(3) 0.4015(2) 0.7492(2) 0.0435(9) Uani 1 1 d . . . . .
H33 H 0.5266 0.3514 0.7241 0.052 Uiso 1 1 calc R U . . .
C34 C 0.5358(3) 0.4731(2) 0.7108(2) 0.0436(9) Uani 1 1 d . . . . .
H34 H 0.5268 0.4732 0.6584 0.052 Uiso 1 1 calc R U . . .
C35 C 0.5496(3) 0.5450(2) 0.74887(19) 0.0350(7) Uani 1 1 d . . . . .
H35 H 0.5501 0.5940 0.7215 0.042 Uiso 1 1 calc R U . . .
C41 C 0.5397(2) 0.86878(18) 0.83964(17) 0.0269(6) Uani 1 1 d . . . . .
H41 H 0.4767 0.8478 0.8408 0.032 Uiso 1 1 calc R U . . .
C42 C 0.5514(3) 0.9514(2) 0.82983(18) 0.0330(7) Uani 1 1 d . . . . .
H42 H 0.4975 0.9860 0.8240 0.040 Uiso 1 1 calc R U . . .
C43 C 0.6425(3) 0.98205(19) 0.82874(18) 0.0340(7) Uani 1 1 d . . . . .
H43 H 0.6525 1.0384 0.8221 0.041 Uiso 1 1 calc R U . . .
C44 C 0.7192(3) 0.9302(2) 0.8374(2) 0.0359(7) Uani 1 1 d . . . . .
H44 H 0.7828 0.9502 0.8371 0.043 Uiso 1 1 calc R U . . .
C45 C 0.7019(2) 0.84820(18) 0.84657(18) 0.0291(7) Uani 1 1 d . . . . .
H45 H 0.7549 0.8126 0.8524 0.035 Uiso 1 1 calc R U . . .
C121 C 0.8740(2) 0.6126(2) 0.89155(18) 0.0310(7) Uani 1 1 d . . . . .
H121 H 0.8292 0.6462 0.9202 0.037 Uiso 1 1 calc R U . . .
C122 C 0.9713(3) 0.6140(2) 0.9332(2) 0.0413(8) Uani 1 1 d . . . . .
H12A H 1.0144 0.5759 0.9101 0.062 Uiso 1 1 calc R U . . .
H12B H 0.9637 0.5984 0.9848 0.062 Uiso 1 1 calc R U . . .
H12C H 0.9982 0.6687 0.9314 0.062 Uiso 1 1 calc R U . . .
C123 C 0.8351(3) 0.5259(2) 0.8887(2) 0.0412(8) Uani 1 1 d . . . . .
H12D H 0.7719 0.5256 0.8630 0.062 Uiso 1 1 calc R U . . .
H12E H 0.8297 0.5055 0.9392 0.062 Uiso 1 1 calc R U . . .
H12F H 0.8787 0.4913 0.8621 0.062 Uiso 1 1 calc R U . . .
C161 C 0.6935(2) 0.72370(18) 0.66311(18) 0.0286(6) Uani 1 1 d . . . . .
H161 H 0.6402 0.7123 0.6965 0.034 Uiso 1 1 calc R U . . .
C162 C 0.6909(3) 0.81409(19) 0.64442(19) 0.0352(7) Uani 1 1 d . . . . .
H16A H 0.6931 0.8457 0.6903 0.053 Uiso 1 1 calc R U . . .
H16B H 0.6319 0.8265 0.6155 0.053 Uiso 1 1 calc R U . . .
H16C H 0.7461 0.8279 0.6155 0.053 Uiso 1 1 calc R U . . .
C163 C 0.6772(3) 0.6723(2) 0.5931(2) 0.0419(8) Uani 1 1 d . . . . .
H16D H 0.7286 0.6825 0.5594 0.063 Uiso 1 1 calc R U . . .
H16E H 0.6157 0.6867 0.5686 0.063 Uiso 1 1 calc R U . . .
H16F H 0.6769 0.6149 0.6066 0.063 Uiso 1 1 calc R U . . .
C221 C 0.4258(2) 0.79653(19) 0.68182(18) 0.0299(7) Uani 1 1 d . . . . .
H221 H 0.4902 0.7919 0.7077 0.036 Uiso 1 1 calc R U . . .
C222 C 0.4118(3) 0.8848(2) 0.6567(2) 0.0390(8) Uani 1 1 d . . . . .
H22A H 0.3532 0.8892 0.6252 0.058 Uiso 1 1 calc R U . . .
H22B H 0.4666 0.9019 0.6287 0.058 Uiso 1 1 calc R U . . .
H22C H 0.4068 0.9197 0.7001 0.058 Uiso 1 1 calc R U . . .
C223 C 0.4232(3) 0.7396(2) 0.6144(2) 0.0404(8) Uani 1 1 d . . . . .
H22D H 0.4362 0.6840 0.6310 0.061 Uiso 1 1 calc R U . . .
H22E H 0.4718 0.7564 0.5804 0.061 Uiso 1 1 calc R U . . .
H22F H 0.3600 0.7421 0.5890 0.061 Uiso 1 1 calc R U . . .
C261 C 0.3287(2) 0.6145(2) 0.89248(17) 0.0298(7) Uani 1 1 d . . . . .
H261 H 0.3994 0.6145 0.9030 0.036 Uiso 1 1 calc R U . . .
C262 C 0.2814(3) 0.6268(3) 0.9661(2) 0.0495(10) Uani 1 1 d . . . . .
H26A H 0.2985 0.6802 0.9861 0.074 Uiso 1 1 calc R U . . .
H26B H 0.3035 0.5849 1.0012 0.074 Uiso 1 1 calc R U . . .
H26C H 0.2118 0.6231 0.9582 0.074 Uiso 1 1 calc R U . . .
C263 C 0.3017(3) 0.5324(2) 0.8573(2) 0.0444(9) Uani 1 1 d . . . . .
H26D H 0.2329 0.5311 0.8449 0.067 Uiso 1 1 calc R U . . .
H26E H 0.3182 0.4889 0.8924 0.067 Uiso 1 1 calc R U . . .
H26F H 0.3368 0.5248 0.8122 0.067 Uiso 1 1 calc R U . . .
C1S C 0.4390(5) 0.3920(4) 0.5587(4) 0.0470(17) Uani 0.5 1 d D U P A -1
H1S H 0.3898 0.3609 0.5794 0.056 Uiso 0.5 1 calc R U P A -1
C2S C 0.5288(6) 0.3584(5) 0.5505(4) 0.0529(18) Uani 0.5 1 d D U P A -1
H2S H 0.5414 0.3042 0.5654 0.063 Uiso 0.5 1 calc R U P A -1
C3S C 0.5991(6) 0.4043(5) 0.5208(4) 0.0545(19) Uani 0.5 1 d D U P A -1
H3S H 0.6606 0.3813 0.5153 0.065 Uiso 0.5 1 calc R U P A -1
C4S C 0.5824(5) 0.4824(5) 0.4989(4) 0.0488(17) Uani 0.5 1 d D U P A -1
H4S H 0.6311 0.5132 0.4772 0.059 Uiso 0.5 1 calc R U P A -1
C5S C 0.4934(7) 0.5157(6) 0.5088(6) 0.052(2) Uani 0.5 1 d D U P A -1
H5S H 0.4818 0.5707 0.4960 0.062 Uiso 0.5 1 calc R U P A -1
C6S C 0.4219(6) 0.4704(5) 0.5368(4) 0.0488(17) Uani 0.5 1 d D U P A -1
H6S H 0.3601 0.4933 0.5411 0.059 Uiso 0.5 1 calc R U P A -1
C1T C 0.3561(3) 0.9554(2) 0.9595(2) 0.0443(8) Uani 1 1 d D U . . .
H1T H 0.3815 0.9229 0.9990 0.053 Uiso 1 1 calc R U . . .
C2T C 0.3670(3) 1.0391(2) 0.9623(2) 0.0406(8) Uani 1 1 d D U . . .
H2T H 0.4000 1.0637 1.0035 0.049 Uiso 1 1 calc R U . . .
C3T C 0.3293(3) 1.0864(2) 0.90467(19) 0.0384(8) Uani 1 1 d D U . . .
H3T H 0.3364 1.1436 0.9064 0.046 Uiso 1 1 calc R U . . .
C4T C 0.2816(3) 1.0504(2) 0.84483(19) 0.0411(8) Uani 1 1 d D U . . .
H4T H 0.2553 1.0827 0.8056 0.049 Uiso 1 1 calc R U . . .
C5T C 0.2720(3) 0.9671(2) 0.8420(2) 0.0447(9) Uani 1 1 d D U . . .
H5T H 0.2400 0.9425 0.8004 0.054 Uiso 1 1 calc R U . . .
C6T C 0.3084(3) 0.9195(2) 0.8994(2) 0.0433(8) Uani 1 1 d D U . . .
H6T H 0.3008 0.8624 0.8976 0.052 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O1 1.953(2) . ?
Nb1 O2 1.9600(19) . ?
Nb1 N4 2.313(2) . ?
Nb1 N3 2.332(2) . ?
Nb1 P1 2.5018(8) . ?
Nb1 P3 2.5273(8) . ?
Nb1 P2 2.5444(8) . ?
P1 P3 2.1623(12) . ?
P1 P2 2.1716(12) . ?
P2 P3 2.1676(12) . ?
O1 C11 1.346(4) . ?
O2 C21 1.351(3) . ?
N3 C35 1.341(4) . ?
N3 C31 1.342(4) . ?
N4 C45 1.336(4) . ?
N4 C41 1.350(4) . ?
C11 C12 1.415(4) . ?
C11 C16 1.416(4) . ?
C12 C13 1.395(4) . ?
C12 C121 1.521(4) . ?
C13 C14 1.386(5) . ?
C14 C15 1.381(5) . ?
C15 C16 1.393(5) . ?
C16 C161 1.513(4) . ?
C21 C26 1.411(4) . ?
C21 C22 1.414(4) . ?
C22 C23 1.392(4) . ?
C22 C221 1.515(4) . ?
C23 C24 1.383(5) . ?
C24 C25 1.381(5) . ?
C25 C26 1.392(4) . ?
C26 C261 1.518(4) . ?
C31 C32 1.386(5) . ?
C32 C33 1.380(6) . ?
C33 C34 1.372(5) . ?
C34 C35 1.384(5) . ?
C41 C42 1.387(4) . ?
C42 C43 1.375(5) . ?
C43 C44 1.377(5) . ?
C44 C45 1.388(4) . ?
C121 C122 1.526(4) . ?
C121 C123 1.534(5) . ?
C161 C162 1.532(4) . ?
C161 C163 1.533(5) . ?
C221 C222 1.539(4) . ?
C221 C223 1.540(5) . ?
C261 C262 1.529(5) . ?
C261 C263 1.539(5) . ?
C1S C6S 1.374(9) . ?
C1S C2S 1.389(9) . ?
C2S C3S 1.373(9) . ?
C3S C4S 1.368(10) . ?
C4S C5S 1.382(10) . ?
C5S C6S 1.367(10) . ?
C1T C6T 1.384(5) . ?
C1T C2T 1.392(5) . ?
C2T C3T 1.389(5) . ?
C3T C4T 1.381(5) . ?
C4T C5T 1.383(5) . ?
C5T C6T 1.382(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 O2 117.68(9) . . ?
O1 Nb1 N4 84.73(9) . . ?
O2 Nb1 N4 85.91(9) . . ?
O1 Nb1 N3 81.35(9) . . ?
O2 Nb1 N3 79.72(9) . . ?
N4 Nb1 N3 152.40(9) . . ?
O1 Nb1 P1 118.67(7) . . ?
O2 Nb1 P1 117.13(6) . . ?
N4 Nb1 P1 124.33(7) . . ?
N3 Nb1 P1 83.27(7) . . ?
O1 Nb1 P3 95.49(7) . . ?
O2 Nb1 P3 142.13(6) . . ?
N4 Nb1 P3 79.13(7) . . ?
N3 Nb1 P3 125.75(7) . . ?
P1 Nb1 P3 50.93(3) . . ?
O1 Nb1 P2 144.83(7) . . ?
O2 Nb1 P2 92.79(6) . . ?
N4 Nb1 P2 80.13(7) . . ?
N3 Nb1 P2 123.71(7) . . ?
P1 Nb1 P2 50.97(3) . . ?
P3 Nb1 P2 50.60(3) . . ?
P3 P1 P2 60.02(4) . . ?
P3 P1 Nb1 65.15(3) . . ?
P2 P1 Nb1 65.53(3) . . ?
P3 P2 P1 59.78(4) . . ?
P3 P2 Nb1 64.29(3) . . ?
P1 P2 Nb1 63.50(3) . . ?
P1 P3 P2 60.20(4) . . ?
P1 P3 Nb1 63.93(3) . . ?
P2 P3 Nb1 65.11(3) . . ?
C11 O1 Nb1 169.07(18) . . ?
C21 O2 Nb1 155.96(19) . . ?
C35 N3 C31 117.0(3) . . ?
C35 N3 Nb1 112.8(2) . . ?
C31 N3 Nb1 130.2(2) . . ?
C45 N4 C41 117.3(3) . . ?
C45 N4 Nb1 121.8(2) . . ?
C41 N4 Nb1 120.8(2) . . ?
O1 C11 C12 119.8(3) . . ?
O1 C11 C16 119.5(3) . . ?
C12 C11 C16 120.6(3) . . ?
C13 C12 C11 118.2(3) . . ?
C13 C12 C121 122.2(3) . . ?
C11 C12 C121 119.5(3) . . ?
C14 C13 C12 121.4(3) . . ?
C15 C14 C13 119.9(3) . . ?
C14 C15 C16 121.4(3) . . ?
C15 C16 C11 118.5(3) . . ?
C15 C16 C161 120.1(3) . . ?
C11 C16 C161 121.3(3) . . ?
O2 C21 C26 119.9(3) . . ?
O2 C21 C22 118.9(3) . . ?
C26 C21 C22 121.1(3) . . ?
C23 C22 C21 118.2(3) . . ?
C23 C22 C221 120.7(3) . . ?
C21 C22 C221 120.9(3) . . ?
C24 C23 C22 121.3(3) . . ?
C25 C24 C23 119.6(3) . . ?
C24 C25 C26 122.0(3) . . ?
C25 C26 C21 117.6(3) . . ?
C25 C26 C261 120.2(3) . . ?
C21 C26 C261 121.9(3) . . ?
N3 C31 C32 123.1(3) . . ?
C33 C32 C31 119.1(3) . . ?
C34 C33 C32 118.3(3) . . ?
C33 C34 C35 119.5(4) . . ?
N3 C35 C34 123.0(3) . . ?
N4 C41 C42 122.9(3) . . ?
C43 C42 C41 118.7(3) . . ?
C42 C43 C44 119.2(3) . . ?
C43 C44 C45 118.8(3) . . ?
N4 C45 C44 123.1(3) . . ?
C12 C121 C122 113.9(3) . . ?
C12 C121 C123 109.8(3) . . ?
C122 C121 C123 109.8(3) . . ?
C16 C161 C162 111.6(3) . . ?
C16 C161 C163 110.4(3) . . ?
C162 C161 C163 110.9(3) . . ?
C22 C221 C222 113.0(3) . . ?
C22 C221 C223 108.9(3) . . ?
C222 C221 C223 110.3(3) . . ?
C26 C261 C262 112.8(3) . . ?
C26 C261 C263 109.6(3) . . ?
C262 C261 C263 111.7(3) . . ?
C6S C1S C2S 119.6(7) . . ?
C3S C2S C1S 119.4(8) . . ?
C4S C3S C2S 121.2(8) . . ?
C3S C4S C5S 118.9(8) . . ?
C6S C5S C4S 120.7(9) . . ?
C5S C6S C1S 120.2(8) . . ?
C6T C1T C2T 120.2(4) . . ?
C3T C2T C1T 119.7(3) . . ?
C4T C3T C2T 119.9(3) . . ?
C3T C4T C5T 120.1(4) . . ?
C6T C5T C4T 120.5(3) . . ?
C5T C6T C1T 119.7(3) . . ?

_refine_diff_density_max         0.351
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.074

_shelxl_version_number           2014-2

####################################################################### 
# 
# 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_final
_database_code_depnum_ccdc_archive 'CCDC 1421301'
_audit_update_record             
;
2015-08-28 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78.24 H108.49 Nb2 O6 P6 Sn'
_chemical_formula_weight         1635.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.234(2)
_cell_length_b                   20.735(2)
_cell_length_c                   20.601(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.989(2)
_cell_angle_gamma                90.00
_cell_volume                     8205.0(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9682
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      30.32

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3392
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9034
_exptl_absorpt_correction_T_max  0.9853
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. 
 The instrument was purchased with the help of funding from the 
 National Science Foundation (NSF) under Grant Number 
 CHE-0946721.  Please acknowledge this grant in all publications 
 of this structure. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            193614
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         30.61
_reflns_number_total             25131
_reflns_number_gt                18222
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2010.7.0 (Bruker-AXS, 2010)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2010)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0197P)²+8.4337P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         25131
_refine_ls_number_parameters     888
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0796
_refine_ls_wR_factor_gt          0.0692
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb -0.408867(10) 0.684020(9) 0.748205(10) 0.01956(4) Uani 1 1 d . . .
Nb2 Nb -0.001532(10) 0.700630(9) 0.570395(9) 0.01722(4) Uani 1 1 d . . .
Sn1 Sn -0.205146(9) 0.785626(8) 0.667136(8) 0.02649(4) Uani 1 1 d . . .
P1 P -0.27803(3) 0.70941(3) 0.75297(3) 0.02373(12) Uani 1 1 d . . .
P2 P -0.33230(4) 0.72436(4) 0.65709(3) 0.03490(16) Uani 1 1 d . . .
P3 P -0.34822(4) 0.79179(3) 0.73677(4) 0.03857(17) Uani 1 1 d . . .
P4 P -0.10271(3) 0.77979(3) 0.56321(3) 0.02515(12) Uani 1 1 d . . .
P5 P -0.04979(3) 0.77008(3) 0.65916(3) 0.02829(13) Uani 1 1 d . . .
P6 P -0.12112(3) 0.69322(3) 0.62223(3) 0.02835(14) Uani 1 1 d . . .
O1 O -0.42909(8) 0.68695(8) 0.83648(7) 0.0243(3) Uani 1 1 d . . .
O2 O -0.49423(8) 0.70511(8) 0.70364(8) 0.0261(3) Uani 1 1 d . . .
O3 O -0.39257(8) 0.59413(7) 0.73604(7) 0.0220(3) Uani 1 1 d . . .
O4 O -0.03382(8) 0.64904(7) 0.49837(7) 0.0201(3) Uani 1 1 d . . .
O5 O 0.04805(8) 0.64663(7) 0.63219(7) 0.0211(3) Uani 1 1 d . . .
O6 O 0.06845(8) 0.75339(7) 0.53722(7) 0.0204(3) Uani 1 1 d . . .
C11 C -0.43927(12) 0.67410(11) 0.90059(11) 0.0257(5) Uani 1 1 d . . .
C12 C -0.39199(13) 0.69882(12) 0.94762(12) 0.0285(5) Uani 1 1 d . . .
C13 C -0.40262(15) 0.68279(14) 1.01233(12) 0.0373(6) Uani 1 1 d . . .
H13 H -0.3710 0.6983 1.0458 0.045 Uiso 1 1 calc R . .
C14 C -0.45825(17) 0.64485(15) 1.02852(14) 0.0454(7) Uani 1 1 d . . .
H14 H -0.4645 0.6345 1.0728 0.054 Uiso 1 1 calc R . .
C15 C -0.50486(16) 0.62191(14) 0.98046(15) 0.0436(7) Uani 1 1 d . . .
H15 H -0.5429 0.5960 0.9922 0.052 Uiso 1 1 calc R . .
C16 C -0.49677(13) 0.63633(12) 0.91496(13) 0.0318(6) Uani 1 1 d . . .
C21 C -0.53975(12) 0.74587(12) 0.67059(12) 0.0264(5) Uani 1 1 d . B .
C22 C -0.56278(14) 0.80162(13) 0.70159(13) 0.0344(6) Uani 1 1 d . . .
C23 C -0.61148(15) 0.84041(14) 0.66719(14) 0.0415(7) Uani 1 1 d . B .
H23 H -0.6287 0.8781 0.6871 0.050 Uiso 1 1 calc R . .
C24 C -0.63482(14) 0.82482(14) 0.60485(13) 0.0371(6) Uani 1 1 d . . .
H24 H -0.6681 0.8516 0.5823 0.045 Uiso 1 1 calc R B .
C25 C -0.61020(13) 0.77083(13) 0.57501(13) 0.0320(5) Uani 1 1 d . B .
H25 H -0.6261 0.7613 0.5316 0.038 Uiso 1 1 calc R . .
C26 C -0.56252(13) 0.72977(12) 0.60686(12) 0.0279(5) Uani 1 1 d . . .
C31 C -0.34623(11) 0.54421(10) 0.73005(11) 0.0210(4) Uani 1 1 d . . .
C32 C -0.30672(12) 0.52270(10) 0.78501(11) 0.0234(5) Uani 1 1 d . . .
C33 C -0.26262(12) 0.47017(11) 0.77713(12) 0.0258(5) Uani 1 1 d . . .
H33 H -0.2354 0.4545 0.8136 0.031 Uiso 1 1 calc R . .
C34 C -0.25773(12) 0.44039(11) 0.71742(12) 0.0283(5) Uani 1 1 d . . .
H34 H -0.2272 0.4048 0.7130 0.034 Uiso 1 1 calc R . .
C35 C -0.29752(12) 0.46273(11) 0.66400(12) 0.0279(5) Uani 1 1 d . . .
H35 H -0.2937 0.4421 0.6231 0.033 Uiso 1 1 calc R . .
C36 C -0.34300(12) 0.51476(11) 0.66886(11) 0.0231(5) Uani 1 1 d . C .
C41 C -0.08892(12) 0.63473(11) 0.45573(11) 0.0232(5) Uani 1 1 d . . .
C42 C -0.12770(12) 0.57849(11) 0.46528(12) 0.0268(5) Uani 1 1 d . . .
C43 C -0.18279(14) 0.56496(14) 0.42034(14) 0.0387(6) Uani 1 1 d . . .
H43 H -0.2101 0.5274 0.4257 0.046 Uiso 1 1 calc R . .
C44 C -0.19798(16) 0.60532(16) 0.36838(15) 0.0468(8) Uani 1 1 d . . .
H44 H -0.2358 0.5956 0.3385 0.056 Uiso 1 1 calc R . .
C45 C -0.15827(16) 0.65978(15) 0.35968(14) 0.0433(7) Uani 1 1 d . . .
H45 H -0.1690 0.6868 0.3233 0.052 Uiso 1 1 calc R . .
C46 C -0.10272(13) 0.67621(12) 0.40281(11) 0.0297(5) Uani 1 1 d . . .
C51 C 0.06563(12) 0.63763(11) 0.69714(11) 0.0225(4) Uani 1 1 d . . .
C52 C 0.12371(12) 0.67042(11) 0.72495(11) 0.0260(5) Uani 1 1 d . . .
C53 C 0.13968(14) 0.66163(13) 0.79098(12) 0.0328(6) Uani 1 1 d . . .
H53 H 0.1789 0.6832 0.8108 0.039 Uiso 1 1 calc R . .
C54 C 0.09966(15) 0.62214(13) 0.82851(12) 0.0363(6) Uani 1 1 d . . .
H54 H 0.1105 0.6178 0.8738 0.044 Uiso 1 1 calc R . .
C55 C 0.04393(14) 0.58911(12) 0.79944(12) 0.0331(6) Uani 1 1 d . . .
H55 H 0.0174 0.5615 0.8253 0.040 Uiso 1 1 calc R . .
C56 C 0.02549(13) 0.59506(11) 0.73341(11) 0.0258(5) Uani 1 1 d . . .
C61 C 0.11968(11) 0.79369(10) 0.51680(10) 0.0189(4) Uani 1 1 d . . .
C62 C 0.11558(12) 0.86002(10) 0.52955(10) 0.0209(4) Uani 1 1 d . . .
C63 C 0.16934(12) 0.89922(11) 0.50889(11) 0.0244(5) Uani 1 1 d . . .
H63 H 0.1681 0.9443 0.5171 0.029 Uiso 1 1 calc R . .
C64 C 0.22427(12) 0.87352(11) 0.47666(12) 0.0274(5) Uani 1 1 d . . .
H64 H 0.2604 0.9008 0.4631 0.033 Uiso 1 1 calc R . .
C65 C 0.22638(12) 0.80804(11) 0.46428(12) 0.0275(5) Uani 1 1 d . . .
H65 H 0.2640 0.7910 0.4416 0.033 Uiso 1 1 calc R . .
C66 C 0.17471(12) 0.76616(11) 0.48419(11) 0.0221(4) Uani 1 1 d . . .
C121 C -0.33460(13) 0.74409(13) 0.92793(12) 0.0304(5) Uani 1 1 d . . .
H121 H -0.3159 0.7267 0.8870 0.036 Uiso 1 1 calc R . .
C122 C -0.36557(15) 0.81092(13) 0.91219(15) 0.0404(6) Uani 1 1 d . . .
H12A H -0.4034 0.8067 0.8787 0.061 Uiso 1 1 calc R . .
H12B H -0.3293 0.8391 0.8962 0.061 Uiso 1 1 calc R . .
H12C H -0.3838 0.8296 0.9516 0.061 Uiso 1 1 calc R . .
C123 C -0.27363(15) 0.74975(16) 0.97790(13) 0.0421(7) Uani 1 1 d . . .
H12D H -0.2893 0.7705 1.0173 0.063 Uiso 1 1 calc R . .
H12E H -0.2367 0.7757 0.9598 0.063 Uiso 1 1 calc R . .
H12F H -0.2557 0.7066 0.9887 0.063 Uiso 1 1 calc R . .
C261 C -0.53629(15) 0.66799(13) 0.57664(13) 0.0360(6) Uani 1 1 d . B .
H261 H -0.4866 0.6620 0.5922 0.043 Uiso 1 1 calc R . .
C262 C -0.53869(17) 0.67105(15) 0.50226(13) 0.0447(7) Uani 1 1 d . . .
H26A H -0.5872 0.6692 0.4853 0.067 Uiso 1 1 calc R B .
H26B H -0.5129 0.6345 0.4854 0.067 Uiso 1 1 calc R . .
H26C H -0.5175 0.7114 0.4885 0.067 Uiso 1 1 calc R . .
C263 C -0.5774(2) 0.61049(15) 0.60026(16) 0.0541(9) Uani 1 1 d . . .
H26D H -0.5725 0.6081 0.6478 0.081 Uiso 1 1 calc R B .
H26E H -0.5595 0.5707 0.5816 0.081 Uiso 1 1 calc R . .
H26F H -0.6267 0.6156 0.5866 0.081 Uiso 1 1 calc R . .
C321 C -0.31131(13) 0.55334(11) 0.85170(11) 0.0270(5) Uani 1 1 d . . .
H321 H -0.3437 0.5910 0.8470 0.032 Uiso 1 1 calc R . .
C322 C -0.34164(15) 0.50613(14) 0.90050(13) 0.0388(6) Uani 1 1 d . . .
H32A H -0.3856 0.4884 0.8820 0.058 Uiso 1 1 calc R . .
H32B H -0.3501 0.5290 0.9410 0.058 Uiso 1 1 calc R . .
H32C H -0.3085 0.4709 0.9096 0.058 Uiso 1 1 calc R . .
C323 C -0.24034(14) 0.57871(13) 0.87809(13) 0.0342(6) Uani 1 1 d . . .
H32D H -0.2084 0.5424 0.8861 0.051 Uiso 1 1 calc R . .
H32E H -0.2461 0.6020 0.9188 0.051 Uiso 1 1 calc R . .
H32F H -0.2211 0.6079 0.8462 0.051 Uiso 1 1 calc R . .
C421 C -0.10866(13) 0.53152(11) 0.51933(13) 0.0289(5) Uani 1 1 d . . .
H421 H -0.0684 0.5501 0.5458 0.035 Uiso 1 1 calc R . .
C422 C -0.08506(14) 0.46732(12) 0.49101(16) 0.0403(7) Uani 1 1 d . . .
H42A H -0.1242 0.4472 0.4663 0.060 Uiso 1 1 calc R . .
H42B H -0.0689 0.4386 0.5264 0.060 Uiso 1 1 calc R . .
H42C H -0.0470 0.4751 0.4622 0.060 Uiso 1 1 calc R . .
C423 C -0.16797(14) 0.52016(13) 0.56475(14) 0.0391(6) Uani 1 1 d . . .
H42D H -0.1809 0.5612 0.5845 0.059 Uiso 1 1 calc R . .
H42E H -0.1527 0.4897 0.5990 0.059 Uiso 1 1 calc R . .
H42F H -0.2083 0.5023 0.5399 0.059 Uiso 1 1 calc R . .
C461 C -0.05646(15) 0.73309(12) 0.39031(12) 0.0333(6) Uani 1 1 d . . .
H461 H -0.0343 0.7464 0.4332 0.040 Uiso 1 1 calc R . .
C462 C -0.0947(2) 0.79149(15) 0.36218(18) 0.0598(10) Uani 1 1 d . . .
H46A H -0.1152 0.7810 0.3189 0.090 Uiso 1 1 calc R . .
H46B H -0.0619 0.8274 0.3588 0.090 Uiso 1 1 calc R . .
H46C H -0.1317 0.8039 0.3907 0.090 Uiso 1 1 calc R . .
C463 C 0.0025(2) 0.71216(18) 0.3475(2) 0.0754(13) Uani 1 1 d . . .
H46D H 0.0295 0.6776 0.3693 0.113 Uiso 1 1 calc R . .
H46E H 0.0330 0.7490 0.3403 0.113 Uiso 1 1 calc R . .
H46F H -0.0174 0.6965 0.3057 0.113 Uiso 1 1 calc R . .
C521 C 0.16895(14) 0.71343(13) 0.68481(13) 0.0344(6) Uani 1 1 d . . .
H521 H 0.1545 0.7068 0.6379 0.041 Uiso 1 1 calc R . .
C522 C 0.15812(19) 0.78468(14) 0.70074(15) 0.0514(8) Uani 1 1 d . . .
H52A H 0.1086 0.7954 0.6944 0.077 Uiso 1 1 calc R . .
H52B H 0.1852 0.8114 0.6720 0.077 Uiso 1 1 calc R . .
H52C H 0.1736 0.7929 0.7461 0.077 Uiso 1 1 calc R . .
C523 C 0.24607(15) 0.69535(19) 0.69422(16) 0.0557(9) Uani 1 1 d . . .
H52D H 0.2619 0.7027 0.7396 0.083 Uiso 1 1 calc R . .
H52E H 0.2735 0.7220 0.6657 0.083 Uiso 1 1 calc R . .
H52F H 0.2521 0.6497 0.6834 0.083 Uiso 1 1 calc R . .
C561 C -0.03303(13) 0.55507(11) 0.70224(12) 0.0285(5) Uani 1 1 d . . .
H561 H -0.0433 0.5721 0.6573 0.034 Uiso 1 1 calc R . .
C562 C -0.09992(14) 0.56027(14) 0.73924(13) 0.0384(6) Uani 1 1 d . . .
H56A H -0.0919 0.5422 0.7829 0.058 Uiso 1 1 calc R . .
H56B H -0.1373 0.5362 0.7159 0.058 Uiso 1 1 calc R . .
H56C H -0.1134 0.6057 0.7426 0.058 Uiso 1 1 calc R . .
C563 C -0.01020(17) 0.48436(12) 0.69629(15) 0.0420(7) Uani 1 1 d . . .
H56D H 0.0299 0.4818 0.6690 0.063 Uiso 1 1 calc R . .
H56E H -0.0487 0.4589 0.6765 0.063 Uiso 1 1 calc R . .
H56F H 0.0027 0.4672 0.7396 0.063 Uiso 1 1 calc R . .
C621 C 0.05228(12) 0.88849(10) 0.55968(11) 0.0252(5) Uani 1 1 d . . .
H621 H 0.0308 0.8537 0.5856 0.030 Uiso 1 1 calc R . .
C622 C -0.00104(13) 0.90804(12) 0.50556(13) 0.0323(6) Uani 1 1 d . . .
H62A H 0.0188 0.9417 0.4787 0.048 Uiso 1 1 calc R . .
H62B H -0.0430 0.9245 0.5248 0.048 Uiso 1 1 calc R . .
H62C H -0.0131 0.8704 0.4785 0.048 Uiso 1 1 calc R . .
C623 C 0.06911(15) 0.94483(12) 0.60552(13) 0.0360(6) Uani 1 1 d . . .
H62D H 0.1042 0.9314 0.6390 0.054 Uiso 1 1 calc R . .
H62E H 0.0267 0.9583 0.6262 0.054 Uiso 1 1 calc R . .
H62F H 0.0872 0.9810 0.5808 0.054 Uiso 1 1 calc R . .
C661 C 0.17775(12) 0.69443(11) 0.47004(11) 0.0255(5) Uani 1 1 d . . .
H661 H 0.1320 0.6750 0.4803 0.031 Uiso 1 1 calc R . .
C662 C 0.1901(2) 0.68114(15) 0.39830(15) 0.0526(8) Uani 1 1 d . . .
H66A H 0.2383 0.6919 0.3895 0.079 Uiso 1 1 calc R . .
H66B H 0.1583 0.7076 0.3708 0.079 Uiso 1 1 calc R . .
H66C H 0.1816 0.6354 0.3888 0.079 Uiso 1 1 calc R . .
C663 C 0.23400(19) 0.66136(14) 0.51107(17) 0.0563(9) Uani 1 1 d . . .
H66D H 0.2793 0.6797 0.5016 0.084 Uiso 1 1 calc R . .
H66E H 0.2337 0.6151 0.5012 0.084 Uiso 1 1 calc R . .
H66F H 0.2256 0.6677 0.5571 0.084 Uiso 1 1 calc R . .
C161 C -0.54753(8) 0.61237(7) 0.86076(8) 0.0388(7) Uani 1 1 d . . .
H161 H -0.5458 0.6434 0.8237 0.047 Uiso 1 1 calc R . .
C162 C -0.52715(8) 0.54628(7) 0.83589(8) 0.0471(8) Uani 1 1 d R . .
H16A H -0.4797 0.5480 0.8209 0.071 Uiso 1 1 calc R . .
H16B H -0.5594 0.5336 0.7997 0.071 Uiso 1 1 calc R . .
H16C H -0.5292 0.5146 0.8711 0.071 Uiso 1 1 calc R . .
C163 C -0.62369(8) 0.61234(7) 0.88407(8) 0.0572(9) Uani 1 1 d R . .
H16D H -0.6563 0.6033 0.8471 0.086 Uiso 1 1 calc R . .
H16E H -0.6342 0.6546 0.9024 0.086 Uiso 1 1 calc R . .
H16F H -0.6282 0.5791 0.9174 0.086 Uiso 1 1 calc R . .
C3T C -0.30409(8) 0.94080(7) 0.63721(8) 0.0514(8) Uani 1 1 d RU A .
H3T H -0.3526 0.9332 0.6393 0.062 Uiso 1 1 calc R . .
C4T C -0.27170(16) 0.92949(13) 0.57987(15) 0.0433(7) Uani 1 1 d U . .
H4T H -0.2980 0.9151 0.5423 0.052 Uiso 1 1 calc R . .
C5T C -0.20112(17) 0.93921(13) 0.57756(15) 0.0436(7) Uani 1 1 d U . .
H5T H -0.1786 0.9311 0.5384 0.052 Uiso 1 1 calc R . .
C6T C -0.16328(18) 0.96055(15) 0.63151(17) 0.0519(8) Uani 1 1 d U . .
H6T H -0.1145 0.9671 0.6296 0.062 Uiso 1 1 calc R . .
C1T C -0.19553(19) 0.97275(16) 0.68906(17) 0.0538(8) Uani 1 1 d U A .
H1T H -0.1691 0.9876 0.7263 0.065 Uiso 1 1 calc R . .
C2T C -0.26604(19) 0.96309(16) 0.69161(16) 0.0537(8) Uani 1 1 d U . .
H2T H -0.2886 0.9717 0.7306 0.064 Uiso 0.757(9) 1 calc PR A 1
C7S C -0.2977(8) 0.9934(7) 0.7557(7) 0.057(4) Uani 0.243(9) 1 d PU A 2
H7S1 H -0.2597 1.0045 0.7872 0.085 Uiso 0.243(9) 1 calc PR A 2
H7S2 H -0.3285 0.9618 0.7750 0.085 Uiso 0.243(9) 1 calc PR A 2
H7S3 H -0.3244 1.0324 0.7439 0.085 Uiso 0.243(9) 1 calc PR A 2
C221 C -0.53704(9) 0.82012(9) 0.76954(8) 0.0399(10) Uani 0.851(7) 1 d PDU B 1
H221 H -0.4965 0.7916 0.7818 0.048 Uiso 0.851(7) 1 calc PR B 1
C222 C -0.59124(9) 0.80792(9) 0.81684(8) 0.0544(12) Uani 0.851(7) 1 d PRDU B 1
H22A H -0.6345 0.8297 0.8022 0.082 Uiso 0.851(7) 1 calc PR B 1
H22B H -0.5754 0.8246 0.8596 0.082 Uiso 0.851(7) 1 calc PR B 1
H22C H -0.5996 0.7614 0.8199 0.082 Uiso 0.851(7) 1 calc PR B 1
C223 C -0.51124(9) 0.88992(9) 0.77384(8) 0.0544(13) Uani 0.851(7) 1 d PRDU B 1
H22D H -0.5508 0.9193 0.7666 0.082 Uiso 0.851(7) 1 calc PR B 1
H22E H -0.4774 0.8974 0.7406 0.082 Uiso 0.851(7) 1 calc PR B 1
H22F H -0.4890 0.8977 0.8170 0.082 Uiso 0.851(7) 1 calc PR B 1
C224 C -0.55742(9) 0.80117(9) 0.77920(8) 0.054(6) Uani 0.149(7) 1 d PRDU B 2
H224 H -0.5191 0.7706 0.7924 0.064 Uiso 0.149(7) 1 calc PR B 2
C225 C -0.61452(9) 0.78627(9) 0.81870(8) 0.0544(12) Uani 0.149(7) 1 d PRDU B 2
H22G H -0.5969 0.7778 0.8634 0.082 Uiso 0.149(7) 1 calc PR B 2
H22H H -0.6389 0.7480 0.8013 0.082 Uiso 0.149(7) 1 calc PR B 2
H22I H -0.6468 0.8228 0.8184 0.082 Uiso 0.149(7) 1 calc PR B 2
C226 C -0.52872(9) 0.87107(9) 0.79390(8) 0.058(6) Uani 0.149(7) 1 d PRDU B 2
H22J H -0.5567 0.9026 0.7685 0.087 Uiso 0.149(7) 1 calc PR B 2
H22K H -0.4801 0.8737 0.7821 0.087 Uiso 0.149(7) 1 calc PR B 2
H22L H -0.5315 0.8804 0.8403 0.087 Uiso 0.149(7) 1 calc PR B 2
C361 C -0.38871(9) 0.53805(9) 0.61142(8) 0.0283(5) Uani 1 1 d RU . .
H361 H -0.4274 0.5645 0.6282 0.034 Uiso 0.612(13) 1 calc PR C 1
H36X H -0.4053 0.5819 0.6235 0.034 Uiso 0.388(13) 1 calc PR C 2
C362 C -0.4203(4) 0.4802(3) 0.5747(3) 0.0445(18) Uani 0.612(13) 1 d PU C 1
H36A H -0.4514 0.4954 0.5387 0.067 Uiso 0.612(13) 1 calc PR C 1
H36B H -0.4467 0.4539 0.6043 0.067 Uiso 0.612(13) 1 calc PR C 1
H36C H -0.3830 0.4541 0.5574 0.067 Uiso 0.612(13) 1 calc PR C 1
C363 C -0.3482(3) 0.5790(3) 0.5690(4) 0.0441(16) Uani 0.612(13) 1 d PU C 1
H36D H -0.3231 0.6118 0.5952 0.066 Uiso 0.612(13) 1 calc PR C 1
H36E H -0.3797 0.6001 0.5366 0.066 Uiso 0.612(13) 1 calc PR C 1
H36F H -0.3147 0.5523 0.5468 0.066 Uiso 0.612(13) 1 calc PR C 1
C364 C -0.4542(6) 0.4973(6) 0.5983(6) 0.055(4) Uani 0.388(13) 1 d PU C 2
H36G H -0.4830 0.5168 0.5629 0.082 Uiso 0.388(13) 1 calc PR C 2
H36H H -0.4807 0.4956 0.6376 0.082 Uiso 0.388(13) 1 calc PR C 2
H36I H -0.4409 0.4536 0.5859 0.082 Uiso 0.388(13) 1 calc PR C 2
C365 C -0.3537(5) 0.5463(9) 0.5441(5) 0.056(4) Uani 0.388(13) 1 d PU C 2
H36J H -0.3877 0.5642 0.5119 0.085 Uiso 0.388(13) 1 calc PR C 2
H36K H -0.3378 0.5042 0.5291 0.085 Uiso 0.388(13) 1 calc PR C 2
H36L H -0.3138 0.5756 0.5495 0.085 Uiso 0.388(13) 1 calc PR C 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O1 1.8804(15) . ?
Nb1 O2 1.8901(16) . ?
Nb1 O3 1.9088(15) . ?
Nb1 P3 2.5375(7) . ?
Nb1 P1 2.5678(7) . ?
Nb1 P2 2.5847(7) . ?
Nb2 O6 1.8899(14) . ?
Nb2 O4 1.9068(15) . ?
Nb2 O5 1.9124(15) . ?
Nb2 P5 2.5410(6) . ?
Nb2 P4 2.5442(7) . ?
Nb2 P6 2.5905(7) . ?
Sn1 P6 2.7009(7) . ?
Sn1 P2 2.7541(8) . ?
Sn1 P1 2.8014(6) . ?
Sn1 P4 2.9867(6) . ?
P1 P3 2.1919(9) . ?
P1 P2 2.2074(9) . ?
P2 P3 2.1901(11) . ?
P4 P5 2.1849(10) . ?
P4 P6 2.2070(9) . ?
P5 P6 2.2117(9) . ?
O1 C11 1.371(3) . ?
O2 C21 1.372(3) . ?
O3 C31 1.376(2) . ?
O4 C41 1.373(3) . ?
O5 C51 1.376(3) . ?
O6 C61 1.374(2) . ?
C11 C12 1.391(3) . ?
C11 C16 1.399(3) . ?
C12 C13 1.399(3) . ?
C12 C121 1.520(3) . ?
C13 C14 1.383(4) . ?
C14 C15 1.385(4) . ?
C15 C16 1.399(4) . ?
C16 C161 1.527(3) . ?
C21 C26 1.403(3) . ?
C21 C22 1.403(3) . ?
C22 C23 1.399(4) . ?
C22 C221 1.510(3) . ?
C22 C224 1.597(3) . ?
C23 C24 1.377(4) . ?
C24 C25 1.373(4) . ?
C25 C26 1.390(4) . ?
C26 C261 1.522(3) . ?
C31 C32 1.403(3) . ?
C31 C36 1.405(3) . ?
C32 C33 1.395(3) . ?
C32 C321 1.520(3) . ?
C33 C34 1.384(3) . ?
C34 C35 1.387(4) . ?
C35 C36 1.396(3) . ?
C36 C361 1.516(3) . ?
C41 C46 1.403(3) . ?
C41 C42 1.404(3) . ?
C42 C43 1.399(4) . ?
C42 C421 1.510(4) . ?
C43 C44 1.378(4) . ?
C44 C45 1.380(4) . ?
C45 C46 1.396(4) . ?
C46 C461 1.508(4) . ?
C51 C52 1.404(3) . ?
C51 C56 1.412(3) . ?
C52 C53 1.391(3) . ?
C52 C521 1.520(3) . ?
C53 C54 1.387(4) . ?
C54 C55 1.382(4) . ?
C55 C56 1.393(3) . ?
C56 C561 1.514(3) . ?
C61 C62 1.403(3) . ?
C61 C66 1.404(3) . ?
C62 C63 1.399(3) . ?
C62 C621 1.515(3) . ?
C63 C64 1.384(3) . ?
C64 C65 1.383(3) . ?
C65 C66 1.397(3) . ?
C66 C661 1.517(3) . ?
C121 C123 1.524(4) . ?
C121 C122 1.536(4) . ?
C261 C263 1.525(4) . ?
C261 C262 1.532(4) . ?
C321 C323 1.536(4) . ?
C321 C322 1.539(3) . ?
C421 C423 1.531(3) . ?
C421 C422 1.532(3) . ?
C461 C462 1.516(4) . ?
C461 C463 1.534(4) . ?
C521 C522 1.530(4) . ?
C521 C523 1.532(4) . ?
C561 C562 1.533(3) . ?
C561 C563 1.537(3) . ?
C621 C623 1.526(3) . ?
C621 C622 1.530(4) . ?
C661 C663 1.503(4) . ?
C661 C662 1.534(4) . ?
C161 C162 1.5216 . ?
C161 C163 1.5652 . ?
C3T C4T 1.384(3) . ?
C3T C2T 1.386(4) . ?
C4T C5T 1.376(4) . ?
C5T C6T 1.370(4) . ?
C6T C1T 1.390(4) . ?
C1T C2T 1.375(5) . ?
C2T C7S 1.611(13) . ?
C221 C222 1.4853 . ?
C221 C223 1.5311 . ?
C224 C225 1.4342 . ?
C224 C226 1.5747 . ?
C361 C363 1.471(6) . ?
C361 C362 1.527(5) . ?
C361 C364 1.529(9) . ?
C361 C365 1.583(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 O2 104.12(7) . . ?
O1 Nb1 O3 101.67(7) . . ?
O2 Nb1 O3 107.86(7) . . ?
O1 Nb1 P3 100.40(5) . . ?
O2 Nb1 P3 98.22(5) . . ?
O3 Nb1 P3 140.20(5) . . ?
O1 Nb1 P1 102.02(5) . . ?
O2 Nb1 P1 142.73(5) . . ?
O3 Nb1 P1 92.17(5) . . ?
P3 Nb1 P1 50.85(2) . . ?
O1 Nb1 P2 147.82(5) . . ?
O2 Nb1 P2 94.92(5) . . ?
O3 Nb1 P2 96.71(5) . . ?
P3 Nb1 P2 50.62(3) . . ?
P1 Nb1 P2 50.73(2) . . ?
O6 Nb2 O4 104.63(6) . . ?
O6 Nb2 O5 103.88(7) . . ?
O4 Nb2 O5 108.69(6) . . ?
O6 Nb2 P5 103.06(5) . . ?
O4 Nb2 P5 139.61(5) . . ?
O5 Nb2 P5 92.35(5) . . ?
O6 Nb2 P4 99.35(5) . . ?
O4 Nb2 P4 95.71(5) . . ?
O5 Nb2 P4 140.34(5) . . ?
P5 Nb2 P4 50.89(2) . . ?
O6 Nb2 P6 147.98(5) . . ?
O4 Nb2 P6 91.57(5) . . ?
O5 Nb2 P6 96.52(5) . . ?
P5 Nb2 P6 51.05(2) . . ?
P4 Nb2 P6 50.90(2) . . ?
P6 Sn1 P2 101.06(2) . . ?
P6 Sn1 P1 98.28(2) . . ?
P2 Sn1 P1 46.813(19) . . ?
P6 Sn1 P4 45.319(17) . . ?
P2 Sn1 P4 122.94(2) . . ?
P1 Sn1 P4 143.143(18) . . ?
P3 P1 P2 59.71(3) . . ?
P3 P1 Nb1 63.86(3) . . ?
P2 P1 Nb1 65.03(2) . . ?
P3 P1 Sn1 77.81(3) . . ?
P2 P1 Sn1 65.47(2) . . ?
Nb1 P1 Sn1 127.82(2) . . ?
P3 P2 P1 59.79(3) . . ?
P3 P2 Nb1 63.58(3) . . ?
P1 P2 Nb1 64.24(2) . . ?
P3 P2 Sn1 78.90(3) . . ?
P1 P2 Sn1 67.72(2) . . ?
Nb1 P2 Sn1 129.20(3) . . ?
P2 P3 P1 60.49(3) . . ?
P2 P3 Nb1 65.81(3) . . ?
P1 P3 Nb1 65.29(3) . . ?
P5 P4 P6 60.47(3) . . ?
P5 P4 Nb2 64.48(2) . . ?
P6 P4 Nb2 65.63(2) . . ?
P5 P4 Sn1 69.44(2) . . ?
P6 P4 Sn1 60.48(2) . . ?
Nb2 P4 Sn1 121.04(2) . . ?
P4 P5 P6 60.26(3) . . ?
P4 P5 Nb2 64.63(2) . . ?
P6 P5 Nb2 65.63(2) . . ?
P4 P6 P5 59.27(3) . . ?
P4 P6 Nb2 63.46(2) . . ?
P5 P6 Nb2 63.32(2) . . ?
P4 P6 Sn1 74.20(2) . . ?
P5 P6 Sn1 75.08(3) . . ?
Nb2 P6 Sn1 131.23(2) . . ?
C11 O1 Nb1 166.47(15) . . ?
C21 O2 Nb1 154.07(15) . . ?
C31 O3 Nb1 149.11(14) . . ?
C41 O4 Nb2 145.91(13) . . ?
C51 O5 Nb2 144.66(14) . . ?
C61 O6 Nb2 176.40(14) . . ?
O1 C11 C12 118.6(2) . . ?
O1 C11 C16 117.8(2) . . ?
C12 C11 C16 123.6(2) . . ?
C11 C12 C13 117.0(2) . . ?
C11 C12 C121 119.9(2) . . ?
C13 C12 C121 123.0(2) . . ?
C14 C13 C12 121.2(3) . . ?
C13 C14 C15 120.2(3) . . ?
C14 C15 C16 121.1(3) . . ?
C15 C16 C11 116.9(3) . . ?
C15 C16 C161 122.5(2) . . ?
C11 C16 C161 120.6(2) . . ?
O2 C21 C26 118.6(2) . . ?
O2 C21 C22 119.3(2) . . ?
C26 C21 C22 122.1(2) . . ?
C23 C22 C21 117.5(2) . . ?
C23 C22 C221 120.1(2) . . ?
C21 C22 C221 122.4(2) . . ?
C23 C22 C224 121.1(2) . . ?
C21 C22 C224 116.4(2) . . ?
C221 C22 C224 21.91(4) . . ?
C24 C23 C22 121.0(3) . . ?
C25 C24 C23 120.4(3) . . ?
C24 C25 C26 121.5(2) . . ?
C25 C26 C21 117.5(2) . . ?
C25 C26 C261 123.2(2) . . ?
C21 C26 C261 119.3(2) . . ?
O3 C31 C32 119.54(19) . . ?
O3 C31 C36 117.8(2) . . ?
C32 C31 C36 122.6(2) . . ?
C33 C32 C31 117.5(2) . . ?
C33 C32 C321 119.7(2) . . ?
C31 C32 C321 122.8(2) . . ?
C34 C33 C32 121.4(2) . . ?
C33 C34 C35 119.7(2) . . ?
C34 C35 C36 121.5(2) . . ?
C35 C36 C31 117.2(2) . . ?
C35 C36 C361 122.04(19) . . ?
C31 C36 C361 120.72(19) . . ?
O4 C41 C46 118.2(2) . . ?
O4 C41 C42 119.2(2) . . ?
C46 C41 C42 122.5(2) . . ?
C43 C42 C41 117.6(2) . . ?
C43 C42 C421 120.3(2) . . ?
C41 C42 C421 121.9(2) . . ?
C44 C43 C42 121.0(3) . . ?
C43 C44 C45 120.1(3) . . ?
C44 C45 C46 121.8(3) . . ?
C45 C46 C41 116.9(2) . . ?
C45 C46 C461 121.4(2) . . ?
C41 C46 C461 121.5(2) . . ?
O5 C51 C52 118.75(19) . . ?
O5 C51 C56 119.1(2) . . ?
C52 C51 C56 122.2(2) . . ?
C53 C52 C51 117.8(2) . . ?
C53 C52 C521 120.4(2) . . ?
C51 C52 C521 121.9(2) . . ?
C54 C53 C52 121.5(2) . . ?
C55 C54 C53 119.4(2) . . ?
C54 C55 C56 122.1(2) . . ?
C55 C56 C51 117.0(2) . . ?
C55 C56 C561 120.8(2) . . ?
C51 C56 C561 122.2(2) . . ?
O6 C61 C62 119.36(18) . . ?
O6 C61 C66 118.02(18) . . ?
C62 C61 C66 122.62(19) . . ?
C63 C62 C61 117.6(2) . . ?
C63 C62 C621 121.38(19) . . ?
C61 C62 C621 120.86(19) . . ?
C64 C63 C62 121.1(2) . . ?
C65 C64 C63 119.8(2) . . ?
C64 C65 C66 121.9(2) . . ?
C65 C66 C61 117.0(2) . . ?
C65 C66 C661 121.2(2) . . ?
C61 C66 C661 121.86(19) . . ?
C12 C121 C123 114.3(2) . . ?
C12 C121 C122 109.5(2) . . ?
C123 C121 C122 110.4(2) . . ?
C26 C261 C263 109.8(2) . . ?
C26 C261 C262 112.4(2) . . ?
C263 C261 C262 111.3(2) . . ?
C32 C321 C323 111.8(2) . . ?
C32 C321 C322 111.5(2) . . ?
C323 C321 C322 110.3(2) . . ?
C42 C421 C423 113.0(2) . . ?
C42 C421 C422 110.2(2) . . ?
C423 C421 C422 110.1(2) . . ?
C46 C461 C462 114.3(3) . . ?
C46 C461 C463 109.7(2) . . ?
C462 C461 C463 111.4(3) . . ?
C52 C521 C522 111.2(2) . . ?
C52 C521 C523 111.4(2) . . ?
C522 C521 C523 110.5(3) . . ?
C56 C561 C562 112.0(2) . . ?
C56 C561 C563 110.3(2) . . ?
C562 C561 C563 110.9(2) . . ?
C62 C621 C623 113.8(2) . . ?
C62 C621 C622 109.10(19) . . ?
C623 C621 C622 111.1(2) . . ?
C663 C661 C66 111.9(2) . . ?
C663 C661 C662 108.4(2) . . ?
C66 C661 C662 111.8(2) . . ?
C162 C161 C16 111.90(11) . . ?
C162 C161 C163 111.4 . . ?
C16 C161 C163 110.41(10) . . ?
C4T C3T C2T 120.3(2) . . ?
C5T C4T C3T 119.6(3) . . ?
C6T C5T C4T 120.2(3) . . ?
C5T C6T C1T 120.6(3) . . ?
C2T C1T C6T 119.4(3) . . ?
C1T C2T C3T 119.9(3) . . ?
C1T C2T C7S 113.0(6) . . ?
C3T C2T C7S 125.9(6) . . ?
C222 C221 C22 110.96(13) . . ?
C222 C221 C223 111.1 . . ?
C22 C221 C223 112.55(13) . . ?
C225 C224 C226 111.1 . . ?
C225 C224 C22 123.92(12) . . ?
C226 C224 C22 101.00(13) . . ?
C363 C361 C36 110.1(3) . . ?
C363 C361 C362 111.6(3) . . ?
C36 C361 C362 109.6(3) . . ?
C363 C361 C364 132.1(4) . . ?
C36 C361 C364 113.7(4) . . ?
C362 C361 C364 34.5(5) . . ?
C363 C361 C365 32.1(5) . . ?
C36 C361 C365 117.5(4) . . ?
C362 C361 C365 80.0(6) . . ?
C364 C361 C365 106.8(6) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        30.61
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_10035p
_database_code_depnum_ccdc_archive 'CCDC 1421302'
_audit_update_record             
;
2015-08-28 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C80 H120 Nb2 O8 P6 Sn'
_chemical_formula_weight         1700.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pca2(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   27.951(3)
_cell_length_b                   25.525(3)
_cell_length_c                   24.007(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     17127(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9609
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      27.77

_exptl_crystal_description       shard
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7088
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8417
_exptl_absorpt_correction_T_max  0.9320
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 'Siemens three-circle diffractometer, Bruker APEX CCD' 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            348710
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         0.80
_diffrn_reflns_theta_max         28.28
_reflns_number_total             42449
_reflns_number_gt                32792
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0226P)²+21.8197P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.048(11)
_refine_ls_number_reflns         42449
_refine_ls_number_parameters     1829
_refine_ls_number_restraints     107
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0842
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.537578(10) 1.319289(12) 0.436361(15) 0.02234(7) Uani 1 1 d . . .
Nb3 Nb 0.462548(13) 1.017164(15) 0.529438(17) 0.01627(8) Uani 1 1 d . . .
P12 P 0.36771(4) 1.18858(5) 0.37570(5) 0.0219(3) Uani 1 1 d . . .
Sn2 Sn 0.448485(10) 1.188328(12) 0.436069(15) 0.02013(7) Uani 1 1 d . . .
Nb2 Nb 0.532219(13) 1.494398(16) 0.518212(17) 0.01760(9) Uani 1 1 d . . .
P6 P 0.49451(4) 1.44190(5) 0.43970(6) 0.0279(3) Uani 1 1 d . . .
Nb4 Nb 0.329755(13) 1.252827(15) 0.305510(16) 0.01530(8) Uani 1 1 d . . .
P11 P 0.41182(4) 1.20930(5) 0.30350(6) 0.0236(3) Uani 1 1 d . . .
Nb1 Nb 0.659228(14) 1.243127(15) 0.317537(17) 0.01743(9) Uani 1 1 d . . .
P5 P 0.49748(4) 1.40143(5) 0.51944(6) 0.0254(3) Uani 1 1 d . . .
P9 P 0.49333(4) 1.07051(5) 0.44750(6) 0.0253(3) Uani 1 1 d . . .
P4 P 0.56375(4) 1.41363(5) 0.47086(6) 0.0261(3) Uani 1 1 d . . .
P8 P 0.49473(4) 1.11102(5) 0.52713(6) 0.0252(3) Uani 1 1 d . . .
P10 P 0.40076(4) 1.26793(5) 0.36800(5) 0.0211(3) Uani 1 1 d . . .
P7 P 0.42577(4) 1.09756(5) 0.48484(6) 0.0236(3) Uani 1 1 d . . .
P3 P 0.62272(5) 1.31150(5) 0.38402(6) 0.0281(3) Uani 1 1 d . . .
P2 P 0.59037(4) 1.23184(5) 0.38483(6) 0.0238(3) Uani 1 1 d . . .
P1 P 0.57676(5) 1.28453(5) 0.31543(6) 0.0285(3) Uani 1 1 d . . .
O5 O 0.57577(10) 1.48246(12) 0.57900(13) 0.0199(7) Uani 1 1 d . . .
O8 O 0.43052(10) 0.96440(12) 0.48821(13) 0.0193(7) Uani 1 1 d . . .
O12 O 0.28695(10) 1.28374(12) 0.35899(12) 0.0169(7) Uani 1 1 d . . .
O3 O 0.64812(10) 1.18599(12) 0.26921(13) 0.0196(7) Uani 1 1 d . . .
O11 O 0.33983(10) 1.30702(12) 0.25314(13) 0.0197(7) Uani 1 1 d . . .
O2 O 0.69055(11) 1.29414(12) 0.27218(13) 0.0210(7) Uani 1 1 d . . .
O10 O 0.29692(11) 1.19772(12) 0.26694(13) 0.0192(7) Uani 1 1 d . . .
O7 O 0.42331(10) 1.02804(12) 0.59458(13) 0.0181(7) Uani 1 1 d . . .
O4 O 0.47468(10) 1.52503(12) 0.54553(13) 0.0221(7) Uani 1 1 d . . .
O1 O 0.70362(11) 1.21566(12) 0.37150(13) 0.0201(7) Uani 1 1 d . . .
O9 O 0.52147(10) 0.98593(12) 0.55076(13) 0.0205(7) Uani 1 1 d . . .
O2S O 0.41175(13) 1.23473(13) 0.51077(14) 0.0303(8) Uani 1 1 d . . .
O1S O 0.57000(11) 1.28688(13) 0.51972(15) 0.0305(8) Uani 1 1 d . . .
O6 O 0.56193(11) 1.54719(12) 0.47411(13) 0.0208(7) Uani 1 1 d . . .
C12 C 0.73226(16) 1.20779(18) 0.5198(2) 0.0249(10) Uani 1 1 d . . .
H12 H 0.7472 1.2282 0.5480 0.030 Uiso 1 1 calc R . .
C10A C 0.29732(15) 1.14717(17) 0.24685(18) 0.0163(9) Uani 1 1 d . . .
C914 C 0.57261(18) 1.03738(19) 0.6358(2) 0.0252(11) Uani 1 1 d . . .
H914 H 0.5444 1.0573 0.6214 0.030 Uiso 1 1 calc R . .
C15 C 0.68811(15) 1.14687(17) 0.4378(2) 0.0222(9) Uani 1 1 d . . .
C85 C 0.38269(17) 0.94711(19) 0.4072(2) 0.0232(11) Uani 1 1 d . . .
C35 C 0.69024(17) 1.11158(18) 0.23662(19) 0.0211(10) Uani 1 1 d . . .
C30D C 0.27536(17) 1.35206(19) 0.5154(2) 0.0285(11) Uani 1 1 d . . .
H30D H 0.2717 1.3681 0.5508 0.034 Uiso 1 1 calc R . .
C20 C 0.69345(16) 1.34293(18) 0.2483(2) 0.0222(10) Uani 1 1 d . A .
C752 C 0.47849(18) 1.1500(2) 0.6764(2) 0.0321(12) Uani 1 1 d . . .
H75A H 0.4863 1.1549 0.6369 0.048 Uiso 1 1 calc R . .
H75B H 0.5081 1.1489 0.6983 0.048 Uiso 1 1 calc R . .
H75C H 0.4585 1.1791 0.6892 0.048 Uiso 1 1 calc R . .
C30A C 0.28415(15) 1.30554(18) 0.41150(19) 0.0195(10) Uani 1 1 d . . .
C60 C 0.59473(15) 1.57753(18) 0.4459(2) 0.0239(11) Uani 1 1 d . . .
C30C C 0.26197(17) 1.30026(18) 0.5077(2) 0.0246(11) Uani 1 1 d . . .
H30C H 0.2496 1.2808 0.5383 0.030 Uiso 1 1 calc R . .
C71 C 0.34318(16) 1.06104(18) 0.59184(19) 0.0216(10) Uani 1 1 d . . .
C50 C 0.61131(16) 1.44916(18) 0.5965(2) 0.0217(10) Uani 1 1 d . . .
C411 C 0.43214(16) 1.47199(19) 0.6355(2) 0.0226(10) Uani 1 1 d . . .
H411 H 0.4606 1.4537 0.6194 0.027 Uiso 1 1 calc R . .
C30B C 0.26648(16) 1.27628(18) 0.45568(18) 0.0193(10) Uani 1 1 d . . .
C34 C 0.68832(17) 1.05926(19) 0.2197(2) 0.0251(11) Uani 1 1 d . . .
H34 H 0.7171 1.0417 0.2099 0.030 Uiso 1 1 calc R . .
C30 C 0.64615(15) 1.13513(17) 0.25100(19) 0.0181(9) Uani 1 1 d . . .
C711 C 0.32783(16) 1.01889(18) 0.55049(19) 0.0207(10) Uani 1 1 d . . .
H711 H 0.3573 0.9996 0.5386 0.025 Uiso 1 1 calc R . .
C10D C 0.29565(18) 1.04623(19) 0.2062(2) 0.0295(12) Uani 1 1 d . . .
H10D H 0.2957 1.0113 0.1926 0.035 Uiso 1 1 calc R . .
C30E C 0.29399(18) 1.38018(19) 0.4714(2) 0.0289(12) Uani 1 1 d . . .
H30E H 0.3041 1.4153 0.4775 0.035 Uiso 1 1 calc R . .
C31F C 0.31766(18) 1.39136(18) 0.3703(2) 0.0257(11) Uani 1 1 d . . .
H31F H 0.3205 1.3682 0.3368 0.031 Uiso 1 1 calc R . .
C451 C 0.42528(19) 1.5761(2) 0.4561(2) 0.0362(14) Uani 1 1 d . . .
H451 H 0.4605 1.5701 0.4595 0.043 Uiso 1 1 calc R . .
C351 C 0.73638(16) 1.1426(2) 0.2397(2) 0.0275(11) Uani 1 1 d . . .
H351 H 0.7366 1.1614 0.2762 0.033 Uiso 1 1 calc R . .
C20B C 0.29996(18) 1.3806(2) 0.2142(2) 0.0277(11) Uani 1 1 d . . .
C30F C 0.29854(17) 1.35870(18) 0.41805(19) 0.0224(10) Uani 1 1 d . . .
C352 C 0.73865(17) 1.1843(2) 0.1938(2) 0.0305(12) Uani 1 1 d . . .
H35A H 0.7386 1.1672 0.1573 0.046 Uiso 1 1 calc R . .
H35B H 0.7680 1.2050 0.1980 0.046 Uiso 1 1 calc R . .
H35C H 0.7108 1.2075 0.1968 0.046 Uiso 1 1 calc R . .
C31A C 0.25232(16) 1.21878(17) 0.44880(19) 0.0230(11) Uani 1 1 d . . .
H31A H 0.2639 1.2068 0.4115 0.028 Uiso 1 1 calc R . .
C14 C 0.69247(17) 1.1296(2) 0.4925(2) 0.0268(11) Uani 1 1 d . . .
H14 H 0.6800 1.0962 0.5022 0.032 Uiso 1 1 calc R . .
C10E C 0.26976(17) 1.05844(19) 0.2529(2) 0.0249(11) Uani 1 1 d . . .
H10E H 0.2515 1.0318 0.2707 0.030 Uiso 1 1 calc R . .
C61 C 0.61013(16) 1.56259(19) 0.3925(2) 0.0245(11) Uani 1 1 d . . .
C40 C 0.42519(15) 1.51989(18) 0.5438(2) 0.0212(10) Uani 1 1 d . . .
C75 C 0.40232(16) 1.09936(18) 0.65621(19) 0.0211(10) Uani 1 1 d . . .
C151 C 0.66632(17) 1.11141(18) 0.3941(2) 0.0243(11) Uani 1 1 d . . .
H151 H 0.6623 1.1325 0.3594 0.029 Uiso 1 1 calc R . .
C25 C 0.72550(16) 1.37957(19) 0.2712(2) 0.0239(11) Uani 1 1 d . . .
C13 C 0.71434(17) 1.1594(2) 0.5334(2) 0.0296(11) Uani 1 1 d . . .
H13 H 0.7169 1.1466 0.5704 0.036 Uiso 1 1 calc R . .
C311 C 0.55652(16) 1.13738(18) 0.2652(2) 0.0218(10) Uani 1 1 d . . .
H311 H 0.5639 1.1593 0.2986 0.026 Uiso 1 1 calc R . .
C412 C 0.40590(19) 1.4325(2) 0.6721(2) 0.0323(13) Uani 1 1 d . . .
H41A H 0.3802 1.4504 0.6924 0.048 Uiso 1 1 calc R . .
H41B H 0.4284 1.4170 0.6986 0.048 Uiso 1 1 calc R . .
H41C H 0.3922 1.4049 0.6486 0.048 Uiso 1 1 calc R . .
C10F C 0.26958(16) 1.10912(18) 0.27524(19) 0.0205(10) Uani 1 1 d . . .
C211 C 0.63437(18) 1.3137(2) 0.1723(2) 0.0271(11) Uani 1 1 d . A .
H211 H 0.6336 1.2817 0.1964 0.033 Uiso 1 1 calc R . .
C23 C 0.70189(18) 1.4408(2) 0.1995(2) 0.0332(13) Uani 1 1 d . . .
H23 H 0.7045 1.4746 0.1832 0.040 Uiso 1 1 calc R A .
C3S C 0.62362(19) 1.2587(2) 0.5892(2) 0.0341(13) Uani 1 1 d . . .
H3S1 H 0.6572 1.2474 0.5943 0.041 Uiso 1 1 calc R . .
H3S2 H 0.6122 1.2756 0.6239 0.041 Uiso 1 1 calc R . .
C11 C 0.72937(16) 1.22809(18) 0.4659(2) 0.0225(10) Uani 1 1 d . . .
C11A C 0.34997(17) 1.1768(2) 0.1659(2) 0.0248(11) Uani 1 1 d . . .
H11A H 0.3505 1.2096 0.1886 0.030 Uiso 1 1 calc R . .
C70 C 0.38985(15) 1.06341(17) 0.61390(19) 0.0171(9) Uani 1 1 d . . .
C353 C 0.78134(17) 1.1084(2) 0.2375(2) 0.0365(14) Uani 1 1 d . . .
H35D H 0.7796 1.0816 0.2668 0.055 Uiso 1 1 calc R . .
H35E H 0.8097 1.1303 0.2434 0.055 Uiso 1 1 calc R . .
H35F H 0.7834 1.0913 0.2010 0.055 Uiso 1 1 calc R . .
C851 C 0.40797(19) 0.9882(2) 0.3735(2) 0.0292(12) Uani 1 1 d . . .
H851 H 0.4221 1.0137 0.4005 0.035 Uiso 1 1 calc R . .
C80 C 0.39502(16) 0.93592(19) 0.4615(2) 0.0212(10) Uani 1 1 d . . .
C551 C 0.66658(15) 1.48959(18) 0.5234(2) 0.0260(11) Uani 1 1 d . . .
H551 H 0.6349 1.5007 0.5081 0.031 Uiso 1 1 calc R . .
C11F C 0.23995(16) 1.12146(19) 0.3259(2) 0.0243(11) Uani 1 1 d . . .
H11F H 0.2435 1.1595 0.3347 0.029 Uiso 1 1 calc R . .
C111 C 0.75224(17) 1.27968(18) 0.4510(2) 0.0279(12) Uani 1 1 d . . .
H111 H 0.7353 1.2934 0.4173 0.033 Uiso 1 1 calc R . .
C90 C 0.57075(15) 0.98582(19) 0.54544(19) 0.0201(10) Uani 1 1 d . . .
C55 C 0.65654(16) 1.45130(19) 0.5703(2) 0.0236(11) Uani 1 1 d . . .
C713 C 0.30420(16) 1.0407(2) 0.4983(2) 0.0263(11) Uani 1 1 d . . .
H71A H 0.2743 1.0584 0.5084 0.039 Uiso 1 1 calc R . .
H71B H 0.2972 1.0119 0.4725 0.039 Uiso 1 1 calc R . .
H71C H 0.3258 1.0657 0.4803 0.039 Uiso 1 1 calc R . .
C10B C 0.32336(16) 1.13557(18) 0.19851(19) 0.0191(10) Uani 1 1 d . . .
C53 C 0.68561(18) 1.3862(2) 0.6355(2) 0.0302(12) Uani 1 1 d . . .
H53 H 0.7110 1.3651 0.6492 0.036 Uiso 1 1 calc R . .
C20A C 0.34278(17) 1.35696(18) 0.23182(19) 0.0213(10) Uani 1 1 d . . .
C93 C 0.66855(16) 0.9875(2) 0.5349(2) 0.0336(13) Uani 1 1 d . . .
H93 H 0.7023 0.9884 0.5308 0.040 Uiso 1 1 calc R . .
C21 C 0.66671(17) 1.35370(19) 0.2001(2) 0.0253(11) Uani 1 1 d . . .
C51 C 0.60269(17) 1.4152(2) 0.6413(2) 0.0251(11) Uani 1 1 d . . .
C45 C 0.40072(18) 1.5428(2) 0.5001(2) 0.0272(11) Uani 1 1 d . . .
C32A C 0.19793(17) 1.2120(2) 0.4501(2) 0.0324(13) Uani 1 1 d . . .
H32A H 0.1899 1.1749 0.4460 0.049 Uiso 1 1 calc R . .
H32B H 0.1836 1.2319 0.4195 0.049 Uiso 1 1 calc R . .
H32C H 0.1855 1.2250 0.4857 0.049 Uiso 1 1 calc R . .
C911 C 0.5626(2) 0.9256(2) 0.4609(2) 0.0358(13) Uani 1 1 d . . .
H911 H 0.5280 0.9327 0.4683 0.043 Uiso 1 1 calc R . .
C82 C 0.33648(19) 0.8681(2) 0.4671(2) 0.0356(14) Uani 1 1 d . . .
H82 H 0.3199 0.8420 0.4877 0.043 Uiso 1 1 calc R . .
C10 C 0.70655(15) 1.19679(17) 0.42526(19) 0.0209(10) Uani 1 1 d . . .
C152 C 0.69908(19) 1.0656(2) 0.3804(2) 0.0339(13) Uani 1 1 d . . .
H15A H 0.7297 1.0790 0.3666 0.051 Uiso 1 1 calc R . .
H15B H 0.6841 1.0437 0.3518 0.051 Uiso 1 1 calc R . .
H15C H 0.7045 1.0447 0.4141 0.051 Uiso 1 1 calc R . .
C153 C 0.61672(17) 1.0917(2) 0.4116(2) 0.0323(12) Uani 1 1 d . . .
H15D H 0.6195 1.0711 0.4458 0.048 Uiso 1 1 calc R . .
H15E H 0.6034 1.0698 0.3819 0.048 Uiso 1 1 calc R . .
H15F H 0.5956 1.1217 0.4181 0.048 Uiso 1 1 calc R . .
C91 C 0.59110(16) 0.9580(2) 0.5017(2) 0.0257(11) Uani 1 1 d . . .
C916 C 0.6036(2) 1.0758(2) 0.6681(2) 0.0390(14) Uani 1 1 d . . .
H91P H 0.6304 1.0571 0.6852 0.058 Uiso 1 1 calc R . .
H91Q H 0.5844 1.0926 0.6972 0.058 Uiso 1 1 calc R . .
H91R H 0.6159 1.1027 0.6427 0.058 Uiso 1 1 calc R . .
C24 C 0.72870(18) 1.4285(2) 0.2458(2) 0.0316(12) Uani 1 1 d . A .
H24 H 0.7499 1.4540 0.2608 0.038 Uiso 1 1 calc R . .
C20E C 0.3872(2) 1.4338(2) 0.2096(2) 0.0418(15) Uani 1 1 d . . .
H20E H 0.4166 1.4521 0.2063 0.050 Uiso 1 1 calc R . .
C511 C 0.55493(18) 1.4123(2) 0.6705(2) 0.0303(12) Uani 1 1 d . . .
H511 H 0.5337 1.4397 0.6539 0.036 Uiso 1 1 calc R . .
C31 C 0.60238(16) 1.10919(18) 0.2485(2) 0.0206(10) Uani 1 1 d . . .
C811 C 0.39113(19) 0.8842(2) 0.5520(2) 0.0305(12) Uani 1 1 d . . .
H811 H 0.3959 0.9185 0.5714 0.037 Uiso 1 1 calc R . .
C552 C 0.69461(18) 1.4658(2) 0.4756(2) 0.0354(13) Uani 1 1 d . . .
H55A H 0.7266 1.4559 0.4886 0.053 Uiso 1 1 calc R . .
H55B H 0.6975 1.4915 0.4455 0.053 Uiso 1 1 calc R . .
H55C H 0.6779 1.4347 0.4618 0.053 Uiso 1 1 calc R . .
C611 C 0.59021(18) 1.5146(2) 0.3644(2) 0.0295(12) Uani 1 1 d . . .
H611 H 0.5823 1.4886 0.3942 0.035 Uiso 1 1 calc R . .
C20F C 0.38715(19) 1.3826(2) 0.2305(2) 0.0294(12) Uani 1 1 d . . .
C33 C 0.64578(19) 1.03263(19) 0.2167(2) 0.0302(12) Uani 1 1 d . . .
H33 H 0.6456 0.9970 0.2051 0.036 Uiso 1 1 calc R . .
C12F C 0.18637(18) 1.1096(3) 0.3156(3) 0.0452(15) Uani 1 1 d . . .
H12A H 0.1746 1.1314 0.2848 0.068 Uiso 1 1 calc R . .
H12B H 0.1681 1.1174 0.3494 0.068 Uiso 1 1 calc R . .
H12C H 0.1825 1.0726 0.3060 0.068 Uiso 1 1 calc R . .
C33A C 0.27691(19) 1.18502(19) 0.4932(2) 0.0325(12) Uani 1 1 d . . .
H33A H 0.3117 1.1890 0.4901 0.049 Uiso 1 1 calc R . .
H33B H 0.2683 1.1482 0.4876 0.049 Uiso 1 1 calc R . .
H33C H 0.2665 1.1963 0.5303 0.049 Uiso 1 1 calc R . .
C22A C 0.2527(2) 1.3065(2) 0.1722(2) 0.0428(15) Uani 1 1 d . . .
H22A H 0.2510 1.3225 0.1351 0.064 Uiso 1 1 calc R . .
H22B H 0.2247 1.2841 0.1781 0.064 Uiso 1 1 calc R . .
H22C H 0.2819 1.2853 0.1750 0.064 Uiso 1 1 calc R . .
C12A C 0.3233(2) 1.1886(2) 0.1113(2) 0.0392(14) Uani 1 1 d . . .
H12D H 0.3235 1.1574 0.0875 0.059 Uiso 1 1 calc R . .
H12E H 0.3391 1.2175 0.0919 0.059 Uiso 1 1 calc R . .
H12F H 0.2901 1.1983 0.1197 0.059 Uiso 1 1 calc R . .
C41 C 0.40300(16) 1.49267(18) 0.5870(2) 0.0230(10) Uani 1 1 d . . .
C313 C 0.51596(17) 1.1000(2) 0.2813(2) 0.0340(13) Uani 1 1 d . . .
H31B H 0.5065 1.0793 0.2486 0.051 Uiso 1 1 calc R . .
H31C H 0.4885 1.1202 0.2945 0.051 Uiso 1 1 calc R . .
H31D H 0.5269 1.0764 0.3108 0.051 Uiso 1 1 calc R . .
C72 C 0.30955(17) 1.0971(2) 0.6120(2) 0.0250(11) Uani 1 1 d . . .
H72 H 0.2778 1.0965 0.5979 0.030 Uiso 1 1 calc R . .
C65 C 0.61190(18) 1.6224(2) 0.4737(2) 0.0296(12) Uani 1 1 d . . .
C83 C 0.32328(19) 0.8776(2) 0.4132(3) 0.0401(15) Uani 1 1 d . . .
H83 H 0.2988 0.8572 0.3963 0.048 Uiso 1 1 calc R . .
C22 C 0.67105(18) 1.40404(19) 0.1767(2) 0.0283(12) Uani 1 1 d . A .
H22 H 0.6526 1.4130 0.1449 0.034 Uiso 1 1 calc R . .
C42 C 0.35370(17) 1.4867(2) 0.5836(2) 0.0306(12) Uani 1 1 d . . .
H42 H 0.3374 1.4674 0.6115 0.037 Uiso 1 1 calc R . .
C21F C 0.43176(18) 1.3553(2) 0.2503(2) 0.0285(12) Uani 1 1 d . . .
H21F H 0.4227 1.3347 0.2841 0.034 Uiso 1 1 calc R . .
C54 C 0.69329(17) 1.4195(2) 0.5911(2) 0.0286(12) Uani 1 1 d . . .
H54 H 0.7240 1.4208 0.5744 0.034 Uiso 1 1 calc R . .
C74 C 0.36800(17) 1.13486(19) 0.6737(2) 0.0246(11) Uani 1 1 d . . .
H74 H 0.3761 1.1604 0.7008 0.030 Uiso 1 1 calc R . .
C10C C 0.32178(17) 1.08440(19) 0.1784(2) 0.0238(11) Uani 1 1 d . . .
H10C H 0.3388 1.0755 0.1455 0.029 Uiso 1 1 calc R . .
C73 C 0.32190(18) 1.1336(2) 0.6520(2) 0.0267(11) Uani 1 1 d . . .
H73 H 0.2987 1.1580 0.6648 0.032 Uiso 1 1 calc R . .
C21A C 0.25376(18) 1.3498(2) 0.2168(2) 0.0320(12) Uani 1 1 d . . .
H21A H 0.2526 1.3322 0.2540 0.038 Uiso 1 1 calc R . .
C751 C 0.45128(16) 1.0984(2) 0.6838(2) 0.0249(11) Uani 1 1 d . . .
H751 H 0.4705 1.0697 0.6666 0.030 Uiso 1 1 calc R . .
C52 C 0.64096(18) 1.3837(2) 0.6601(2) 0.0301(12) Uani 1 1 d . . .
H52 H 0.6359 1.3603 0.6902 0.036 Uiso 1 1 calc R . .
C712 C 0.29452(18) 0.9792(2) 0.5788(2) 0.0317(12) Uani 1 1 d . . .
H71D H 0.3113 0.9626 0.6099 0.048 Uiso 1 1 calc R . .
H71E H 0.2850 0.9524 0.5517 0.048 Uiso 1 1 calc R . .
H71F H 0.2660 0.9973 0.5927 0.048 Uiso 1 1 calc R . .
C62 C 0.64411(19) 1.5951(2) 0.3667(2) 0.0360(13) Uani 1 1 d . . .
H62 H 0.6548 1.5867 0.3303 0.043 Uiso 1 1 calc R . .
C1S C 0.5506(2) 1.2401(2) 0.5440(3) 0.0519(18) Uani 1 1 d . . .
H1S1 H 0.5369 1.2172 0.5148 0.062 Uiso 1 1 calc R . .
H1S2 H 0.5251 1.2489 0.5710 0.062 Uiso 1 1 calc R . .
C753 C 0.44595(19) 1.0871(2) 0.7463(2) 0.0307(12) Uani 1 1 d . . .
H75D H 0.4298 1.1166 0.7644 0.046 Uiso 1 1 calc R . .
H75E H 0.4777 1.0823 0.7629 0.046 Uiso 1 1 calc R . .
H75F H 0.4270 1.0551 0.7515 0.046 Uiso 1 1 calc R . .
C81 C 0.37369(17) 0.8955(2) 0.4929(2) 0.0261(11) Uani 1 1 d . . .
C6S C 0.3946(2) 1.3063(2) 0.5692(2) 0.0351(13) Uani 1 1 d . . .
H6S1 H 0.4263 1.3154 0.5848 0.042 Uiso 1 1 calc R . .
H6S2 H 0.3726 1.3363 0.5742 0.042 Uiso 1 1 calc R . .
C312 C 0.54021(18) 1.1743(2) 0.2188(2) 0.0344(13) Uani 1 1 d . . .
H31E H 0.5666 1.1978 0.2088 0.052 Uiso 1 1 calc R . .
H31G H 0.5129 1.1951 0.2319 0.052 Uiso 1 1 calc R . .
H31H H 0.5307 1.1538 0.1862 0.052 Uiso 1 1 calc R . .
C812 C 0.4398(2) 0.8563(2) 0.5493(2) 0.0452(15) Uani 1 1 d . . .
H81A H 0.4358 0.8218 0.5319 0.068 Uiso 1 1 calc R . .
H81B H 0.4524 0.8519 0.5871 0.068 Uiso 1 1 calc R . .
H81C H 0.4622 0.8773 0.5272 0.068 Uiso 1 1 calc R . .
C94 C 0.64705(17) 1.0138(2) 0.5784(2) 0.0303(12) Uani 1 1 d . . .
H94 H 0.6664 1.0329 0.6039 0.036 Uiso 1 1 calc R . .
C8S C 0.4005(2) 1.2136(2) 0.5661(2) 0.0322(13) Uani 1 1 d . . .
H8S1 H 0.4302 1.2039 0.5861 0.039 Uiso 1 1 calc R . .
H8S2 H 0.3799 1.1822 0.5629 0.039 Uiso 1 1 calc R . .
C912 C 0.5723(2) 0.9411(3) 0.4003(3) 0.0552(19) Uani 1 1 d . . .
H91A H 0.5637 0.9780 0.3948 0.083 Uiso 1 1 calc R . .
H91B H 0.5531 0.9191 0.3755 0.083 Uiso 1 1 calc R . .
H91C H 0.6063 0.9362 0.3920 0.083 Uiso 1 1 calc R . .
C64 C 0.64578(19) 1.6521(2) 0.4454(3) 0.0391(14) Uani 1 1 d . . .
H64 H 0.6582 1.6827 0.4627 0.047 Uiso 1 1 calc R . .
C95 C 0.59761(16) 1.01305(19) 0.5858(2) 0.0237(11) Uani 1 1 d . . .
C513 C 0.53091(19) 1.3588(2) 0.6618(3) 0.0390(14) Uani 1 1 d . . .
H51A H 0.5287 1.3515 0.6218 0.058 Uiso 1 1 calc R . .
H51B H 0.4987 1.3594 0.6780 0.058 Uiso 1 1 calc R . .
H51C H 0.5500 1.3315 0.6799 0.058 Uiso 1 1 calc R . .
C7S C 0.3747(2) 1.2570(2) 0.5961(2) 0.0348(13) Uani 1 1 d . . .
H7S1 H 0.3817 1.2562 0.6365 0.042 Uiso 1 1 calc R . .
H7S2 H 0.3397 1.2543 0.5905 0.042 Uiso 1 1 calc R . .
C413 C 0.45107(17) 1.51689(19) 0.6726(2) 0.0273(11) Uani 1 1 d . . .
H41D H 0.4241 1.5347 0.6905 0.041 Uiso 1 1 calc R . .
H41E H 0.4688 1.5420 0.6496 0.041 Uiso 1 1 calc R . .
H41F H 0.4723 1.5025 0.7012 0.041 Uiso 1 1 calc R . .
C5S C 0.39843(18) 1.29058(19) 0.5081(2) 0.0271(11) Uani 1 1 d . . .
H5S1 H 0.3675 1.2954 0.4887 0.032 Uiso 1 1 calc R . .
H5S2 H 0.4233 1.3113 0.4888 0.032 Uiso 1 1 calc R . .
C651 C 0.59303(19) 1.6359(2) 0.5306(2) 0.0371(13) Uani 1 1 d . . .
H651 H 0.5904 1.6025 0.5522 0.045 Uiso 1 1 calc R . .
C13F C 0.2556(2) 1.0897(2) 0.3761(2) 0.0405(14) Uani 1 1 d . . .
H13A H 0.2524 1.0523 0.3678 0.061 Uiso 1 1 calc R . .
H13B H 0.2354 1.0986 0.4081 0.061 Uiso 1 1 calc R . .
H13C H 0.2891 1.0977 0.3848 0.061 Uiso 1 1 calc R . .
C33F C 0.2832(2) 1.4363(2) 0.3560(3) 0.0469(16) Uani 1 1 d . . .
H33D H 0.2520 1.4217 0.3455 0.070 Uiso 1 1 calc R . .
H33E H 0.2962 1.4565 0.3248 0.070 Uiso 1 1 calc R . .
H33F H 0.2794 1.4591 0.3885 0.070 Uiso 1 1 calc R . .
C453 C 0.4106(2) 1.5613(3) 0.3965(3) 0.0544(19) Uani 1 1 d . . .
H45A H 0.4199 1.5250 0.3890 0.082 Uiso 1 1 calc R . .
H45B H 0.4267 1.5846 0.3700 0.082 Uiso 1 1 calc R . .
H45C H 0.3759 1.5649 0.3925 0.082 Uiso 1 1 calc R . .
C13A C 0.40204(19) 1.1612(2) 0.1535(2) 0.0408(15) Uani 1 1 d . . .
H13D H 0.4182 1.1519 0.1883 0.061 Uiso 1 1 calc R . .
H13E H 0.4187 1.1908 0.1360 0.061 Uiso 1 1 calc R . .
H13F H 0.4024 1.1311 0.1282 0.061 Uiso 1 1 calc R . .
C32 C 0.60297(17) 1.0570(2) 0.2304(2) 0.0266(11) Uani 1 1 d . . .
H32 H 0.5738 1.0381 0.2274 0.032 Uiso 1 1 calc R . .
C20C C 0.3023(2) 1.4319(2) 0.1951(2) 0.0427(15) Uani 1 1 d . . .
H20C H 0.2739 1.4490 0.1831 0.051 Uiso 1 1 calc R . .
C22F C 0.45003(19) 1.3163(2) 0.2077(2) 0.0378(14) Uani 1 1 d . . .
H22D H 0.4244 1.2918 0.1979 0.057 Uiso 1 1 calc R . .
H22E H 0.4771 1.2969 0.2234 0.057 Uiso 1 1 calc R . .
H22F H 0.4605 1.3351 0.1742 0.057 Uiso 1 1 calc R . .
C813 C 0.3558(2) 0.8516(2) 0.5865(2) 0.0451(16) Uani 1 1 d . . .
H81D H 0.3244 0.8686 0.5862 0.068 Uiso 1 1 calc R . .
H81E H 0.3674 0.8490 0.6249 0.068 Uiso 1 1 calc R . .
H81F H 0.3531 0.8165 0.5704 0.068 Uiso 1 1 calc R . .
C23F C 0.47169(19) 1.3928(2) 0.2680(3) 0.0414(15) Uani 1 1 d . . .
H23A H 0.4847 1.4104 0.2350 0.062 Uiso 1 1 calc R . .
H23B H 0.4972 1.3730 0.2864 0.062 Uiso 1 1 calc R . .
H23C H 0.4588 1.4189 0.2938 0.062 Uiso 1 1 calc R . .
C63 C 0.6622(2) 1.6385(2) 0.3924(2) 0.0409(15) Uani 1 1 d . . .
H63 H 0.6857 1.6593 0.3744 0.049 Uiso 1 1 calc R . .
C652 C 0.5432(2) 1.6593(2) 0.5263(3) 0.0506(16) Uani 1 1 d . . .
H65A H 0.5448 1.6930 0.5068 0.076 Uiso 1 1 calc R . .
H65B H 0.5301 1.6646 0.5637 0.076 Uiso 1 1 calc R . .
H65C H 0.5224 1.6353 0.5055 0.076 Uiso 1 1 calc R . .
C32F C 0.3677(2) 1.4132(2) 0.3838(3) 0.0426(15) Uani 1 1 d . . .
H32D H 0.3656 1.4368 0.4159 0.064 Uiso 1 1 calc R . .
H32E H 0.3799 1.4326 0.3515 0.064 Uiso 1 1 calc R . .
H32F H 0.3894 1.3842 0.3924 0.064 Uiso 1 1 calc R . .
C612 C 0.54345(19) 1.5282(2) 0.3342(2) 0.0384(14) Uani 1 1 d . . .
H61A H 0.5208 1.5434 0.3608 0.058 Uiso 1 1 calc R . .
H61B H 0.5297 1.4964 0.3179 0.058 Uiso 1 1 calc R . .
H61C H 0.5500 1.5536 0.3045 0.058 Uiso 1 1 calc R . .
C512 C 0.5589(2) 1.4235(2) 0.7331(2) 0.0428(15) Uani 1 1 d . . .
H51D H 0.5780 1.3960 0.7509 0.064 Uiso 1 1 calc R . .
H51E H 0.5268 1.4241 0.7497 0.064 Uiso 1 1 calc R . .
H51F H 0.5744 1.4576 0.7388 0.064 Uiso 1 1 calc R . .
C653 C 0.6262(2) 1.6727(3) 0.5633(3) 0.0511(17) Uani 1 1 d . . .
H65D H 0.6591 1.6597 0.5611 0.077 Uiso 1 1 calc R . .
H65E H 0.6160 1.6738 0.6024 0.077 Uiso 1 1 calc R . .
H65F H 0.6245 1.7080 0.5474 0.077 Uiso 1 1 calc R . .
C553 C 0.69132(19) 1.5394(2) 0.5458(3) 0.0407(15) Uani 1 1 d . . .
H55D H 0.6700 1.5571 0.5723 0.061 Uiso 1 1 calc R . .
H55E H 0.6985 1.5630 0.5148 0.061 Uiso 1 1 calc R . .
H55F H 0.7211 1.5296 0.5647 0.061 Uiso 1 1 calc R . .
C43 C 0.32815(17) 1.5083(2) 0.5404(2) 0.0364(14) Uani 1 1 d . . .
H43 H 0.2944 1.5039 0.5391 0.044 Uiso 1 1 calc R . .
C113 C 0.8036(2) 1.2717(2) 0.4354(4) 0.077(3) Uani 1 1 d . . .
H11B H 0.8209 1.2567 0.4671 0.115 Uiso 1 1 calc R . .
H11C H 0.8179 1.3054 0.4253 0.115 Uiso 1 1 calc R . .
H11D H 0.8055 1.2477 0.4036 0.115 Uiso 1 1 calc R . .
C4S C 0.61842(18) 1.2950(2) 0.5393(2) 0.0375(14) Uani 1 1 d . . .
H4S1 H 0.6234 1.3320 0.5504 0.045 Uiso 1 1 calc R . .
H4S2 H 0.6419 1.2859 0.5099 0.045 Uiso 1 1 calc R . .
C913 C 0.5708(2) 0.8674(2) 0.4713(3) 0.060(2) Uani 1 1 d . . .
H91D H 0.6047 0.8591 0.4658 0.090 Uiso 1 1 calc R . .
H91E H 0.5515 0.8469 0.4452 0.090 Uiso 1 1 calc R . .
H91F H 0.5615 0.8588 0.5095 0.090 Uiso 1 1 calc R . .
C84 C 0.34560(19) 0.9171(2) 0.3832(2) 0.0349(13) Uani 1 1 d . . .
H84 H 0.3358 0.9240 0.3460 0.042 Uiso 1 1 calc R . .
C212 C 0.58261(19) 1.3335(2) 0.1657(2) 0.0402(14) Uani 1 1 d . . .
H21B H 0.5821 1.3632 0.1398 0.060 Uiso 1 1 calc R A .
H21C H 0.5703 1.3447 0.2020 0.060 Uiso 1 1 calc R . .
H21D H 0.5625 1.3052 0.1510 0.060 Uiso 1 1 calc R . .
C915 C 0.55372(18) 0.9952(2) 0.6749(2) 0.0304(12) Uani 1 1 d . . .
H91G H 0.5331 0.9711 0.6540 0.046 Uiso 1 1 calc R . .
H91H H 0.5353 1.0116 0.7049 0.046 Uiso 1 1 calc R . .
H91I H 0.5807 0.9757 0.6908 0.046 Uiso 1 1 calc R . .
C613 C 0.6248(2) 1.4879(2) 0.3239(3) 0.0478(16) Uani 1 1 d . . .
H61D H 0.6320 1.5118 0.2931 0.072 Uiso 1 1 calc R . .
H61E H 0.6102 1.4559 0.3093 0.072 Uiso 1 1 calc R . .
H61F H 0.6545 1.4791 0.3436 0.072 Uiso 1 1 calc R . .
C20D C 0.3452(2) 1.4582(2) 0.1935(3) 0.0471(17) Uani 1 1 d . . .
H20D H 0.3461 1.4936 0.1813 0.057 Uiso 1 1 calc R . .
C251 C 0.7551(6) 1.3648(16) 0.3218(19) 0.028(3) Uani 0.52(2) 1 d PDU A 1
H251 H 0.7348 1.3429 0.3469 0.034 Uiso 0.52(2) 1 calc PR A 1
C252 C 0.7966(5) 1.3311(6) 0.3011(6) 0.040(3) Uani 0.52(2) 1 d PDU A 1
H25A H 0.7841 1.3022 0.2786 0.060 Uiso 0.52(2) 1 calc PR A 1
H25B H 0.8143 1.3171 0.3330 0.060 Uiso 0.52(2) 1 calc PR A 1
H25C H 0.8181 1.3526 0.2783 0.060 Uiso 0.52(2) 1 calc PR A 1
C253 C 0.7740(6) 1.4108(6) 0.3551(7) 0.038(3) Uani 0.52(2) 1 d PDU A 1
H25D H 0.7925 1.3978 0.3869 0.057 Uiso 0.52(2) 1 calc PR A 1
H25E H 0.7472 1.4319 0.3685 0.057 Uiso 0.52(2) 1 calc PR A 1
H25F H 0.7947 1.4323 0.3314 0.057 Uiso 0.52(2) 1 calc PR A 1
C254 C 0.7594(6) 1.3648(18) 0.318(2) 0.027(3) Uani 0.48(2) 1 d PDU A 2
H254 H 0.7490 1.3301 0.3331 0.032 Uiso 0.48(2) 1 calc PR A 2
C255 C 0.8111(5) 1.3591(8) 0.2974(6) 0.042(3) Uani 0.48(2) 1 d PDU A 2
H25G H 0.8317 1.3488 0.3285 0.063 Uiso 0.48(2) 1 calc PR A 2
H25H H 0.8221 1.3927 0.2822 0.063 Uiso 0.48(2) 1 calc PR A 2
H25I H 0.8124 1.3323 0.2683 0.063 Uiso 0.48(2) 1 calc PR A 2
C256 C 0.7557(6) 1.4044(6) 0.3650(7) 0.034(3) Uani 0.48(2) 1 d PDU A 2
H25J H 0.7783 1.3951 0.3946 0.051 Uiso 0.48(2) 1 calc PR A 2
H25K H 0.7231 1.4044 0.3799 0.051 Uiso 0.48(2) 1 calc PR A 2
H25L H 0.7634 1.4394 0.3507 0.051 Uiso 0.48(2) 1 calc PR A 2
C112 C 0.7487(2) 1.3213(2) 0.4959(3) 0.059(2) Uani 1 1 d . . .
H11E H 0.7150 1.3280 0.5045 0.089 Uiso 1 1 calc R . .
H11G H 0.7637 1.3537 0.4826 0.089 Uiso 1 1 calc R . .
H11H H 0.7652 1.3092 0.5295 0.089 Uiso 1 1 calc R . .
C92 C 0.64110(17) 0.9597(2) 0.4972(2) 0.0312(12) Uani 1 1 d . . .
H92 H 0.6564 0.9414 0.4677 0.037 Uiso 1 1 calc R . .
C452 C 0.4161(3) 1.6337(2) 0.4678(3) 0.067(2) Uani 1 1 d . . .
H45D H 0.3819 1.6411 0.4638 0.101 Uiso 1 1 calc R . .
H45E H 0.4343 1.6551 0.4413 0.101 Uiso 1 1 calc R . .
H45F H 0.4263 1.6420 0.5058 0.101 Uiso 1 1 calc R . .
C23A C 0.2090(2) 1.3842(3) 0.2119(3) 0.0507(18) Uani 1 1 d . . .
H23D H 0.2105 1.4123 0.2396 0.076 Uiso 1 1 calc R . .
H23E H 0.1804 1.3628 0.2186 0.076 Uiso 1 1 calc R . .
H23F H 0.2074 1.3993 0.1745 0.076 Uiso 1 1 calc R . .
C44 C 0.35079(18) 1.5365(2) 0.4987(2) 0.0357(13) Uani 1 1 d . . .
H44 H 0.3326 1.5515 0.4693 0.043 Uiso 1 1 calc R . .
C213 C 0.6549(2) 1.2980(2) 0.1162(2) 0.0460(16) Uani 1 1 d . . .
H21E H 0.6579 1.3291 0.0926 0.069 Uiso 1 1 calc R A .
H21G H 0.6335 1.2727 0.0983 0.069 Uiso 1 1 calc R . .
H21H H 0.6865 1.2821 0.1215 0.069 Uiso 1 1 calc R . .
C2S C 0.5918(2) 1.2129(2) 0.5730(3) 0.0478(16) Uani 1 1 d . . .
H2S1 H 0.6086 1.1886 0.5475 0.057 Uiso 1 1 calc R . .
H2S2 H 0.5808 1.1934 0.6062 0.057 Uiso 1 1 calc R . .
C852 C 0.4484(2) 0.9652(3) 0.3418(3) 0.070(2) Uani 1 1 d . . .
H85A H 0.4716 0.9502 0.3678 0.105 Uiso 1 1 calc R . .
H85B H 0.4639 0.9926 0.3196 0.105 Uiso 1 1 calc R . .
H85C H 0.4364 0.9377 0.3170 0.105 Uiso 1 1 calc R . .
O4S O 0.40960(19) 1.2606(2) 0.7564(2) 0.0741(16) Uani 1 1 d . . .
C15S C 0.3819(2) 1.2452(3) 0.8029(3) 0.0555(17) Uani 1 1 d . . .
H15G H 0.3878 1.2686 0.8350 0.067 Uiso 1 1 calc R . .
H15H H 0.3895 1.2087 0.8139 0.067 Uiso 1 1 calc R . .
C13S C 0.4671(3) 1.3164(3) 0.8059(4) 0.085(3) Uani 1 1 d . . .
H13G H 0.4539 1.3463 0.7854 0.128 Uiso 1 1 calc R . .
H13H H 0.5015 1.3214 0.8114 0.128 Uiso 1 1 calc R . .
H13I H 0.4512 1.3136 0.8422 0.128 Uiso 1 1 calc R . .
C16S C 0.3300(3) 1.2495(3) 0.7833(3) 0.075(2) Uani 1 1 d . . .
H16A H 0.3219 1.2864 0.7772 0.112 Uiso 1 1 calc R . .
H16B H 0.3087 1.2347 0.8117 0.112 Uiso 1 1 calc R . .
H16C H 0.3260 1.2300 0.7484 0.112 Uiso 1 1 calc R . .
C853 C 0.3767(3) 1.0194(3) 0.3344(3) 0.091(3) Uani 1 1 d . . .
H85D H 0.3934 1.0515 0.3233 0.136 Uiso 1 1 calc R . .
H85E H 0.3467 1.0285 0.3532 0.136 Uiso 1 1 calc R . .
H85F H 0.3696 0.9983 0.3012 0.136 Uiso 1 1 calc R . .
C14S C 0.4589(3) 1.2680(4) 0.7738(5) 0.102(3) Uani 1 1 d . . .
H14A H 0.4795 1.2686 0.7402 0.123 Uiso 1 1 calc R . .
H14B H 0.4687 1.2376 0.7967 0.123 Uiso 1 1 calc R . .
C9T C 0.6069(3) 1.2262(3) 0.7435(3) 0.076(2) Uani 1 1 d U . .
H9T1 H 0.5773 1.2368 0.7247 0.115 Uiso 1 1 calc R . .
H9T2 H 0.6257 1.2037 0.7187 0.115 Uiso 1 1 calc R . .
H9T3 H 0.6256 1.2575 0.7530 0.115 Uiso 1 1 calc R . .
C10T C 0.5952(4) 1.1974(4) 0.7945(4) 0.123(4) Uani 1 1 d U . .
H10A H 0.5769 1.1657 0.7840 0.148 Uiso 1 1 calc R . .
H10B H 0.6254 1.1856 0.8118 0.148 Uiso 1 1 calc R . .
O3T O 0.57023(19) 1.2233(2) 0.8327(2) 0.0761(15) Uani 1 1 d U . .
C11T C 0.5552(3) 1.1970(4) 0.8821(3) 0.088(3) Uani 1 1 d U . .
H11I H 0.5835 1.1816 0.9008 0.106 Uiso 1 1 calc R . .
H11J H 0.5334 1.1680 0.8719 0.106 Uiso 1 1 calc R . .
C12T C 0.5313(4) 1.2314(3) 0.9200(4) 0.119(4) Uani 1 1 d U . .
H12G H 0.5550 1.2507 0.9418 0.178 Uiso 1 1 calc R . .
H12H H 0.5109 1.2109 0.9450 0.178 Uiso 1 1 calc R . .
H12I H 0.5115 1.2562 0.8990 0.178 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 O1S 2.347(4) . ?
Sn1 P4 2.6493(14) . ?
Sn1 P3 2.6985(14) . ?
Sn1 P2 2.9479(13) . ?
Nb3 O8 1.896(3) . ?
Nb3 O9 1.900(3) . ?
Nb3 O7 1.930(3) . ?
Nb3 P7 2.5326(13) . ?
Nb3 P9 2.5423(13) . ?
Nb3 P8 2.5596(13) . ?
P12 P11 2.1918(18) . ?
P12 P10 2.2338(17) . ?
P12 Nb4 2.5796(13) . ?
P12 Sn2 2.6827(13) . ?
Sn2 O2S 2.382(3) . ?
Sn2 P7 2.6723(13) . ?
Sn2 P10 2.9288(13) . ?
Nb2 O6 1.904(3) . ?
Nb2 O4 1.905(3) . ?
Nb2 O5 1.925(3) . ?
Nb2 P4 2.5139(14) . ?
Nb2 P6 2.5415(14) . ?
Nb2 P5 2.5640(13) . ?
P6 P5 2.177(2) . ?
P6 P4 2.1967(18) . ?
Nb4 O11 1.890(3) . ?
Nb4 O10 1.918(3) . ?
Nb4 O12 1.924(3) . ?
Nb4 P10 2.5176(13) . ?
Nb4 P11 2.5491(13) . ?
P11 P10 2.1755(18) . ?
Nb1 O3 1.889(3) . ?
Nb1 O2 1.910(3) . ?
Nb1 O1 1.926(3) . ?
Nb1 P2 2.5292(13) . ?
Nb1 P1 2.5361(13) . ?
Nb1 P3 2.5757(14) . ?
P5 P4 2.2108(18) . ?
P9 P8 2.1736(19) . ?
P9 P7 2.2013(17) . ?
P8 P7 2.2053(18) . ?
P3 P1 2.199(2) . ?
P3 P2 2.2254(18) . ?
P2 P1 2.1746(19) . ?
O5 C50 1.373(5) . ?
O8 C80 1.387(5) . ?
O12 C30A 1.380(5) . ?
O3 C30 1.371(5) . ?
O11 C20A 1.376(5) . ?
O2 C20 1.373(5) . ?
O10 C10A 1.377(5) . ?
O7 C70 1.380(5) . ?
O4 C40 1.390(5) . ?
O1 C10 1.380(5) . ?
O9 C90 1.384(5) . ?
O2S C8S 1.467(6) . ?
O2S C5S 1.475(6) . ?
O1S C1S 1.434(6) . ?
O1S C4S 1.447(6) . ?
O6 C60 1.378(5) . ?
C12 C13 1.372(7) . ?
C12 C11 1.395(7) . ?
C10A C10B 1.402(6) . ?
C10A C10F 1.417(6) . ?
C914 C95 1.520(7) . ?
C914 C916 1.522(7) . ?
C914 C915 1.523(7) . ?
C15 C14 1.390(7) . ?
C15 C10 1.407(6) . ?
C15 C151 1.513(7) . ?
C85 C80 1.379(6) . ?
C85 C84 1.413(7) . ?
C85 C851 1.502(7) . ?
C35 C34 1.397(6) . ?
C35 C30 1.414(6) . ?
C35 C351 1.516(7) . ?
C30D C30E 1.379(7) . ?
C30D C30C 1.386(7) . ?
C20 C21 1.403(7) . ?
C20 C25 1.407(7) . ?
C752 C751 1.530(7) . ?
C30A C30B 1.388(6) . ?
C30A C30F 1.424(6) . ?
C60 C61 1.406(7) . ?
C60 C65 1.409(7) . ?
C30C C30B 1.397(6) . ?
C71 C72 1.402(7) . ?
C71 C70 1.409(6) . ?
C71 C711 1.526(6) . ?
C50 C51 1.402(7) . ?
C50 C55 1.414(6) . ?
C411 C41 1.514(7) . ?
C411 C412 1.524(7) . ?
C411 C413 1.545(6) . ?
C30B C31A 1.529(6) . ?
C34 C33 1.372(7) . ?
C30 C31 1.392(6) . ?
C711 C713 1.522(6) . ?
C711 C712 1.534(6) . ?
C10D C10E 1.372(7) . ?
C10D C10C 1.388(7) . ?
C30E C30F 1.398(7) . ?
C31F C30F 1.515(6) . ?
C31F C33F 1.536(7) . ?
C31F C32F 1.539(7) . ?
C451 C452 1.517(8) . ?
C451 C45 1.519(7) . ?
C451 C453 1.537(8) . ?
C351 C353 1.532(6) . ?
C351 C352 1.533(7) . ?
C20B C20C 1.387(7) . ?
C20B C20A 1.406(6) . ?
C20B C21A 1.514(7) . ?
C31A C32A 1.530(6) . ?
C31A C33A 1.533(6) . ?
C14 C13 1.384(7) . ?
C10E C10F 1.400(6) . ?
C61 C62 1.405(7) . ?
C61 C611 1.507(7) . ?
C40 C45 1.383(7) . ?
C40 C41 1.394(7) . ?
C75 C74 1.384(6) . ?
C75 C70 1.412(6) . ?
C75 C751 1.520(6) . ?
C151 C152 1.520(7) . ?
C151 C153 1.533(6) . ?
C25 C24 1.393(7) . ?
C25 C251 1.52(5) . ?
C25 C254 1.52(5) . ?
C311 C31 1.524(6) . ?
C311 C312 1.529(7) . ?
C311 C313 1.532(6) . ?
C10F C11F 1.504(6) . ?
C211 C213 1.517(7) . ?
C211 C21 1.519(7) . ?
C211 C212 1.541(7) . ?
C23 C24 1.376(7) . ?
C23 C22 1.387(7) . ?
C3S C2S 1.518(8) . ?
C3S C4S 1.523(7) . ?
C11 C10 1.414(6) . ?
C11 C111 1.507(6) . ?
C11A C10B 1.507(6) . ?
C11A C13A 1.538(7) . ?
C11A C12A 1.538(7) . ?
C851 C852 1.483(8) . ?
C851 C853 1.509(8) . ?
C80 C81 1.409(7) . ?
C551 C55 1.516(7) . ?
C551 C552 1.517(7) . ?
C551 C553 1.543(7) . ?
C11F C13F 1.518(7) . ?
C11F C12F 1.548(7) . ?
C111 C113 1.497(7) . ?
C111 C112 1.516(8) . ?
C90 C91 1.389(7) . ?
C90 C95 1.409(7) . ?
C55 C54 1.402(7) . ?
C10B C10C 1.393(6) . ?
C53 C54 1.380(7) . ?
C53 C52 1.382(7) . ?
C20A C20F 1.403(7) . ?
C93 C94 1.381(7) . ?
C93 C92 1.381(8) . ?
C21 C22 1.408(7) . ?
C51 C52 1.412(7) . ?
C51 C511 1.510(7) . ?
C45 C44 1.405(7) . ?
C911 C91 1.510(7) . ?
C911 C913 1.524(8) . ?
C911 C912 1.530(8) . ?
C82 C83 1.368(8) . ?
C82 C81 1.398(7) . ?
C91 C92 1.402(6) . ?
C20E C20D 1.383(8) . ?
C20E C20F 1.398(7) . ?
C511 C512 1.533(7) . ?
C511 C513 1.536(7) . ?
C31 C32 1.402(7) . ?
C811 C81 1.528(7) . ?
C811 C813 1.534(7) . ?
C811 C812 1.537(7) . ?
C611 C613 1.530(7) . ?
C611 C612 1.534(7) . ?
C20F C21F 1.505(7) . ?
C33 C32 1.388(7) . ?
C22A C21A 1.539(8) . ?
C41 C42 1.389(6) . ?
C72 C73 1.381(7) . ?
C65 C64 1.391(7) . ?
C65 C651 1.503(8) . ?
C83 C84 1.387(8) . ?
C42 C43 1.375(7) . ?
C21F C22F 1.515(7) . ?
C21F C23F 1.530(7) . ?
C74 C73 1.390(7) . ?
C21A C23A 1.534(7) . ?
C751 C753 1.536(7) . ?
C62 C63 1.365(8) . ?
C1S C2S 1.515(8) . ?
C6S C7S 1.519(7) . ?
C6S C5S 1.525(7) . ?
C94 C95 1.393(6) . ?
C8S C7S 1.504(7) . ?
C64 C63 1.396(8) . ?
C651 C652 1.519(8) . ?
C651 C653 1.535(7) . ?
C20C C20D 1.377(8) . ?
C43 C44 1.385(8) . ?
C251 C253 1.515(15) . ?
C251 C252 1.527(16) . ?
C254 C256 1.516(15) . ?
C254 C255 1.534(17) . ?
O4S C15S 1.414(8) . ?
O4S C14S 1.452(9) . ?
C15S C16S 1.529(9) . ?
C13S C14S 1.474(11) . ?
C9T C10T 1.466(11) . ?
C10T O3T 1.326(9) . ?
O3T C11T 1.427(9) . ?
C11T C12T 1.430(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1S Sn1 P4 86.98(9) . . ?
O1S Sn1 P3 91.75(9) . . ?
P4 Sn1 P3 88.22(4) . . ?
O1S Sn1 P2 84.12(9) . . ?
P4 Sn1 P2 132.93(4) . . ?
P3 Sn1 P2 46.16(4) . . ?
O8 Nb3 O9 104.59(13) . . ?
O8 Nb3 O7 104.88(13) . . ?
O9 Nb3 O7 109.55(13) . . ?
O8 Nb3 P7 99.40(10) . . ?
O9 Nb3 P7 143.67(10) . . ?
O7 Nb3 P7 89.73(9) . . ?
O8 Nb3 P9 97.84(10) . . ?
O9 Nb3 P9 98.04(10) . . ?
O7 Nb3 P9 137.91(10) . . ?
P7 Nb3 P9 51.41(4) . . ?
O8 Nb3 P8 145.03(10) . . ?
O9 Nb3 P8 95.39(10) . . ?
O7 Nb3 P8 94.74(10) . . ?
P7 Nb3 P8 51.32(4) . . ?
P9 Nb3 P8 50.43(4) . . ?
P11 P12 P10 58.88(6) . . ?
P11 P12 Nb4 63.98(5) . . ?
P10 P12 Nb4 62.59(4) . . ?
P11 P12 Sn2 87.39(5) . . ?
P10 P12 Sn2 72.48(5) . . ?
Nb4 P12 Sn2 134.47(5) . . ?
O2S Sn2 P7 89.93(9) . . ?
O2S Sn2 P12 92.45(9) . . ?
P7 Sn2 P12 92.23(4) . . ?
O2S Sn2 P10 83.04(9) . . ?
P7 Sn2 P10 137.54(4) . . ?
P12 Sn2 P10 46.66(4) . . ?
O6 Nb2 O4 105.61(14) . . ?
O6 Nb2 O5 104.94(13) . . ?
O4 Nb2 O5 109.75(13) . . ?
O6 Nb2 P4 100.14(10) . . ?
O4 Nb2 P4 142.03(10) . . ?
O5 Nb2 P4 89.50(10) . . ?
O6 Nb2 P6 98.14(10) . . ?
O4 Nb2 P6 96.99(10) . . ?
O5 Nb2 P6 137.83(10) . . ?
P4 Nb2 P6 51.51(4) . . ?
O6 Nb2 P5 145.73(10) . . ?
O4 Nb2 P5 93.22(10) . . ?
O5 Nb2 P5 94.84(10) . . ?
P4 Nb2 P5 51.61(4) . . ?
P6 Nb2 P5 50.47(5) . . ?
P5 P6 P4 60.73(6) . . ?
P5 P6 Nb2 65.30(5) . . ?
P4 P6 Nb2 63.60(5) . . ?
O11 Nb4 O10 106.67(13) . . ?
O11 Nb4 O12 103.66(13) . . ?
O10 Nb4 O12 108.99(13) . . ?
O11 Nb4 P10 99.60(10) . . ?
O10 Nb4 P10 141.01(10) . . ?
O12 Nb4 P10 91.71(9) . . ?
O11 Nb4 P11 99.92(10) . . ?
O10 Nb4 P11 95.84(10) . . ?
O12 Nb4 P11 138.67(9) . . ?
P10 Nb4 P11 50.85(4) . . ?
O11 Nb4 P12 146.97(9) . . ?
O10 Nb4 P12 92.63(10) . . ?
O12 Nb4 P12 94.63(9) . . ?
P10 Nb4 P12 51.97(4) . . ?
P11 Nb4 P12 50.60(4) . . ?
P10 P11 P12 61.52(6) . . ?
P10 P11 Nb4 63.82(5) . . ?
P12 P11 Nb4 65.42(5) . . ?
O3 Nb1 O2 104.57(13) . . ?
O3 Nb1 O1 103.77(13) . . ?
O2 Nb1 O1 109.66(13) . . ?
O3 Nb1 P2 100.33(10) . . ?
O2 Nb1 P2 142.25(10) . . ?
O1 Nb1 P2 91.09(10) . . ?
O3 Nb1 P1 99.21(10) . . ?
O2 Nb1 P1 96.96(10) . . ?
O1 Nb1 P1 138.64(10) . . ?
P2 Nb1 P1 50.85(5) . . ?
O3 Nb1 P3 146.98(10) . . ?
O2 Nb1 P3 94.18(10) . . ?
O1 Nb1 P3 94.88(10) . . ?
P2 Nb1 P3 51.68(4) . . ?
P1 Nb1 P3 50.95(4) . . ?
P6 P5 P4 60.08(6) . . ?
P6 P5 Nb2 64.23(5) . . ?
P4 P5 Nb2 63.03(5) . . ?
P8 P9 P7 60.54(6) . . ?
P8 P9 Nb3 65.20(5) . . ?
P7 P9 Nb3 64.07(5) . . ?
P6 P4 P5 59.19(6) . . ?
P6 P4 Nb2 64.90(5) . . ?
P5 P4 Nb2 65.37(5) . . ?
P6 P4 Sn1 87.07(5) . . ?
P5 P4 Sn1 78.79(5) . . ?
Nb2 P4 Sn1 142.18(5) . . ?
P9 P8 P7 60.35(6) . . ?
P9 P8 Nb3 64.37(5) . . ?
P7 P8 Nb3 63.71(5) . . ?
P11 P10 P12 59.60(6) . . ?
P11 P10 Nb4 65.32(5) . . ?
P12 P10 Nb4 65.45(4) . . ?
P11 P10 Sn2 81.67(5) . . ?
P12 P10 Sn2 60.86(4) . . ?
Nb4 P10 Sn2 125.82(5) . . ?
P9 P7 P8 59.11(6) . . ?
P9 P7 Nb3 64.52(5) . . ?
P8 P7 Nb3 64.97(5) . . ?
P9 P7 Sn2 83.67(5) . . ?
P8 P7 Sn2 81.90(5) . . ?
Nb3 P7 Sn2 142.31(5) . . ?
P1 P3 P2 58.88(6) . . ?
P1 P3 Nb1 63.59(5) . . ?
P2 P3 Nb1 63.08(5) . . ?
P1 P3 Sn1 81.75(5) . . ?
P2 P3 Sn1 72.84(5) . . ?
Nb1 P3 Sn1 133.46(5) . . ?
P1 P2 P3 59.96(6) . . ?
P1 P2 Nb1 64.74(5) . . ?
P3 P2 Nb1 65.24(5) . . ?
P1 P2 Sn1 76.45(5) . . ?
P3 P2 Sn1 61.00(5) . . ?
Nb1 P2 Sn1 124.24(5) . . ?
P2 P1 P3 61.17(6) . . ?
P2 P1 Nb1 64.41(5) . . ?
P3 P1 Nb1 65.46(5) . . ?
C50 O5 Nb2 141.9(3) . . ?
C80 O8 Nb3 162.0(3) . . ?
C30A O12 Nb4 144.1(3) . . ?
C30 O3 Nb1 159.0(3) . . ?
C20A O11 Nb4 159.1(3) . . ?
C20 O2 Nb1 152.0(3) . . ?
C10A O10 Nb4 148.4(3) . . ?
C70 O7 Nb3 138.7(3) . . ?
C40 O4 Nb2 142.3(3) . . ?
C10 O1 Nb1 142.6(3) . . ?
C90 O9 Nb3 147.1(3) . . ?
C8S O2S C5S 109.9(4) . . ?
C8S O2S Sn2 126.3(3) . . ?
C5S O2S Sn2 123.8(3) . . ?
C1S O1S C4S 110.0(4) . . ?
C1S O1S Sn1 119.6(3) . . ?
C4S O1S Sn1 125.9(3) . . ?
C60 O6 Nb2 163.9(3) . . ?
C13 C12 C11 122.3(5) . . ?
O10 C10A C10B 119.5(4) . . ?
O10 C10A C10F 118.0(4) . . ?
C10B C10A C10F 122.5(4) . . ?
C95 C914 C916 113.9(4) . . ?
C95 C914 C915 110.9(4) . . ?
C916 C914 C915 109.8(4) . . ?
C14 C15 C10 117.2(4) . . ?
C14 C15 C151 120.0(4) . . ?
C10 C15 C151 122.7(5) . . ?
C80 C85 C84 117.2(5) . . ?
C80 C85 C851 122.5(5) . . ?
C84 C85 C851 120.3(5) . . ?
C34 C35 C30 116.4(4) . . ?
C34 C35 C351 123.2(4) . . ?
C30 C35 C351 120.5(4) . . ?
C30E C30D C30C 119.8(5) . . ?
O2 C20 C21 119.4(4) . . ?
O2 C20 C25 118.5(4) . . ?
C21 C20 C25 122.0(4) . . ?
O12 C30A C30B 120.1(4) . . ?
O12 C30A C30F 118.0(4) . . ?
C30B C30A C30F 121.9(4) . . ?
O6 C60 C61 120.0(4) . . ?
O6 C60 C65 116.8(4) . . ?
C61 C60 C65 123.2(4) . . ?
C30D C30C C30B 120.8(5) . . ?
C72 C71 C70 117.6(4) . . ?
C72 C71 C711 120.0(4) . . ?
C70 C71 C711 122.3(4) . . ?
O5 C50 C51 119.5(4) . . ?
O5 C50 C55 119.1(4) . . ?
C51 C50 C55 121.3(4) . . ?
C41 C411 C412 114.5(4) . . ?
C41 C411 C413 111.6(4) . . ?
C412 C411 C413 108.8(4) . . ?
C30A C30B C30C 118.7(4) . . ?
C30A C30B C31A 121.7(4) . . ?
C30C C30B C31A 119.6(4) . . ?
C33 C34 C35 121.5(4) . . ?
O3 C30 C31 120.0(4) . . ?
O3 C30 C35 116.5(4) . . ?
C31 C30 C35 123.6(4) . . ?
C713 C711 C71 113.6(4) . . ?
C713 C711 C712 110.0(4) . . ?
C71 C711 C712 110.4(4) . . ?
C10E C10D C10C 120.7(5) . . ?
C30D C30E C30F 122.1(5) . . ?
C30F C31F C33F 111.0(4) . . ?
C30F C31F C32F 111.1(4) . . ?
C33F C31F C32F 110.2(4) . . ?
C452 C451 C45 109.7(5) . . ?
C452 C451 C453 111.4(5) . . ?
C45 C451 C453 112.9(5) . . ?
C35 C351 C353 113.4(4) . . ?
C35 C351 C352 111.3(4) . . ?
C353 C351 C352 109.8(4) . . ?
C20C C20B C20A 117.7(5) . . ?
C20C C20B C21A 123.0(5) . . ?
C20A C20B C21A 119.3(4) . . ?
C30E C30F C30A 116.7(4) . . ?
C30E C30F C31F 120.6(4) . . ?
C30A C30F C31F 122.7(4) . . ?
C30B C31A C32A 111.3(4) . . ?
C30B C31A C33A 110.4(4) . . ?
C32A C31A C33A 111.6(4) . . ?
C13 C14 C15 122.3(5) . . ?
C10D C10E C10F 121.7(5) . . ?
C62 C61 C60 116.7(5) . . ?
C62 C61 C611 122.2(5) . . ?
C60 C61 C611 121.1(4) . . ?
C45 C40 O4 118.3(4) . . ?
C45 C40 C41 123.8(4) . . ?
O4 C40 C41 117.9(4) . . ?
C74 C75 C70 118.2(4) . . ?
C74 C75 C751 120.1(4) . . ?
C70 C75 C751 121.7(4) . . ?
C15 C151 C152 111.5(4) . . ?
C15 C151 C153 111.8(4) . . ?
C152 C151 C153 110.6(4) . . ?
C24 C25 C20 117.8(5) . . ?
C24 C25 C251 122.5(15) . . ?
C20 C25 C251 119.7(15) . . ?
C24 C25 C254 120.4(18) . . ?
C20 C25 C254 121.5(17) . . ?
C251 C25 C254 6(2) . . ?
C12 C13 C14 119.1(5) . . ?
C31 C311 C312 110.5(4) . . ?
C31 C311 C313 113.2(4) . . ?
C312 C311 C313 110.3(4) . . ?
C10E C10F C10A 116.6(4) . . ?
C10E C10F C11F 120.3(4) . . ?
C10A C10F C11F 123.1(4) . . ?
C213 C211 C21 110.1(4) . . ?
C213 C211 C212 110.5(5) . . ?
C21 C211 C212 112.5(4) . . ?
C24 C23 C22 120.2(5) . . ?
C2S C3S C4S 102.2(4) . . ?
C12 C11 C10 117.1(4) . . ?
C12 C11 C111 121.3(4) . . ?
C10 C11 C111 121.4(4) . . ?
C10B C11A C13A 112.8(4) . . ?
C10B C11A C12A 109.9(4) . . ?
C13A C11A C12A 110.2(4) . . ?
O7 C70 C71 118.2(4) . . ?
O7 C70 C75 120.0(4) . . ?
C71 C70 C75 121.8(4) . . ?
C852 C851 C85 111.0(5) . . ?
C852 C851 C853 109.4(5) . . ?
C85 C851 C853 115.5(5) . . ?
C85 C80 O8 120.5(4) . . ?
C85 C80 C81 123.4(5) . . ?
O8 C80 C81 116.1(4) . . ?
C55 C551 C552 113.5(4) . . ?
C55 C551 C553 110.8(4) . . ?
C552 C551 C553 111.2(4) . . ?
C10F C11F C13F 111.8(4) . . ?
C10F C11F C12F 111.3(4) . . ?
C13F C11F C12F 107.6(4) . . ?
C113 C111 C11 110.3(4) . . ?
C113 C111 C112 109.6(5) . . ?
C11 C111 C112 114.6(5) . . ?
O9 C90 C91 118.6(4) . . ?
O9 C90 C95 117.8(4) . . ?
C91 C90 C95 123.6(4) . . ?
C54 C55 C50 118.3(5) . . ?
C54 C55 C551 120.2(4) . . ?
C50 C55 C551 121.4(4) . . ?
C10C C10B C10A 117.9(4) . . ?
C10C C10B C11A 119.3(4) . . ?
C10A C10B C11A 122.6(4) . . ?
C54 C53 C52 119.9(5) . . ?
O11 C20A C20F 119.6(4) . . ?
O11 C20A C20B 117.3(4) . . ?
C20F C20A C20B 123.0(4) . . ?
C94 C93 C92 120.2(4) . . ?
C20 C21 C22 117.5(5) . . ?
C20 C21 C211 123.2(4) . . ?
C22 C21 C211 119.3(5) . . ?
C50 C51 C52 117.8(4) . . ?
C50 C51 C511 122.6(4) . . ?
C52 C51 C511 119.6(5) . . ?
C40 C45 C44 117.5(5) . . ?
C40 C45 C451 122.8(5) . . ?
C44 C45 C451 119.7(5) . . ?
C91 C911 C913 110.4(5) . . ?
C91 C911 C912 112.4(5) . . ?
C913 C911 C912 112.4(5) . . ?
C83 C82 C81 122.0(5) . . ?
O1 C10 C15 119.7(4) . . ?
O1 C10 C11 118.4(4) . . ?
C15 C10 C11 121.9(4) . . ?
C90 C91 C92 116.7(5) . . ?
C90 C91 C911 123.7(4) . . ?
C92 C91 C911 119.5(5) . . ?
C23 C24 C25 121.5(5) . . ?
C20D C20E C20F 121.5(5) . . ?
C51 C511 C512 112.5(4) . . ?
C51 C511 C513 111.4(4) . . ?
C512 C511 C513 109.4(5) . . ?
C30 C31 C32 117.1(4) . . ?
C30 C31 C311 120.2(4) . . ?
C32 C31 C311 122.7(4) . . ?
C81 C811 C813 113.5(5) . . ?
C81 C811 C812 109.3(4) . . ?
C813 C811 C812 109.9(5) . . ?
C61 C611 C613 114.3(5) . . ?
C61 C611 C612 110.0(4) . . ?
C613 C611 C612 109.9(4) . . ?
C20E C20F C20A 116.4(5) . . ?
C20E C20F C21F 123.1(5) . . ?
C20A C20F C21F 120.6(4) . . ?
C34 C33 C32 120.9(4) . . ?
C42 C41 C40 116.8(5) . . ?
C42 C41 C411 122.8(5) . . ?
C40 C41 C411 120.4(4) . . ?
C73 C72 C71 121.0(4) . . ?
C64 C65 C60 116.4(5) . . ?
C64 C65 C651 123.8(5) . . ?
C60 C65 C651 119.8(4) . . ?
C82 C83 C84 120.0(5) . . ?
C23 C22 C21 120.9(5) . . ?
C43 C42 C41 121.1(5) . . ?
C20F C21F C22F 111.8(4) . . ?
C20F C21F C23F 113.7(4) . . ?
C22F C21F C23F 110.6(4) . . ?
C53 C54 C55 121.3(5) . . ?
C75 C74 C73 120.9(5) . . ?
C10D C10C C10B 120.6(5) . . ?
C72 C73 C74 120.5(5) . . ?
C20B C21A C23A 113.3(5) . . ?
C20B C21A C22A 111.1(4) . . ?
C23A C21A C22A 110.0(5) . . ?
C75 C751 C752 112.6(4) . . ?
C75 C751 C753 109.9(4) . . ?
C752 C751 C753 108.9(4) . . ?
C53 C52 C51 121.5(5) . . ?
C63 C62 C61 122.0(5) . . ?
O1S C1S C2S 106.3(5) . . ?
C82 C81 C80 116.4(5) . . ?
C82 C81 C811 123.6(5) . . ?
C80 C81 C811 120.0(4) . . ?
C7S C6S C5S 102.5(4) . . ?
C93 C94 C95 121.4(5) . . ?
O2S C8S C7S 105.5(4) . . ?
C65 C64 C63 122.2(5) . . ?
C94 C95 C90 116.6(5) . . ?
C94 C95 C914 123.4(5) . . ?
C90 C95 C914 119.9(4) . . ?
C8S C7S C6S 103.3(4) . . ?
O2S C5S C6S 103.3(4) . . ?
C65 C651 C652 110.5(5) . . ?
C65 C651 C653 113.2(5) . . ?
C652 C651 C653 110.4(5) . . ?
C33 C32 C31 120.6(4) . . ?
C20D C20C C20B 120.7(5) . . ?
C62 C63 C64 119.5(5) . . ?
C42 C43 C44 121.1(5) . . ?
O1S C4S C3S 104.9(4) . . ?
C83 C84 C85 120.8(5) . . ?
C20C C20D C20E 120.7(5) . . ?
C253 C251 C25 115(3) . . ?
C253 C251 C252 110.0(13) . . ?
C25 C251 C252 107(2) . . ?
C256 C254 C25 110(3) . . ?
C256 C254 C255 111.5(13) . . ?
C25 C254 C255 112(3) . . ?
C93 C92 C91 121.3(5) . . ?
C43 C44 C45 119.7(5) . . ?
C1S C2S C3S 102.2(5) . . ?
C15S O4S C14S 109.3(6) . . ?
O4S C15S C16S 104.9(6) . . ?
O4S C14S C13S 113.9(7) . . ?
O3T C10T C9T 116.4(8) . . ?
C10T O3T C11T 119.6(7) . . ?
O3T C11T C12T 112.2(7) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.103
####################################################################### 
# 
# 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_final1
_database_code_depnum_ccdc_archive 'CCDC 1421303'
_audit_update_record             
;
2015-08-28 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48.80 H69.19 Nb O4 P3 Pb0.50'
_chemical_formula_weight         1009.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.9973(14)
_cell_length_b                   12.5011(7)
_cell_length_c                   33.949(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.4730(10)
_cell_angle_gamma                90.00
_cell_volume                     9944.0(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9568
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      30.68

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4168
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4925
_exptl_absorpt_correction_T_max  0.9039
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'

_exptl_special_details           
; 
 'Siemens three-circle diffractometer, Bruker APEX CCD' 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            109407
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         29.57
_reflns_number_total             13959
_reflns_number_gt                12695
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0158P)²+20.7899P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13959
_refine_ls_number_parameters     668
_refine_ls_number_restraints     485
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0585
_refine_ls_wR_factor_gt          0.0569
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.075208(7) 0.290307(14) 0.131502(5) 0.01690(4) Uani 1 1 d . . .
Pb1 Pb 0.0000 0.429862(9) 0.2500 0.01899(3) Uani 1 2 d S . .
P1 P 0.04200(3) 0.28420(4) 0.198989(16) 0.02414(11) Uani 1 1 d . . .
P2 P 0.11511(3) 0.38697(5) 0.197372(17) 0.02715(12) Uani 1 1 d . . .
P3 P 0.03067(3) 0.43589(5) 0.164749(16) 0.02599(11) Uani 1 1 d . . .
O1 O 0.10438(6) 0.37203(11) 0.09369(4) 0.0201(3) Uani 1 1 d . . .
O2 O 0.13126(6) 0.17748(12) 0.14692(4) 0.0236(3) Uani 1 1 d . . .
O3 O 0.00560(6) 0.23159(12) 0.10019(4) 0.0226(3) Uani 1 1 d . . .
C11 C 0.13923(8) 0.42343(17) 0.07274(6) 0.0211(4) Uani 1 1 d . . .
C12 C 0.15865(8) 0.36437(18) 0.04317(6) 0.0235(4) Uani 1 1 d . . .
C121 C 0.13813(9) 0.25043(18) 0.03380(6) 0.0257(4) Uani 1 1 d . . .
H121 H 0.1397 0.2136 0.0602 0.031 Uiso 1 1 calc R . .
C122 C 0.17522(12) 0.1860(2) 0.01102(8) 0.0399(6) Uani 1 1 d . . .
H12A H 0.1731 0.2178 -0.0156 0.060 Uiso 1 1 calc R . .
H12B H 0.1615 0.1120 0.0079 0.060 Uiso 1 1 calc R . .
H12C H 0.2149 0.1869 0.0262 0.060 Uiso 1 1 calc R . .
C123 C 0.07560(10) 0.2489(2) 0.01069(7) 0.0314(5) Uani 1 1 d . . .
H12D H 0.0522 0.2893 0.0259 0.047 Uiso 1 1 calc R . .
H12E H 0.0621 0.1749 0.0074 0.047 Uiso 1 1 calc R . .
H12F H 0.0727 0.2818 -0.0159 0.047 Uiso 1 1 calc R . .
C13 C 0.19677(9) 0.4158(2) 0.02369(7) 0.0316(5) Uani 1 1 d . . .
H13 H 0.2114 0.3782 0.0038 0.038 Uiso 1 1 calc R . .
C14 C 0.21369(10) 0.5207(2) 0.03276(8) 0.0373(6) Uani 1 1 d . . .
H14 H 0.2400 0.5539 0.0193 0.045 Uiso 1 1 calc R . .
C15 C 0.19245(10) 0.5770(2) 0.06132(7) 0.0345(5) Uani 1 1 d . . .
H15 H 0.2037 0.6493 0.0668 0.041 Uiso 1 1 calc R . .
C16 C 0.15487(9) 0.52978(18) 0.08224(6) 0.0258(4) Uani 1 1 d . . .
C161 C 0.13063(11) 0.59071(18) 0.11314(7) 0.0318(5) Uani 1 1 d . . .
H161 H 0.1228 0.5373 0.1332 0.038 Uiso 1 1 calc R . .
C162 C 0.07392(13) 0.6415(3) 0.09362(9) 0.0473(7) Uani 1 1 d . . .
H16A H 0.0801 0.6962 0.0743 0.071 Uiso 1 1 calc R . .
H16B H 0.0570 0.6747 0.1145 0.071 Uiso 1 1 calc R . .
H16C H 0.0481 0.5865 0.0795 0.071 Uiso 1 1 calc R . .
C163 C 0.17185(15) 0.6734(2) 0.13650(9) 0.0524(8) Uani 1 1 d . . .
H16D H 0.2095 0.6407 0.1458 0.079 Uiso 1 1 calc R . .
H16E H 0.1575 0.6985 0.1598 0.079 Uiso 1 1 calc R . .
H16F H 0.1750 0.7341 0.1188 0.079 Uiso 1 1 calc R . .
C21 C 0.17569(10) 0.15610(19) 0.17900(6) 0.0293(5) Uani 1 1 d . . .
C22 C 0.16711(12) 0.0831(2) 0.20858(7) 0.0395(6) Uani 1 1 d . . .
C221 C 0.11241(13) 0.0201(2) 0.20383(8) 0.0420(6) Uani 1 1 d . . .
H221 H 0.0824 0.0588 0.1839 0.050 Uiso 1 1 calc R . .
C222 C 0.11994(17) -0.0906(2) 0.18625(10) 0.0598(9) Uani 1 1 d . . .
H22A H 0.1303 -0.0823 0.1600 0.090 Uiso 1 1 calc R . .
H22B H 0.0841 -0.1306 0.1828 0.090 Uiso 1 1 calc R . .
H22C H 0.1502 -0.1296 0.2047 0.090 Uiso 1 1 calc R . .
C223 C 0.09083(16) 0.0083(3) 0.24297(9) 0.0573(9) Uani 1 1 d . . .
H22D H 0.0538 -0.0282 0.2372 0.086 Uiso 1 1 calc R . .
H22E H 0.0866 0.0792 0.2542 0.086 Uiso 1 1 calc R . .
H22F H 0.1183 -0.0338 0.2625 0.086 Uiso 1 1 calc R . .
C23 C 0.21307(15) 0.0675(3) 0.24151(8) 0.0547(9) Uani 1 1 d . . .
H23 H 0.2087 0.0191 0.2622 0.066 Uiso 1 1 calc R . .
C24 C 0.26418(14) 0.1201(3) 0.24472(8) 0.0580(9) Uani 1 1 d . . .
H24 H 0.2941 0.1092 0.2677 0.070 Uiso 1 1 calc R . .
C25 C 0.27185(12) 0.1882(3) 0.21476(8) 0.0483(7) Uani 1 1 d . . .
H25 H 0.3076 0.2231 0.2170 0.058 Uiso 1 1 calc R . .
C26 C 0.22820(11) 0.2074(2) 0.18080(7) 0.0347(5) Uani 1 1 d . . .
C261 C 0.23869(10) 0.2778(2) 0.14683(8) 0.0354(5) Uani 1 1 d . . .
H261 H 0.2010 0.2887 0.1278 0.042 Uiso 1 1 calc R . .
C263 C 0.26217(13) 0.3884(3) 0.16060(11) 0.0544(8) Uani 1 1 d . . .
H26A H 0.2366 0.4236 0.1755 0.082 Uiso 1 1 calc R . .
H26B H 0.2649 0.4316 0.1370 0.082 Uiso 1 1 calc R . .
H26C H 0.3001 0.3810 0.1782 0.082 Uiso 1 1 calc R . .
C262 C 0.27790(14) 0.2228(3) 0.12311(9) 0.0526(8) Uani 1 1 d . . .
H26D H 0.3155 0.2112 0.1408 0.079 Uiso 1 1 calc R . .
H26E H 0.2820 0.2681 0.1003 0.079 Uiso 1 1 calc R . .
H26F H 0.2614 0.1538 0.1130 0.079 Uiso 1 1 calc R . .
C31 C -0.05264(9) 0.22696(19) 0.09329(6) 0.0261(4) Uani 1 1 d . . .
C32 C -0.07820(11) 0.1308(2) 0.10155(7) 0.0335(5) Uani 1 1 d . . .
C321 C -0.04307(12) 0.0344(2) 0.11784(8) 0.0391(6) Uani 1 1 d . . .
H321 H -0.0020 0.0545 0.1208 0.047 Uiso 1 1 calc R . .
C322 C -0.05451(19) -0.0614(3) 0.08888(11) 0.0711(11) Uani 1 1 d . . .
H32A H -0.0944 -0.0839 0.0855 0.107 Uiso 1 1 calc R . .
H32B H -0.0293 -0.1207 0.1000 0.107 Uiso 1 1 calc R . .
H32C H -0.0472 -0.0406 0.0626 0.107 Uiso 1 1 calc R . .
C323 C -0.05147(17) 0.0027(3) 0.15971(10) 0.0619(9) Uani 1 1 d . . .
H32D H -0.0427 0.0640 0.1780 0.093 Uiso 1 1 calc R . .
H32E H -0.0259 -0.0567 0.1701 0.093 Uiso 1 1 calc R . .
H32F H -0.0911 -0.0194 0.1578 0.093 Uiso 1 1 calc R . .
C33 C -0.13818(12) 0.1276(3) 0.09333(8) 0.0453(7) Uani 1 1 d . . .
H33 H -0.1568 0.0638 0.0986 0.054 Uiso 1 1 calc R . .
C34 C -0.17038(11) 0.2149(3) 0.07777(9) 0.0487(7) Uani 1 1 d . . .
H34 H -0.2108 0.2110 0.0727 0.058 Uiso 1 1 calc R . .
C35 C -0.14451(10) 0.3079(3) 0.06952(8) 0.0404(6) Uani 1 1 d . . .
H35 H -0.1675 0.3671 0.0585 0.048 Uiso 1 1 calc R . .
C36 C -0.08501(9) 0.3169(2) 0.07707(6) 0.0285(5) Uani 1 1 d . . .
C361 C -0.05820(9) 0.4191(2) 0.06592(7) 0.0300(5) Uani 1 1 d . . .
H361 H -0.0168 0.4176 0.0795 0.036 Uiso 1 1 calc R . .
C362 C -0.08445(12) 0.5193(2) 0.08072(9) 0.0429(6) Uani 1 1 d . . .
H36A H -0.1239 0.5276 0.0657 0.064 Uiso 1 1 calc R . .
H36B H -0.0622 0.5824 0.0764 0.064 Uiso 1 1 calc R . .
H36C H -0.0839 0.5121 0.1095 0.064 Uiso 1 1 calc R . .
C363 C -0.06205(11) 0.4246(2) 0.02028(7) 0.0388(6) Uani 1 1 d . . .
H36D H -0.0429 0.3622 0.0117 0.058 Uiso 1 1 calc R . .
H36E H -0.0434 0.4900 0.0138 0.058 Uiso 1 1 calc R . .
H36F H -0.1022 0.4250 0.0061 0.058 Uiso 1 1 calc R . .
O1S O -0.09680(7) 0.39782(13) 0.20021(5) 0.0302(3) Uani 1 1 d . . .
C1SA C -0.1428(4) 0.4718(10) 0.1945(4) 0.0422(14) Uani 0.762(13) 1 d PU A 1
H1S1 H -0.1352 0.5335 0.1781 0.051 Uiso 0.762(13) 1 calc PR A 1
H1S2 H -0.1486 0.4986 0.2207 0.051 Uiso 0.762(13) 1 calc PR A 1
C2SA C -0.19443(18) 0.4106(5) 0.1727(2) 0.0653(19) Uani 0.762(13) 1 d PU A 1
H2S1 H -0.2293 0.4351 0.1812 0.078 Uiso 0.762(13) 1 calc PR A 1
H2S2 H -0.2000 0.4193 0.1431 0.078 Uiso 0.762(13) 1 calc PR A 1
C3SA C -0.1815(4) 0.2994(8) 0.1845(3) 0.071(3) Uani 0.762(13) 1 d PU A 1
H3S1 H -0.2027 0.2493 0.1641 0.085 Uiso 0.762(13) 1 calc PR A 1
H3S2 H -0.1907 0.2836 0.2110 0.085 Uiso 0.762(13) 1 calc PR A 1
C4SA C -0.1135(3) 0.2924(7) 0.1869(3) 0.0341(10) Uani 0.762(13) 1 d PU A 1
H4S1 H -0.0950 0.2379 0.2066 0.041 Uiso 0.762(13) 1 calc PR A 1
H4S2 H -0.1049 0.2771 0.1602 0.041 Uiso 0.762(13) 1 calc PR A 1
C1SB C -0.1531(15) 0.459(4) 0.1930(15) 0.0422(14) Uani 0.238(13) 1 d PU A 2
H1S3 H -0.1515 0.5159 0.2135 0.051 Uiso 0.238(13) 1 calc PR A 2
H1S4 H -0.1611 0.4925 0.1659 0.051 Uiso 0.238(13) 1 calc PR A 2
C2SB C -0.1993(5) 0.3780(16) 0.1960(7) 0.056(4) Uani 0.238(13) 1 d PU A 2
H2S3 H -0.2101 0.3817 0.2225 0.067 Uiso 0.238(13) 1 calc PR A 2
H2S4 H -0.2337 0.3877 0.1743 0.067 Uiso 0.238(13) 1 calc PR A 2
C3SB C -0.1694(11) 0.277(2) 0.1912(7) 0.046(4) Uani 0.238(13) 1 d PU A 2
H3S3 H -0.1729 0.2276 0.2135 0.056 Uiso 0.238(13) 1 calc PR A 2
H3S4 H -0.1886 0.2424 0.1656 0.056 Uiso 0.238(13) 1 calc PR A 2
C4SB C -0.1248(11) 0.287(3) 0.1912(10) 0.0341(10) Uani 0.238(13) 1 d PU A 2
H4S3 H -0.1193 0.2641 0.1643 0.041 Uiso 0.238(13) 1 calc PR A 2
H4S4 H -0.1032 0.2358 0.2111 0.041 Uiso 0.238(13) 1 calc PR A 2
C1T C 0.1625(2) 0.9791(5) 0.08566(17) 0.0378(10) Uani 0.854(16) 1 d PDU B 1
H1T H 0.1778 1.0167 0.1099 0.045 Uiso 0.854(16) 1 calc PR B 1
C2T C 0.19896(19) 0.9223(4) 0.06580(16) 0.0365(10) Uani 0.854(16) 1 d PDU B 1
H2T H 0.2390 0.9218 0.0765 0.044 Uiso 0.854(16) 1 calc PR B 1
C3T C 0.1765(3) 0.8676(3) 0.03082(16) 0.0384(12) Uani 0.854(16) 1 d PDU B 1
H3T H 0.2012 0.8287 0.0176 0.046 Uiso 0.854(16) 1 calc PR B 1
C4T C 0.1189(3) 0.8684(4) 0.01472(13) 0.0419(14) Uani 0.854(16) 1 d PDU B 1
H4T H 0.1039 0.8305 -0.0095 0.050 Uiso 0.854(16) 1 calc PR B 1
C5T C 0.0824(2) 0.9247(7) 0.0338(2) 0.0477(13) Uani 0.854(16) 1 d PDU B 1
H5T H 0.0425 0.9258 0.0226 0.057 Uiso 0.854(16) 1 calc PR B 1
C6T C 0.1043(2) 0.9799(3) 0.06980(15) 0.0431(12) Uani 0.854(16) 1 d PDU B 1
H6T H 0.0794 1.0176 0.0832 0.052 Uiso 0.854(16) 1 calc PR B 1
C1U C 0.1725(17) 0.960(3) 0.0793(10) 0.051(6) Uani 0.146(16) 1 d PDU B 2
H1U H 0.1992 0.9902 0.1012 0.061 Uiso 0.146(16) 1 calc PR B 2
C2U C 0.1890(16) 0.894(3) 0.0538(12) 0.056(6) Uani 0.146(16) 1 d PDU B 2
H2U H 0.2270 0.8677 0.0590 0.068 Uiso 0.146(16) 1 calc PR B 2
C3U C 0.151(2) 0.866(3) 0.0201(10) 0.054(7) Uani 0.146(16) 1 d PDU B 2
H3U H 0.1644 0.8305 -0.0008 0.064 Uiso 0.146(16) 1 calc PR B 2
C4U C 0.0942(19) 0.885(3) 0.0147(9) 0.055(6) Uani 0.146(16) 1 d PDU B 2
H4U H 0.0684 0.8579 -0.0084 0.066 Uiso 0.146(16) 1 calc PR B 2
C5U C 0.0746(16) 0.944(4) 0.0421(12) 0.046(6) Uani 0.146(16) 1 d PDU B 2
H5U H 0.0349 0.9559 0.0393 0.056 Uiso 0.146(16) 1 calc PR B 2
C6U C 0.1116(5) 0.9844(4) 0.0729(4) 0.048(7) Uani 0.146(16) 1 d PDU B 2
H6U H 0.0985 1.0304 0.0913 0.058 Uiso 0.146(16) 1 calc PR B 2
C1V C -0.0593(5) 0.6935(4) 0.2587(4) 0.049(3) Uani 0.300(3) 1 d PRDU C -1
H1V H -0.0964 0.6889 0.2643 0.059 Uiso 0.300(3) 1 d PR C -1
C2V C -0.0530(5) 0.6970(4) 0.2190(4) 0.054(4) Uani 0.300(3) 1 d PRDU C -1
H2V H -0.0857 0.6948 0.1975 0.065 Uiso 0.300(3) 1 d PR C -1
C3V C 0.0011(5) 0.7037(4) 0.2107(4) 0.054(4) Uani 0.300(3) 1 d PRDU C -1
H3V H 0.0054 0.7061 0.1836 0.065 Uiso 0.300(3) 1 d PR C -1
C4V C 0.0490(5) 0.7070(4) 0.2422(4) 0.045(3) Uani 0.300(3) 1 d PRDU C -1
H4V H 0.0860 0.7116 0.2365 0.053 Uiso 0.300(3) 1 d PR C -1
C5V C 0.0427(5) 0.7035(4) 0.2819(4) 0.058(4) Uani 0.300(3) 1 d PRDU C -1
H5V H 0.0754 0.7057 0.3034 0.070 Uiso 0.300(3) 1 d PR C -1
C6V C -0.0115(5) 0.6968(4) 0.2902(4) 0.045(3) Uani 0.300(3) 1 d PRDU C -1
H6V H -0.0158 0.6944 0.3173 0.054 Uiso 0.300(3) 1 d PR C -1
C1W C 0.0509(15) 0.697(4) 0.3151(6) 0.053(7) Uani 0.200(3) 1 d PDU C -2
H1W1 H 0.0529 0.6196 0.3202 0.080 Uiso 0.200(3) 1 calc PR C -2
H1W2 H 0.0510 0.7349 0.3404 0.080 Uiso 0.200(3) 1 calc PR C -2
H1W3 H 0.0840 0.7191 0.3045 0.080 Uiso 0.200(3) 1 calc PR C -2
C2W C -0.0048(11) 0.723(2) 0.2838(6) 0.056(5) Uani 0.200(3) 1 d PDU C -2
H2W1 H -0.0375 0.6954 0.2941 0.067 Uiso 0.200(3) 1 calc PR C -2
H2W2 H -0.0088 0.8021 0.2819 0.067 Uiso 0.200(3) 1 calc PR C -2
C3W C -0.0078(7) 0.6855(7) 0.2477(5) 0.034(3) Uani 0.200(3) 1 d PDU C -2
H3W1 H -0.0124 0.6069 0.2486 0.041 Uiso 0.200(3) 1 calc PR C -2
H3W2 H 0.0289 0.6997 0.2399 0.041 Uiso 0.200(3) 1 calc PR C -2
C4W C -0.0488(9) 0.723(2) 0.2194(6) 0.044(4) Uani 0.200(3) 1 d PDU C -2
H4W1 H -0.0503 0.8018 0.2226 0.053 Uiso 0.200(3) 1 calc PR C -2
H4W2 H -0.0855 0.6936 0.2233 0.053 Uiso 0.200(3) 1 calc PR C -2
C5W C -0.0429(17) 0.698(3) 0.1755(6) 0.058(8) Uani 0.200(3) 1 d PDU C -2
H5W1 H -0.0095 0.7355 0.1700 0.087 Uiso 0.200(3) 1 calc PR C -2
H5W2 H -0.0773 0.7223 0.1564 0.087 Uiso 0.200(3) 1 calc PR C -2
H5W3 H -0.0382 0.6209 0.1725 0.087 Uiso 0.200(3) 1 calc PR C -2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O1 1.8893(14) . ?
Nb1 O3 1.9215(14) . ?
Nb1 O2 1.9413(14) . ?
Nb1 P3 2.4999(6) . ?
Nb1 P2 2.5402(6) . ?
Nb1 P1 2.5843(6) . ?
Pb1 O1S 2.5920(16) 2 ?
Pb1 O1S 2.5920(16) . ?
Pb1 P1 2.8433(5) 2 ?
Pb1 P1 2.8433(5) . ?
Pb1 P3 3.1374(6) . ?
Pb1 P3 3.1375(6) 2 ?
P1 P2 2.1847(8) . ?
P1 P3 2.2100(8) . ?
P2 P3 2.1765(8) . ?
O1 C11 1.369(2) . ?
O2 C21 1.376(2) . ?
O3 C31 1.367(2) . ?
C11 C16 1.400(3) . ?
C11 C12 1.404(3) . ?
C12 C13 1.396(3) . ?
C12 C121 1.518(3) . ?
C121 C122 1.528(3) . ?
C121 C123 1.536(3) . ?
C13 C14 1.387(4) . ?
C14 C15 1.382(4) . ?
C15 C16 1.394(3) . ?
C16 C161 1.511(3) . ?
C161 C162 1.518(4) . ?
C161 C163 1.529(3) . ?
C21 C26 1.403(4) . ?
C21 C22 1.405(3) . ?
C22 C23 1.404(4) . ?
C22 C221 1.510(4) . ?
C221 C222 1.532(4) . ?
C221 C223 1.534(4) . ?
C23 C24 1.375(5) . ?
C24 C25 1.369(5) . ?
C25 C26 1.401(3) . ?
C26 C261 1.514(4) . ?
C261 C262 1.527(4) . ?
C261 C263 1.528(4) . ?
C31 C32 1.405(3) . ?
C31 C36 1.409(3) . ?
C32 C33 1.406(4) . ?
C32 C321 1.506(4) . ?
C321 C323 1.530(4) . ?
C321 C322 1.536(4) . ?
C33 C34 1.375(5) . ?
C34 C35 1.374(4) . ?
C35 C36 1.400(3) . ?
C36 C361 1.515(3) . ?
C361 C363 1.534(3) . ?
C361 C362 1.535(4) . ?
O1S C1SA 1.421(13) . ?
O1S C4SA 1.422(8) . ?
O1S C1SB 1.53(4) . ?
O1S C4SB 1.55(3) . ?
C1SA C2SA 1.508(9) . ?
C2SA C3SA 1.462(10) . ?
C3SA C4SA 1.619(13) . ?
C1SB C2SB 1.52(4) . ?
C2SB C3SB 1.48(3) . ?
C3SB C4SB 1.08(4) . ?
C1T C6T 1.384(6) . ?
C1T C2T 1.406(5) . ?
C2T C3T 1.376(5) . ?
C3T C4T 1.373(6) . ?
C4T C5T 1.389(6) . ?
C5T C6T 1.402(6) . ?
C1U C2U 1.31(3) . ?
C1U C6U 1.46(4) . ?
C2U C3U 1.35(3) . ?
C3U C4U 1.35(4) . ?
C4U C5U 1.35(2) . ?
C5U C6U 1.32(3) . ?
C1V C6V 1.3898 . ?
C1V C2V 1.3900 . ?
C2V C3V 1.3899 . ?
C3V C4V 1.3900 . ?
C4V C5V 1.3900 . ?
C5V C6V 1.3901 . ?
C1W C2W 1.55(3) . ?
C2W C3W 1.304(19) . ?
C3W C4W 1.304(18) . ?
C4W C5W 1.56(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 O3 103.65(6) . . ?
O1 Nb1 O2 103.84(6) . . ?
O3 Nb1 O2 109.91(6) . . ?
O1 Nb1 P3 99.81(4) . . ?
O3 Nb1 P3 97.04(5) . . ?
O2 Nb1 P3 138.26(4) . . ?
O1 Nb1 P2 102.49(4) . . ?
O3 Nb1 P2 141.82(4) . . ?
O2 Nb1 P2 90.05(4) . . ?
P3 Nb1 P2 51.16(2) . . ?
O1 Nb1 P1 148.07(4) . . ?
O3 Nb1 P1 94.68(4) . . ?
O2 Nb1 P1 93.90(4) . . ?
P3 Nb1 P1 51.497(18) . . ?
P2 Nb1 P1 50.459(19) . . ?
O1S Pb1 O1S 162.22(7) 2 . ?
O1S Pb1 P1 83.65(4) 2 2 ?
O1S Pb1 P1 84.99(4) . 2 ?
O1S Pb1 P1 84.99(4) 2 . ?
O1S Pb1 P1 83.65(4) . . ?
P1 Pb1 P1 100.35(2) 2 . ?
O1S Pb1 P3 104.46(4) 2 . ?
O1S Pb1 P3 75.99(4) . . ?
P1 Pb1 P3 139.627(16) 2 . ?
P1 Pb1 P3 43.022(15) . . ?
O1S Pb1 P3 75.98(4) 2 2 ?
O1S Pb1 P3 104.45(4) . 2 ?
P1 Pb1 P3 43.023(15) 2 2 ?
P1 Pb1 P3 139.628(16) . 2 ?
P3 Pb1 P3 177.25(2) . 2 ?
P2 P1 P3 59.37(3) . . ?
P2 P1 Nb1 63.72(2) . . ?
P3 P1 Nb1 62.28(2) . . ?
P2 P1 Pb1 91.77(2) . . ?
P3 P1 Pb1 75.60(2) . . ?
Nb1 P1 Pb1 137.63(2) . . ?
P3 P2 P1 60.89(3) . . ?
P3 P2 Nb1 63.46(2) . . ?
P1 P2 Nb1 65.82(2) . . ?
P2 P3 P1 59.73(3) . . ?
P2 P3 Nb1 65.38(2) . . ?
P1 P3 Nb1 66.22(2) . . ?
P2 P3 Pb1 84.37(2) . . ?
P1 P3 Pb1 61.377(19) . . ?
Nb1 P3 Pb1 127.40(2) . . ?
C11 O1 Nb1 164.60(13) . . ?
C21 O2 Nb1 136.71(13) . . ?
C31 O3 Nb1 147.68(13) . . ?
O1 C11 C16 119.30(18) . . ?
O1 C11 C12 117.31(18) . . ?
C16 C11 C12 123.38(19) . . ?
C13 C12 C11 116.7(2) . . ?
C13 C12 C121 123.3(2) . . ?
C11 C12 C121 120.03(18) . . ?
C12 C121 C122 113.74(19) . . ?
C12 C121 C123 110.81(18) . . ?
C122 C121 C123 110.3(2) . . ?
C14 C13 C12 121.4(2) . . ?
C15 C14 C13 120.2(2) . . ?
C14 C15 C16 121.2(2) . . ?
C15 C16 C11 117.1(2) . . ?
C15 C16 C161 121.9(2) . . ?
C11 C16 C161 120.96(19) . . ?
C16 C161 C162 110.6(2) . . ?
C16 C161 C163 113.5(2) . . ?
C162 C161 C163 111.2(2) . . ?
O2 C21 C26 118.7(2) . . ?
O2 C21 C22 118.9(2) . . ?
C26 C21 C22 122.3(2) . . ?
C23 C22 C21 116.6(3) . . ?
C23 C22 C221 121.9(3) . . ?
C21 C22 C221 121.4(2) . . ?
C22 C221 C222 109.9(2) . . ?
C22 C221 C223 114.0(3) . . ?
C222 C221 C223 109.9(2) . . ?
C24 C23 C22 122.0(3) . . ?
C25 C24 C23 120.0(3) . . ?
C24 C25 C26 121.4(3) . . ?
C25 C26 C21 117.5(3) . . ?
C25 C26 C261 120.6(3) . . ?
C21 C26 C261 121.9(2) . . ?
C26 C261 C262 111.3(2) . . ?
C26 C261 C263 113.8(2) . . ?
C262 C261 C263 109.9(2) . . ?
O3 C31 C32 118.4(2) . . ?
O3 C31 C36 119.33(19) . . ?
C32 C31 C36 122.2(2) . . ?
C31 C32 C33 117.2(3) . . ?
C31 C32 C321 121.6(2) . . ?
C33 C32 C321 121.2(2) . . ?
C32 C321 C323 111.9(2) . . ?
C32 C321 C322 112.3(3) . . ?
C323 C321 C322 110.6(3) . . ?
C34 C33 C32 121.3(3) . . ?
C35 C34 C33 120.6(2) . . ?
C34 C35 C36 121.2(3) . . ?
C35 C36 C31 117.5(2) . . ?
C35 C36 C361 119.6(2) . . ?
C31 C36 C361 122.85(19) . . ?
C36 C361 C363 110.7(2) . . ?
C36 C361 C362 112.4(2) . . ?
C363 C361 C362 110.8(2) . . ?
C1SA O1S C4SA 113.8(5) . . ?
C1SA O1S C1SB 10.6(16) . . ?
C4SA O1S C1SB 103.6(14) . . ?
C1SA O1S C4SB 105.5(12) . . ?
C4SA O1S C4SB 12.4(10) . . ?
C1SB O1S C4SB 95.0(18) . . ?
C1SA O1S Pb1 123.3(4) . . ?
C4SA O1S Pb1 120.1(4) . . ?
C1SB O1S Pb1 131.7(16) . . ?
C4SB O1S Pb1 124.0(13) . . ?
O1S C1SA C2SA 105.6(8) . . ?
C3SA C2SA C1SA 104.2(6) . . ?
C2SA C3SA C4SA 102.5(7) . . ?
O1S C4SA C3SA 100.3(6) . . ?
C2SB C1SB O1S 107(3) . . ?
C3SB C2SB C1SB 101(2) . . ?
C4SB C3SB C2SB 114(3) . . ?
C3SB C4SB O1S 120(3) . . ?
C6T C1T C2T 119.8(4) . . ?
C3T C2T C1T 119.7(4) . . ?
C4T C3T C2T 120.9(4) . . ?
C3T C4T C5T 120.0(4) . . ?
C4T C5T C6T 120.0(4) . . ?
C1T C6T C5T 119.5(4) . . ?
C2U C1U C6U 118(2) . . ?
C1U C2U C3U 118(3) . . ?
C2U C3U C4U 123(2) . . ?
C5U C4U C3U 120(2) . . ?
C6U C5U C4U 119(3) . . ?
C5U C6U C1U 121.1(16) . . ?
C6V C1V C2V 120.0 . . ?
C3V C2V C1V 120.0 . . ?
C2V C3V C4V 120.0 . . ?
C5V C4V C3V 120.0 . . ?
C4V C5V C6V 120.0 . . ?
C1V C6V C5V 120.0 . . ?
C3W C2W C1W 116(2) . . ?
C2W C3W C4W 116.2(19) . . ?
C3W C4W C5W 115(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        29.57
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.089
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.072
