# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_fo4322
_audit_creation_date             2013-05-12
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C30 H34 N O10 V, 2(C H4 O)'
_chemical_formula_sum            'C32 H42 N O12 V'
_chemical_formula_weight         683.60
_chemical_absolute_configuration syn
_chemical_melting_point          ?
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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.54420(10)
_cell_length_b                   25.1111(4)
_cell_length_c                   27.5039(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6591.73(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            40163
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         1.783
_diffrn_ambient_temperature      133.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                14245
_reflns_number_total             15122
_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.
;
_reflns_threshold_expression     'I > 2\s(I)'
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 
;
 Flack x determined using 5987 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.018(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         15122
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0407
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+5.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0968
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Shared sites
{C152, C153}
{H203, H202}
2. Others
 Fixed Sof: H14A(0.5) H14B(0.5) H14C(0.5) H14D(0.5) C152(0.5) C162(0.5)
 H162(0.5) C172(0.5) H172(0.5) C182(0.5) H182(0.5) C192(0.5) H192(0.5)
 C202(0.5) H202(0.5) C153(0.5) C163(0.5) H163(0.5) C173(0.5) H173(0.5)
 C183(0.5) H183(0.5) C193(0.5) H193(0.5) C203(0.5) H203(0.5) O3M(0.5) H3M(0.5)
 C3M(0.5) H3MA(0.5) H3MB(0.5) H3MC(0.5) O3MA(0.5) H3MD(0.5) C3MA(0.5) H3ME(0.5)
 H3MF(0.5) H3MG(0.5) O4M(0.5) H4M(0.5) C4M(0.5) H4MA(0.5) H4MB(0.5) H4MC(0.5)
 O4MA(0.5) H4MD(0.5) C4MA(0.5) H4ME(0.5) H4MF(0.5) H4MG(0.5)
 Fixed Uiso: H11(0.023) H21(0.022) H31(0.02) H41(0.021) H51(0.022) H61A(0.028)
 H61B(0.028) H71(0.025) H91(0.035) H101(0.038) H111(0.039) H14E(0.042)
 H14F(0.042) H161(0.059) H171(0.084) H181(0.07) H191(0.06) H201(0.047)
 H211(0.024) H231(0.034) H241(0.044) H251(0.043) H261(0.044) H271(0.038)
 H28D(0.1) H28E(0.1) H28F(0.1) H29D(0.063) H29E(0.063) H29F(0.063) H12(0.023)
 H22(0.022) H32(0.021) H42(0.022) H52(0.023) H62A(0.029) H62B(0.029) H72(0.026)
 H92(0.036) H102(0.043) H112(0.04) H14A(0.029) H14B(0.029) H14C(0.029)
 H14D(0.029) H162(0.048) H172(0.047) H182(0.037) H192(0.029) H202(0.02)
 H163(0.025) H173(0.034) H183(0.034) H193(0.034) H203(0.048) H212(0.026)
 H232(0.038) H242(0.045) H252(0.047) H262(0.047) H272(0.04) H28A(0.07)
 H28B(0.07) H28C(0.07) H29A(0.065) H29B(0.065) H29C(0.065) H1M1(0.029)
 H1MD(0.091) H1ME(0.091) H1MF(0.091) H1M2(0.031) H1MA(0.082) H1MB(0.082)
 H1MC(0.082) H1M(0.113) H1MG(0.062) H1MH(0.062) H1MI(0.062) H2M(0.07)
 H2MA(0.067) H2MB(0.067) H2MC(0.067) H3M(0.066) H3MA(0.088) H3MB(0.088)
 H3MC(0.088) H3MD(0.139) H3ME(0.106) H3MF(0.106) H3MG(0.106) H4M(0.075)
 H4MA(0.096) H4MB(0.096) H4MC(0.096) H4MD(0.081) H4ME(0.093) H4MF(0.093)
 H4MG(0.093)
 Fixed X: H11(-0.0475) H21(0.0273) H31(0.2756) H41(0.0378) H51(0.118) H61A(-
 0.1171) H61B(-0.0786) H71(0.1233) H91(0.2436) H101(0.3923) H111(0.5142) H14E(-
 0.0328) H14F(0.0137) H161(0.18) H171(0.3238) H181(0.3779) H191(0.2982)
 H201(0.1521) H211(0.0361) H231(0.3618) H241(0.4891) H251(0.3994) H261(0.1845)
 H271(0.064) H28D(0.5574) H28E(0.603) H28F(0.5728) H29D(0.6435) H29E(0.5616)
 H29F(0.68) H12(0.3841) H22(0.3245) H32(0.0656) H42(0.3145) H52(0.2047)
 H62A(0.4506) H62B(0.3909) H72(0.2067) H92(0.067) H102(-0.0886) H112(-0.1804)
 H14A(0.3619) H14B(0.277) H14C(0.3574) H14D(0.2871) H162(0.108) H172(-0.0409)
 H182(-0.057) H192(0.0484) H202(0.1906) H163(0.128) H173(-0.0119) H183(-0.0735)
 H193(0.0231) H203(0.1818) H212(0.3133) H232(-0.0483) H242(-0.1691) H252(-
 0.0458) H262(0.1964) H272(0.3179) H28A(-0.1651) H28B(-0.2137) H28C(-0.1342)
 H29A(-0.2808) H29B(-0.2293) H29C(-0.3279) H1M1(0.086) H1MD(-0.0411)
 H1ME(0.0791) H1MF(0.0969) H1M2(0.2805) H1MA(0.4318) H1MB(0.3164) H1MC(0.3068)
 H1M(0.3098) H1MG(0.1194) H1MH(0.2098) H1MI(0.1954) H2M(0.0898) H2MA(-0.0243)
 H2MB(-0.0507) H2MC(-0.1184) H3M(0.3809) H3MA(0.4669) H3MB(0.3132) H3MC(0.3464)
 H3MD(0.4358) H3ME(0.4629) H3MF(0.4033) H3MG(0.3205) H4M(0.2207) H4MA(0.1651)
 H4MB(0.1083) H4MC(0.2498) H4MD(0.2226) H4ME(0.1583) H4MF(0.1573) H4MG(0.2887)
 Fixed Y: H11(0.1704) H21(0.1443) H31(0.2087) H41(0.2223) H51(0.2829)
 H61A(0.3009) H61B(0.3365) H71(0.1122) H91(0.066) H101(-0.0012) H111(-0.0534)
 H14E(0.2237) H14F(0.2775) H161(0.3328) H171(0.3541) H181(0.289) H191(0.2036)
 H201(0.1824) H211(0.2995) H231(0.301) H241(0.36) H251(0.444) H261(0.4702)
 H271(0.4134) H28D(0.0246) H28E(0.0652) H28F(0.0868) H29D(-0.1025) H29E(-
 0.1106) H29F(-0.0658) H12(-0.1789) H22(-0.1491) H32(-0.2078) H42(-0.2262) H52(-
 0.2853) H62A(-0.3103) H62B(-0.3453) H72(-0.1184) H92(-0.0759) H102(-0.0095)
 H112(0.0498) H14A(-0.2431) H14B(-0.2909) H14C(-0.241) H14D(-0.2896) H162(-
 0.3347) H172(-0.3393) H182(-0.2644) H192(-0.1857) H202(-0.1814) H163(-0.3405)
 H173(-0.3537) H183(-0.2848) H193(-0.2015) H203(-0.1893) H212(-0.3012) H232(-
 0.3338) H242(-0.391) H252(-0.442) H262(-0.4349) H272(-0.3765) H28A(-0.0285)
 H28B(-0.0789) H28C(-0.0875) H29A(0.1022) H29B(0.1079) H29C(0.0592)
 H1M1(0.0336) H1MD(0.0651) H1ME(0.0287) H1MF(0.0921) H1M2(-0.0319) H1MA(-
 0.0649) H1MB(-0.0331) H1MC(-0.0965) H1M(0.1666) H1MG(0.1761) H1MH(0.1976)
 H1MI(0.2328) H2M(-0.1695) H2MA(-0.2378) H2MB(-0.199) H2MC(-0.1856) H3M(0.1208)
 H3MA(0.0249) H3MB(0.0386) H3MC(0.042) H3MD(0.1309) H3ME(0.0273) H3MF(0.0535)
 H3MG(0.0609) H4M(-0.1283) H4MA(-0.0426) H4MB(-0.072) H4MC(-0.0379) H4MD(-
 0.1342) H4ME(-0.0584) H4MF(-0.0938) H4MG(-0.0564)
 Fixed Z: H11(1.0281) H21(0.9519) H31(0.9601) H41(0.8967) H51(0.9818)
 H61A(0.9187) H61B(0.9654) H71(1.0555) H91(1.1217) H101(1.1483) H111(1.0929)
 H14E(1.0958) H14F(1.0687) H161(1.1048) H171(1.1715) H181(1.228) H191(1.2184)
 H201(1.1535) H211(0.8515) H231(0.8267) H241(0.7779) H251(0.7597) H261(0.7928)
 H271(0.8449) H28D(0.8512) H28E(0.8932) H28F(0.8394) H29D(0.9826) H29E(1.0328)
 H29F(1.0284) H12(1.0322) H22(0.9557) H32(0.9561) H42(0.8991) H52(0.9809)
 H62A(0.9245) H62B(0.9688) H72(1.058) H92(1.1212) H102(1.1453) H112(1.0888)
 H14A(1.0923) H14B(1.0669) H14C(1.0946) H14D(1.0656) H162(1.1148) H172(1.1843)
 H182(1.2333) H192(1.2124) H202(1.1449) H163(1.1101) H173(1.1776) H183(1.228)
 H193(1.2163) H203(1.1523) H212(0.8527) H232(0.8619) H242(0.8094) H252(0.7531)
 H262(0.7474) H272(0.7989) H28A(0.837) H28B(0.8683) H28C(0.8177) H29A(0.9754)
 H29B(1.0305) H29C(1.0151) H1M1(0.9234) H1MD(0.866) H1ME(0.8427) H1MF(0.8439)
 H1M2(0.9284) H1MA(0.8793) H1MB(0.8487) H1MC(0.8535) H1M(0.8386) H1MG(0.7991)
 H1MH(0.7541) H1MI(0.8023) H2M(0.8365) H2MA(0.8036) H2MB(0.7583) H2MC(0.8101)
 H3M(0.7561) H3MA(0.7365) H3MB(0.7169) H3MC(0.7738) H3MD(0.761) H3ME(0.7655)
 H3MF(0.7166) H3MG(0.7668) H4M(0.7742) H4MA(0.7751) H4MB(0.7274) H4MC(0.7251)
 H4MD(0.7765) H4ME(0.7533) H4MF(0.705) H4MG(0.7168)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
V1 V 0.33298(5) 0.09463(2) 0.93151(2) 0.01940(11) Uani 1 1 d . . . . .
O11 O 0.4664(3) 0.11941(9) 0.95778(9) 0.0272(5) Uani 1 1 d . . . . .
O21 O 0.3336(3) 0.02882(9) 0.96660(8) 0.0223(5) Uani 1 1 d . . . . .
O31 O 0.2523(2) 0.15686(8) 0.90594(8) 0.0210(5) Uani 1 1 d . . . . .
O41 O 0.4024(3) 0.06863(10) 0.87638(9) 0.0291(5) Uani 1 1 d . . . . .
O51 O 0.1180(2) 0.21272(9) 1.04589(8) 0.0192(4) Uani 1 1 d . . . . .
O61 O 0.1980(2) 0.27333(8) 0.89079(8) 0.0182(4) Uani 1 1 d . . . . .
O71 O -0.0492(2) 0.23511(9) 0.98680(8) 0.0206(4) Uani 1 1 d . . . . .
O81 O 0.0541(3) 0.34596(9) 0.90965(8) 0.0236(5) Uani 1 1 d . . . . .
O91 O 0.5018(3) -0.04691(10) 0.99592(10) 0.0345(6) Uani 1 1 d . . . . .
N1 N 0.1907(3) 0.11675(10) 0.98945(10) 0.0179(5) Uani 1 1 d . . . . .
C11 C 0.0228(3) 0.19356(13) 1.01131(11) 0.0192(6) Uani 1 1 d . . . . .
H11 H -0.0475 0.1704 1.0281 0.023 Uiso 1 1 calc R U . . .
C21 C 0.1003(3) 0.16039(12) 0.97344(11) 0.0185(6) Uani 1 1 d . . . . .
H21 H 0.0273 0.1443 0.9519 0.022 Uiso 1 1 calc R U . . .
C31 C 0.1974(3) 0.19334(12) 0.94041(11) 0.0169(6) Uani 1 1 d . . . . .
H31 H 0.2756 0.2087 0.9601 0.020 Uiso 1 1 calc R U . . .
C41 C 0.1120(3) 0.23768(12) 0.91822(11) 0.0176(6) Uani 1 1 d . . . . .
H41 H 0.0378 0.2223 0.8967 0.021 Uiso 1 1 calc R U . . .
C51 C 0.0436(3) 0.26875(12) 0.95971(11) 0.0185(6) Uani 1 1 d . . . . .
H51 H 0.1180 0.2829 0.9818 0.022 Uiso 1 1 calc R U . . .
C61 C -0.0389(3) 0.31453(13) 0.93884(12) 0.0231(6) Uani 1 1 d . . . . .
H61A H -0.1171 0.3009 0.9187 0.028 Uiso 1 1 calc R U . . .
H61B H -0.0786 0.3365 0.9654 0.028 Uiso 1 1 calc R U . . .
C71 C 0.1877(3) 0.09760(13) 1.03278(11) 0.0207(6) Uani 1 1 d . . . . .
H71 H 0.1233 0.1122 1.0555 0.025 Uiso 1 1 calc R U . . .
C81 C 0.2785(4) 0.05475(13) 1.04836(12) 0.0215(6) Uani 1 1 d . . . . .
C91 C 0.2936(4) 0.04504(14) 1.09878(13) 0.0294(8) Uani 1 1 d . . . . .
H91 H 0.2436 0.0660 1.1217 0.035 Uiso 1 1 calc R U . . .
C101 C 0.3813(4) 0.00503(14) 1.11443(14) 0.0321(8) Uani 1 1 d . . . . .
H101 H 0.3923 -0.0012 1.1483 0.038 Uiso 1 1 calc R U . . .
C111 C 0.4534(4) -0.02621(14) 1.08145(14) 0.0327(8) Uani 1 1 d . . . . .
H111 H 0.5142 -0.0534 1.0929 0.039 Uiso 1 1 calc R U . . .
C121 C 0.4379(4) -0.01830(14) 1.03163(13) 0.0257(7) Uani 1 1 d . . . . .
C131 C 0.3495(3) 0.02299(12) 1.01471(12) 0.0213(6) Uani 1 1 d . . . . .
C141 C 0.0486(4) 0.24378(17) 1.08296(13) 0.0352(9) Uani 1 1 d . . . . .
H14E H -0.0328 0.2237 1.0958 0.042 Uiso 1 1 calc R U . . .
H14F H 0.0137 0.2775 1.0687 0.042 Uiso 1 1 calc R U . . .
C151 C 0.1478(3) 0.25571(14) 1.12321(12) 0.0253(7) Uani 1 1 d . . . . .
C161 C 0.2016(5) 0.30630(18) 1.12825(19) 0.0492(11) Uani 1 1 d . . . . .
H161 H 0.1800 0.3328 1.1048 0.059 Uiso 1 1 calc R U . . .
C171 C 0.2882(6) 0.3190(2) 1.1678(2) 0.0700(18) Uani 1 1 d . . . . .
H171 H 0.3238 0.3541 1.1715 0.084 Uiso 1 1 calc R U . . .
C181 C 0.3206(5) 0.2804(3) 1.20084(18) 0.0586(15) Uani 1 1 d . . . . .
H181 H 0.3779 0.2890 1.2280 0.070 Uiso 1 1 calc R U . . .
C191 C 0.2726(4) 0.2303(2) 1.19558(15) 0.0499(13) Uani 1 1 d . . . . .
H191 H 0.2982 0.2036 1.2184 0.060 Uiso 1 1 calc R U . . .
C201 C 0.1859(4) 0.21776(19) 1.15690(15) 0.0395(9) Uani 1 1 d . . . . .
H201 H 0.1521 0.1824 1.1535 0.047 Uiso 1 1 calc R U . . .
C211 C 0.1129(3) 0.31513(12) 0.87173(11) 0.0203(6) Uani 1 1 d . . . . .
H211 H 0.0361 0.2995 0.8515 0.024 Uiso 1 1 calc R U . . .
C221 C 0.2011(4) 0.35176(13) 0.84078(12) 0.0215(6) Uani 1 1 d . . . . .
C231 C 0.3265(4) 0.33575(14) 0.82051(13) 0.0287(7) Uani 1 1 d . . . . .
H231 H 0.3618 0.3010 0.8267 0.034 Uiso 1 1 calc R U . . .
C241 C 0.4012(4) 0.37067(17) 0.79096(14) 0.0367(9) Uani 1 1 d . . . . .
H241 H 0.4891 0.3600 0.7779 0.044 Uiso 1 1 calc R U . . .
C251 C 0.3488(5) 0.42056(15) 0.78040(14) 0.0362(9) Uani 1 1 d . . . . .
H251 H 0.3994 0.4440 0.7597 0.043 Uiso 1 1 calc R U . . .
C261 C 0.2219(5) 0.43614(15) 0.80022(15) 0.0370(9) Uani 1 1 d . . . . .
H261 H 0.1845 0.4702 0.7928 0.044 Uiso 1 1 calc R U . . .
C271 C 0.1497(4) 0.40214(15) 0.83072(13) 0.0314(8) Uani 1 1 d . . . . .
H271 H 0.0640 0.4134 0.8449 0.038 Uiso 1 1 calc R U . . .
C281 C 0.5449(5) 0.0607(2) 0.8641(2) 0.0669(17) Uani 1 1 d . . . . .
H28D H 0.5574 0.0246 0.8512 0.100 Uiso 1 1 calc R U . . .
H28E H 0.6030 0.0652 0.8932 0.100 Uiso 1 1 calc R U . . .
H28F H 0.5728 0.0868 0.8394 0.100 Uiso 1 1 calc R U . . .
C291 C 0.6047(4) -0.08436(16) 1.01111(18) 0.0418(10) Uani 1 1 d . . . . .
H29D H 0.6435 -0.1025 0.9826 0.063 Uiso 1 1 calc R U . . .
H29E H 0.5616 -0.1106 1.0328 0.063 Uiso 1 1 calc R U . . .
H29F H 0.6800 -0.0658 1.0284 0.063 Uiso 1 1 calc R U . . .
V2 V 0.03555(5) -0.09163(2) 0.92869(2) 0.01905(11) Uani 1 1 d . . . . .
O12 O -0.1097(3) -0.11431(9) 0.94916(9) 0.0264(5) Uani 1 1 d . . . . .
O22 O 0.0358(2) -0.02737(8) 0.96600(8) 0.0214(5) Uani 1 1 d . . . . .
O32 O 0.1120(2) -0.15563(8) 0.90420(8) 0.0205(5) Uani 1 1 d . . . . .
O42 O -0.0113(3) -0.06473(9) 0.87122(9) 0.0265(5) Uani 1 1 d . . . . .
O52 O 0.2101(2) -0.21802(9) 1.04677(8) 0.0194(4) Uani 1 1 d . . . . .
O62 O 0.1467(2) -0.27282(9) 0.88784(8) 0.0197(4) Uani 1 1 d . . . . .
O72 O 0.3809(2) -0.24279(9) 0.98976(8) 0.0206(5) Uani 1 1 d . . . . .
O82 O 0.2725(3) -0.34914(9) 0.90853(8) 0.0233(5) Uani 1 1 d . . . . .
O92 O -0.1308(3) 0.05140(10) 0.99355(10) 0.0341(6) Uani 1 1 d . . . . .
N2 N 0.1579(3) -0.11954(10) 0.99018(10) 0.0187(5) Uani 1 1 d . . . . .
C12 C 0.3126(3) -0.20009(12) 1.01395(11) 0.0192(6) Uani 1 1 d . . . . .
H12 H 0.3841 -0.1789 1.0322 0.023 Uiso 1 1 calc R U . . .
C22 C 0.2457(3) -0.16445(12) 0.97516(11) 0.0180(6) Uani 1 1 d . . . . .
H22 H 0.3245 -0.1491 0.9557 0.022 Uiso 1 1 calc R U . . .
C32 C 0.1508(3) -0.19411(11) 0.93901(11) 0.0179(6) Uani 1 1 d . . . . .
H32 H 0.0656 -0.2078 0.9561 0.021 Uiso 1 1 calc R U . . .
C42 C 0.2332(3) -0.23999(12) 0.91821(11) 0.0183(6) Uani 1 1 d . . . . .
H42 H 0.3145 -0.2262 0.8991 0.022 Uiso 1 1 calc R U . . .
C52 C 0.2858(3) -0.27343(12) 0.96061(11) 0.0188(6) Uani 1 1 d . . . . .
H52 H 0.2047 -0.2853 0.9809 0.023 Uiso 1 1 calc R U . . .
C62 C 0.3642(4) -0.32161(13) 0.94159(12) 0.0239(7) Uani 1 1 d . . . . .
H62A H 0.4506 -0.3103 0.9245 0.029 Uiso 1 1 calc R U . . .
H62B H 0.3909 -0.3453 0.9688 0.029 Uiso 1 1 calc R U . . .
C72 C 0.1501(3) -0.10209(12) 1.03383(12) 0.0213(6) Uani 1 1 d . . . . .
H72 H 0.2067 -0.1184 1.0580 0.026 Uiso 1 1 calc R U . . .
C82 C 0.0590(3) -0.05865(13) 1.04813(12) 0.0226(6) Uani 1 1 d . . . . .
C92 C 0.0268(4) -0.05267(14) 1.09773(13) 0.0296(8) Uani 1 1 d . . . . .
H92 H 0.0670 -0.0759 1.1212 0.036 Uiso 1 1 calc R U . . .
C102 C -0.0639(5) -0.01280(16) 1.11203(14) 0.0357(9) Uani 1 1 d . . . . .
H102 H -0.0886 -0.0095 1.1453 0.043 Uiso 1 1 calc R U . . .
C112 C -0.1190(4) 0.02229(15) 1.07837(14) 0.0336(8) Uani 1 1 d . . . . .
H112 H -0.1804 0.0498 1.0888 0.040 Uiso 1 1 calc R U . . .
C122 C -0.0852(3) 0.01774(14) 1.02936(13) 0.0255(7) Uani 1 1 d . . . . .
C132 C 0.0040(3) -0.02364(13) 1.01349(12) 0.0219(7) Uani 1 1 d . . . . .
C142 C 0.2679(4) -0.25508(13) 1.08168(12) 0.0238(7) Uani 1 1 d . . . . .
H14A H 0.3619 -0.2431 1.0923 0.029 Uiso 0.5 1 calc R U P A 1
H14B H 0.2770 -0.2909 1.0669 0.029 Uiso 0.5 1 calc R U P A 1
H14C H 0.3574 -0.2410 1.0946 0.029 Uiso 0.5 1 calc R U P B 2
H14D H 0.2871 -0.2896 1.0656 0.029 Uiso 0.5 1 calc R U P B 2
C152 C 0.1700(16) -0.2570(5) 1.1241(5) 0.026(5) Uiso 0.5 1 d D . P C 1
C162 C 0.0973(15) -0.3045(5) 1.1352(5) 0.040(5) Uiso 0.5 1 d D . P C 1
H162 H 0.1080 -0.3347 1.1148 0.048 Uiso 0.5 1 calc R U P C 1
C172 C 0.0086(12) -0.3076(5) 1.1765(4) 0.039(3) Uiso 0.5 1 d D . P C 1
H172 H -0.0409 -0.3393 1.1843 0.047 Uiso 0.5 1 calc R U P C 1
C182 C -0.0022(10) -0.2629(4) 1.2045(3) 0.031(2) Uiso 0.5 1 d D . P C 1
H182 H -0.0570 -0.2644 1.2333 0.037 Uiso 0.5 1 calc R U P C 1
C192 C 0.0621(9) -0.2165(4) 1.1928(3) 0.024(2) Uiso 0.5 1 d D . P C 1
H192 H 0.0484 -0.1857 1.2124 0.029 Uiso 0.5 1 calc R U P C 1
C202 C 0.1467(10) -0.2142(4) 1.1528(3) 0.017(2) Uiso 0.5 1 d D . P C 1
H202 H 0.1906 -0.1814 1.1449 0.020 Uiso 0.5 1 calc R U P C 1
C153 C 0.1663(14) -0.2632(5) 1.1227(4) 0.017(4) Uiso 0.5 1 d D . P C 2
C163 C 0.1092(11) -0.3116(4) 1.1315(4) 0.020(3) Uiso 0.5 1 d D . P C 2
H163 H 0.1280 -0.3405 1.1101 0.025 Uiso 0.5 1 calc R U P C 2
C173 C 0.0241(10) -0.3191(4) 1.1713(3) 0.028(2) Uiso 0.5 1 d D . P C 2
H173 H -0.0119 -0.3537 1.1776 0.034 Uiso 0.5 1 calc R U P C 2
C183 C -0.0103(9) -0.2787(4) 1.2019(3) 0.028(2) Uiso 0.5 1 d D . P C 2
H183 H -0.0735 -0.2848 1.2280 0.034 Uiso 0.5 1 calc R U P C 2
C193 C 0.0455(10) -0.2301(4) 1.1952(3) 0.028(2) Uiso 0.5 1 d D . P C 2
H193 H 0.0231 -0.2015 1.2163 0.034 Uiso 0.5 1 calc R U P C 2
C203 C 0.1374(14) -0.2229(5) 1.1561(4) 0.040(4) Uiso 0.5 1 d D . P C 2
H203 H 0.1818 -0.1893 1.1523 0.048 Uiso 0.5 1 calc R U P C 2
C212 C 0.2291(4) -0.31561(12) 0.86998(11) 0.0214(6) Uani 1 1 d . . . . .
H212 H 0.3133 -0.3012 0.8527 0.026 Uiso 1 1 calc R U . . .
C222 C 0.1454(4) -0.34983(13) 0.83568(12) 0.0245(7) Uani 1 1 d . . . . .
C232 C 0.0019(4) -0.35416(15) 0.83858(14) 0.0314(8) Uani 1 1 d . . . . .
H232 H -0.0483 -0.3338 0.8619 0.038 Uiso 1 1 calc R U . . .
C242 C -0.0699(5) -0.38833(15) 0.80751(15) 0.0373(9) Uani 1 1 d . . . . .
H242 H -0.1691 -0.3910 0.8094 0.045 Uiso 1 1 calc R U . . .
C252 C 0.0033(5) -0.41832(15) 0.77401(14) 0.0391(10) Uani 1 1 d . . . . .
H252 H -0.0458 -0.4420 0.7531 0.047 Uiso 1 1 calc R U . . .
C262 C 0.1467(5) -0.41423(15) 0.77064(14) 0.0393(10) Uani 1 1 d . . . . .
H262 H 0.1964 -0.4349 0.7474 0.047 Uiso 1 1 calc R U . . .
C272 C 0.2190(5) -0.37969(14) 0.80135(14) 0.0337(8) Uani 1 1 d . . . . .
H272 H 0.3179 -0.3765 0.7989 0.040 Uiso 1 1 calc R U . . .
C282 C -0.1409(5) -0.06492(18) 0.84672(17) 0.0469(11) Uani 1 1 d . . . . .
H28A H -0.1651 -0.0285 0.8370 0.070 Uiso 1 1 calc R U . . .
H28B H -0.2137 -0.0789 0.8683 0.070 Uiso 1 1 calc R U . . .
H28C H -0.1342 -0.0875 0.8177 0.070 Uiso 1 1 calc R U . . .
C292 C -0.2517(4) 0.08264(16) 1.00449(19) 0.0433(11) Uani 1 1 d . . . . .
H29A H -0.2808 0.1022 0.9754 0.065 Uiso 1 1 calc R U . . .
H29B H -0.2293 0.1079 1.0305 0.065 Uiso 1 1 calc R U . . .
H29C H -0.3279 0.0592 1.0151 0.065 Uiso 1 1 calc R U . . .
O1M1 O 0.1254(3) 0.05737(9) 0.90681(8) 0.0245(5) Uani 1 1 d . . . . .
H1M1 H 0.0860 0.0336 0.9234 0.029 Uiso 1 1 calc R U . . .
C1M1 C 0.0602(6) 0.06108(19) 0.86146(17) 0.0604(16) Uani 1 1 d . . . . .
H1MD H -0.0411 0.0651 0.8660 0.091 Uiso 1 1 calc R U . . .
H1ME H 0.0791 0.0287 0.8427 0.091 Uiso 1 1 calc R U . . .
H1MF H 0.0969 0.0921 0.8439 0.091 Uiso 1 1 calc R U . . .
O1M2 O 0.2511(3) -0.05788(9) 0.91209(9) 0.0255(5) Uani 1 1 d . . . . .
H1M2 H 0.2805 -0.0319 0.9284 0.031 Uiso 1 1 calc R U . . .
C1M2 C 0.3326(6) -0.0635(2) 0.87030(18) 0.0545(13) Uani 1 1 d . . . . .
H1MA H 0.4318 -0.0649 0.8793 0.082 Uiso 1 1 calc R U . . .
H1MB H 0.3164 -0.0331 0.8487 0.082 Uiso 1 1 calc R U . . .
H1MC H 0.3068 -0.0965 0.8535 0.082 Uiso 1 1 calc R U . . .
O1M O 0.3216(5) 0.17217(18) 0.80878(13) 0.0755(14) Uani 1 1 d . . . . .
H1M H 0.3098 0.1666 0.8386 0.113 Uiso 1 1 calc R U . . .
C1M C 0.2028(5) 0.19647(18) 0.78968(15) 0.0414(10) Uani 1 1 d . . . . .
H1MG H 0.1194 0.1761 0.7991 0.062 Uiso 1 1 calc R U . . .
H1MH H 0.2098 0.1976 0.7541 0.062 Uiso 1 1 calc R U . . .
H1MI H 0.1954 0.2328 0.8023 0.062 Uiso 1 1 calc R U . . .
O2M O 0.0833(3) -0.17137(14) 0.80612(10) 0.0469(8) Uani 1 1 d . . . . .
H2M H 0.0898 -0.1695 0.8365 0.070 Uiso 1 1 calc R U . . .
C2M C -0.0365(5) -0.2007(2) 0.79360(15) 0.0449(10) Uani 1 1 d . . . . .
H2MA H -0.0243 -0.2378 0.8036 0.067 Uiso 1 1 calc R U . . .
H2MB H -0.0507 -0.1990 0.7583 0.067 Uiso 1 1 calc R U . . .
H2MC H -0.1184 -0.1856 0.8101 0.067 Uiso 1 1 calc R U . . .
O3M O 0.4241(7) 0.1022(2) 0.7356(2) 0.0439(14) Uiso 0.5 1 d D . P D 1
H3M H 0.3809 0.1208 0.7561 0.066 Uiso 0.5 1 calc R U P D 1
C3M C 0.3845(15) 0.0476(5) 0.7411(5) 0.058(3) Uiso 0.5 1 d D . P D 1
H3MA H 0.4669 0.0249 0.7365 0.088 Uiso 0.5 1 calc R U P D 1
H3MB H 0.3132 0.0386 0.7169 0.088 Uiso 0.5 1 calc R U P D 1
H3MC H 0.3464 0.0420 0.7738 0.088 Uiso 0.5 1 calc R U P D 1
O3MA O 0.4899(11) 0.1045(4) 0.7614(4) 0.093(3) Uiso 0.5 1 d D . P E 2
H3MD H 0.4358 0.1309 0.7610 0.139 Uiso 0.5 1 calc R U P E 2
C3MA C 0.4134(16) 0.0581(6) 0.7519(6) 0.071(4) Uiso 0.5 1 d D . P E 2
H3ME H 0.4629 0.0273 0.7655 0.106 Uiso 0.5 1 calc R U P E 2
H3MF H 0.4033 0.0535 0.7166 0.106 Uiso 0.5 1 calc R U P E 2
H3MG H 0.3205 0.0609 0.7668 0.106 Uiso 0.5 1 calc R U P E 2
O4M O 0.2710(10) -0.1074(4) 0.7578(3) 0.050(3) Uiso 0.5 1 d D . P F 1
H4M H 0.2207 -0.1283 0.7742 0.075 Uiso 0.5 1 calc R U P F 1
C4M C 0.1925(14) -0.0614(5) 0.7454(5) 0.064(3) Uiso 0.5 1 d D . P F 1
H4MA H 0.1651 -0.0426 0.7751 0.096 Uiso 0.5 1 calc R U P F 1
H4MB H 0.1083 -0.0720 0.7274 0.096 Uiso 0.5 1 calc R U P F 1
H4MC H 0.2498 -0.0379 0.7251 0.096 Uiso 0.5 1 calc R U P F 1
O4MA O 0.2800(11) -0.1213(4) 0.7565(4) 0.054(3) Uiso 0.5 1 d D . P G 2
H4MD H 0.2226 -0.1342 0.7765 0.081 Uiso 0.5 1 calc R U P G 2
C4MA C 0.2162(14) -0.0793(5) 0.7310(4) 0.062(3) Uiso 0.5 1 d D . P G 2
H4ME H 0.1583 -0.0584 0.7533 0.093 Uiso 0.5 1 calc R U P G 2
H4MF H 0.1573 -0.0938 0.7050 0.093 Uiso 0.5 1 calc R U P G 2
H4MG H 0.2887 -0.0564 0.7168 0.093 Uiso 0.5 1 calc R U P G 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0199(2) 0.0151(2) 0.0232(2) 0.0009(2) 0.0027(2) 0.0010(2)
O11 0.0217(12) 0.0238(12) 0.0360(13) 0.0005(10) 0.0014(10) -0.0007(10)
O21 0.0260(11) 0.0166(11) 0.0244(11) 0.0019(9) 0.0004(10) 0.0016(9)
O31 0.0280(12) 0.0135(10) 0.0215(11) 0.0006(9) 0.0040(9) 0.0036(9)
O41 0.0317(13) 0.0220(12) 0.0335(13) -0.0029(10) 0.0114(11) 0.0043(10)
O51 0.0138(10) 0.0236(11) 0.0202(10) -0.0030(9) -0.0009(8) 0.0014(9)
O61 0.0177(10) 0.0144(10) 0.0225(11) 0.0027(8) 0.0015(8) 0.0011(8)
O71 0.0138(10) 0.0248(11) 0.0233(11) 0.0031(9) 0.0012(9) 0.0011(9)
O81 0.0276(12) 0.0178(11) 0.0253(11) -0.0014(9) 0.0029(10) 0.0056(9)
O91 0.0308(13) 0.0283(13) 0.0442(16) 0.0057(12) 0.0007(12) 0.0099(11)
N1 0.0151(12) 0.0153(12) 0.0233(13) -0.0002(10) -0.0035(10) -0.0023(10)
C11 0.0139(14) 0.0218(15) 0.0219(15) 0.0013(12) -0.0010(12) -0.0009(12)
C21 0.0183(14) 0.0169(14) 0.0201(14) -0.0009(11) -0.0008(12) -0.0013(12)
C31 0.0156(13) 0.0156(14) 0.0196(14) -0.0013(11) 0.0020(11) -0.0008(11)
C41 0.0167(13) 0.0157(13) 0.0205(15) 0.0000(11) -0.0002(11) -0.0005(11)
C51 0.0167(14) 0.0192(14) 0.0196(14) 0.0000(12) 0.0006(12) 0.0021(12)
C61 0.0201(15) 0.0260(16) 0.0231(16) 0.0014(13) 0.0033(13) 0.0072(13)
C71 0.0203(14) 0.0179(14) 0.0239(15) -0.0014(13) 0.0004(12) -0.0036(13)
C81 0.0241(15) 0.0161(14) 0.0243(16) 0.0038(12) -0.0037(13) -0.0025(12)
C91 0.039(2) 0.0225(17) 0.0265(17) 0.0040(14) -0.0044(15) -0.0032(15)
C101 0.040(2) 0.0267(18) 0.0296(18) 0.0080(14) -0.0091(16) -0.0054(16)
C111 0.0322(18) 0.0237(17) 0.042(2) 0.0115(15) -0.0136(16) -0.0032(15)
C121 0.0206(16) 0.0214(16) 0.0351(18) 0.0052(14) -0.0013(14) -0.0011(13)
C131 0.0198(15) 0.0161(14) 0.0278(16) 0.0031(12) -0.0035(13) -0.0034(12)
C141 0.0253(17) 0.051(2) 0.0288(19) -0.0141(16) -0.0020(15) 0.0105(17)
C151 0.0197(15) 0.0347(18) 0.0215(15) -0.0060(14) 0.0036(13) 0.0062(14)
C161 0.050(3) 0.034(2) 0.064(3) 0.000(2) -0.016(2) 0.006(2)
C171 0.068(4) 0.042(3) 0.100(5) -0.033(3) -0.021(3) 0.001(3)
C181 0.042(3) 0.091(4) 0.043(3) -0.036(3) -0.014(2) 0.025(3)
C191 0.027(2) 0.092(4) 0.031(2) 0.013(2) 0.0016(17) 0.014(2)
C201 0.0275(19) 0.050(2) 0.041(2) 0.0128(19) 0.0025(17) 0.0001(18)
C211 0.0219(15) 0.0177(14) 0.0212(15) 0.0000(12) -0.0020(12) 0.0033(12)
C221 0.0267(17) 0.0177(15) 0.0202(15) 0.0005(12) -0.0048(13) -0.0019(13)
C231 0.0344(18) 0.0237(17) 0.0280(17) 0.0035(14) 0.0056(15) 0.0004(15)
C241 0.039(2) 0.037(2) 0.033(2) 0.0030(16) 0.0131(17) -0.0040(18)
C251 0.049(2) 0.031(2) 0.0287(18) 0.0073(15) 0.0026(17) -0.0124(17)
C261 0.048(2) 0.0233(18) 0.040(2) 0.0104(16) -0.0049(18) -0.0031(17)
C271 0.0353(19) 0.0250(17) 0.0339(18) 0.0044(15) -0.0030(15) 0.0039(16)
C281 0.037(2) 0.069(3) 0.095(4) -0.044(3) 0.026(3) -0.007(2)
C291 0.0263(18) 0.029(2) 0.071(3) 0.0065(19) -0.0048(19) 0.0082(16)
V2 0.0210(2) 0.0141(2) 0.0220(2) 0.0015(2) -0.0002(2) 0.0009(2)
O12 0.0243(12) 0.0212(11) 0.0337(13) 0.0012(10) -0.0003(10) -0.0019(10)
O22 0.0250(12) 0.0146(10) 0.0245(11) -0.0004(9) 0.0027(10) 0.0007(9)
O32 0.0268(11) 0.0150(10) 0.0198(10) 0.0012(8) -0.0017(9) 0.0036(9)
O42 0.0332(13) 0.0202(11) 0.0261(12) 0.0040(9) -0.0043(10) 0.0017(10)
O52 0.0175(10) 0.0201(11) 0.0207(11) 0.0032(9) 0.0009(9) 0.0025(9)
O62 0.0205(11) 0.0163(10) 0.0223(11) -0.0020(9) -0.0023(9) 0.0014(9)
O72 0.0171(10) 0.0198(11) 0.0248(11) -0.0002(9) 0.0002(9) 0.0014(9)
O82 0.0268(12) 0.0172(11) 0.0259(12) 0.0001(9) -0.0013(10) 0.0049(9)
O92 0.0285(13) 0.0290(13) 0.0447(15) -0.0026(12) 0.0004(12) 0.0139(11)
N2 0.0182(12) 0.0145(12) 0.0232(13) 0.0014(10) 0.0020(11) -0.0018(10)
C12 0.0175(15) 0.0187(15) 0.0213(15) 0.0008(12) 0.0013(12) -0.0005(12)
C22 0.0155(14) 0.0156(14) 0.0229(15) 0.0005(12) 0.0014(12) -0.0012(12)
C32 0.0192(14) 0.0153(13) 0.0191(14) 0.0026(11) -0.0003(11) -0.0014(11)
C42 0.0185(14) 0.0153(14) 0.0212(15) 0.0002(11) 0.0001(12) -0.0008(11)
C52 0.0168(14) 0.0178(14) 0.0217(15) -0.0001(12) 0.0008(12) 0.0012(12)
C62 0.0246(16) 0.0218(15) 0.0253(16) 0.0008(12) -0.0005(13) 0.0065(13)
C72 0.0227(15) 0.0164(15) 0.0247(15) -0.0003(12) -0.0012(13) -0.0033(12)
C82 0.0207(15) 0.0195(15) 0.0275(16) -0.0044(12) 0.0032(13) -0.0059(13)
C92 0.040(2) 0.0215(16) 0.0275(17) -0.0030(14) 0.0026(16) -0.0015(15)
C102 0.043(2) 0.034(2) 0.0297(19) -0.0057(15) 0.0118(17) -0.0025(18)
C112 0.0313(18) 0.0275(17) 0.042(2) -0.0106(16) 0.0106(17) 0.0021(15)
C122 0.0196(15) 0.0212(16) 0.0357(19) -0.0031(14) 0.0020(14) -0.0016(13)
C132 0.0204(15) 0.0171(14) 0.0283(16) -0.0031(12) 0.0039(13) -0.0068(12)
C142 0.0242(16) 0.0240(16) 0.0232(16) 0.0043(13) -0.0021(13) 0.0043(13)
C212 0.0249(16) 0.0186(15) 0.0206(15) -0.0012(12) 0.0032(13) 0.0029(13)
C222 0.0349(19) 0.0162(14) 0.0223(15) 0.0008(12) -0.0003(14) 0.0007(14)
C232 0.037(2) 0.0263(18) 0.0310(19) -0.0053(15) -0.0047(16) 0.0025(15)
C242 0.040(2) 0.0306(19) 0.042(2) -0.0012(16) -0.0125(18) -0.0041(17)
C252 0.069(3) 0.0229(18) 0.0257(18) -0.0007(14) -0.0101(19) -0.0073(18)
C262 0.068(3) 0.0223(18) 0.0274(18) -0.0046(15) 0.0068(19) -0.0013(19)
C272 0.048(2) 0.0232(17) 0.0301(19) -0.0041(15) 0.0079(17) 0.0001(17)
C282 0.049(3) 0.042(2) 0.049(2) 0.012(2) -0.026(2) -0.002(2)
C292 0.0198(17) 0.029(2) 0.081(3) 0.003(2) 0.0054(19) 0.0067(15)
O1M1 0.0279(12) 0.0208(11) 0.0249(11) 0.0038(9) -0.0034(10) -0.0052(10)
C1M1 0.092(4) 0.041(2) 0.049(3) 0.023(2) -0.041(3) -0.031(3)
O1M2 0.0276(12) 0.0207(11) 0.0281(12) -0.0026(9) 0.0059(10) -0.0027(10)
C1M2 0.061(3) 0.050(3) 0.053(3) -0.024(2) 0.032(2) -0.022(2)
O1M 0.084(3) 0.098(3) 0.0451(19) 0.034(2) 0.030(2) 0.055(3)
C1M 0.054(3) 0.040(2) 0.031(2) -0.0023(17) 0.0040(19) 0.006(2)
O2M 0.057(2) 0.059(2) 0.0247(13) 0.0005(13) 0.0043(14) -0.0204(16)
C2M 0.042(2) 0.059(3) 0.034(2) -0.0032(19) 0.0056(19) -0.007(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
V1 O11 1.591(2) . ?
V1 O21 1.914(2) . ?
V1 O31 1.879(2) . ?
V1 O41 1.779(2) . ?
V1 N1 2.166(3) . ?
V1 O1M1 2.294(2) . ?
O21 C131 1.340(4) . ?
O31 C31 1.419(4) . ?
O41 C281 1.415(5) . ?
O51 C11 1.401(4) . ?
O51 C141 1.445(4) . ?
O61 C41 1.430(4) . ?
O61 C211 1.427(4) . ?
O71 C11 1.419(4) . ?
O71 C51 1.433(4) . ?
O81 C61 1.433(4) . ?
O81 C211 1.415(4) . ?
O91 C121 1.361(4) . ?
O91 C291 1.423(4) . ?
N1 C21 1.462(4) . ?
N1 C71 1.285(4) . ?
C11 H11 1.0000 . ?
C11 C21 1.525(4) . ?
C21 H21 1.0000 . ?
C21 C31 1.539(4) . ?
C31 H31 1.0000 . ?
C31 C41 1.509(4) . ?
C41 H41 1.0000 . ?
C41 C51 1.529(4) . ?
C51 H51 1.0000 . ?
C51 C61 1.507(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C71 H71 0.9500 . ?
C71 C81 1.447(4) . ?
C81 C91 1.415(5) . ?
C81 C131 1.397(5) . ?
C91 H91 0.9500 . ?
C91 C101 1.376(5) . ?
C101 H101 0.9500 . ?
C101 C111 1.383(6) . ?
C111 H111 0.9500 . ?
C111 C121 1.392(5) . ?
C121 C131 1.416(5) . ?
C141 H14E 0.9900 . ?
C141 H14F 0.9900 . ?
C141 C151 1.487(5) . ?
C151 C161 1.377(6) . ?
C151 C201 1.378(5) . ?
C161 H161 0.9500 . ?
C161 C171 1.403(7) . ?
C171 H171 0.9500 . ?
C171 C181 1.365(8) . ?
C181 H181 0.9500 . ?
C181 C191 1.347(8) . ?
C191 H191 0.9500 . ?
C191 C201 1.384(6) . ?
C201 H201 0.9500 . ?
C211 H211 1.0000 . ?
C211 C221 1.510(4) . ?
C221 C231 1.381(5) . ?
C221 C271 1.385(5) . ?
C231 H231 0.9500 . ?
C231 C241 1.392(5) . ?
C241 H241 0.9500 . ?
C241 C251 1.380(6) . ?
C251 H251 0.9500 . ?
C251 C261 1.385(6) . ?
C261 H261 0.9500 . ?
C261 C271 1.381(5) . ?
C271 H271 0.9500 . ?
C281 H28D 0.9800 . ?
C281 H28E 0.9800 . ?
C281 H28F 0.9800 . ?
C291 H29D 0.9800 . ?
C291 H29E 0.9800 . ?
C291 H29F 0.9800 . ?
V2 O12 1.601(2) . ?
V2 O22 1.912(2) . ?
V2 O32 1.889(2) . ?
V2 O42 1.776(2) . ?
V2 N2 2.171(3) . ?
V2 O1M2 2.271(2) . ?
O22 C132 1.344(4) . ?
O32 C32 1.410(4) . ?
O42 C282 1.409(5) . ?
O52 C12 1.405(4) . ?
O52 C142 1.446(4) . ?
O62 C42 1.435(4) . ?
O62 C212 1.420(4) . ?
O72 C12 1.420(4) . ?
O72 C52 1.435(4) . ?
O82 C62 1.439(4) . ?
O82 C212 1.416(4) . ?
O92 C122 1.369(4) . ?
O92 C292 1.428(4) . ?
N2 C22 1.465(4) . ?
N2 C72 1.280(4) . ?
C12 H12 1.0000 . ?
C12 C22 1.532(4) . ?
C22 H22 1.0000 . ?
C22 C32 1.537(4) . ?
C32 H32 1.0000 . ?
C32 C42 1.508(4) . ?
C42 H42 1.0000 . ?
C42 C52 1.522(4) . ?
C52 H52 1.0000 . ?
C52 C62 1.516(4) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C72 H72 0.9500 . ?
C72 C82 1.449(5) . ?
C82 C92 1.406(5) . ?
C82 C132 1.399(5) . ?
C92 H92 0.9500 . ?
C92 C102 1.381(5) . ?
C102 H102 0.9500 . ?
C102 C112 1.382(6) . ?
C112 H112 0.9500 . ?
C112 C122 1.391(5) . ?
C122 C132 1.412(5) . ?
C142 H14A 0.9900 . ?
C142 H14B 0.9900 . ?
C142 H14C 0.9900 . ?
C142 H14D 0.9900 . ?
C142 C152 1.495(13) . ?
C142 C153 1.500(11) . ?
C152 C162 1.413(14) . ?
C152 C202 1.352(13) . ?
C162 H162 0.9500 . ?
C162 C172 1.419(14) . ?
C172 H172 0.9500 . ?
C172 C182 1.363(13) . ?
C182 H182 0.9500 . ?
C182 C192 1.357(12) . ?
C192 H192 0.9500 . ?
C192 C202 1.365(11) . ?
C202 H202 0.9500 . ?
C153 C163 1.355(12) . ?
C153 C203 1.396(13) . ?
C163 H163 0.9500 . ?
C163 C173 1.377(12) . ?
C173 H173 0.9500 . ?
C173 C183 1.358(12) . ?
C183 H183 0.9500 . ?
C183 C193 1.343(13) . ?
C193 H193 0.9500 . ?
C193 C203 1.398(13) . ?
C203 H203 0.9500 . ?
C212 H212 1.0000 . ?
C212 C222 1.506(5) . ?
C222 C232 1.376(5) . ?
C222 C272 1.395(5) . ?
C232 H232 0.9500 . ?
C232 C242 1.392(5) . ?
C242 H242 0.9500 . ?
C242 C252 1.380(6) . ?
C252 H252 0.9500 . ?
C252 C262 1.376(7) . ?
C262 H262 0.9500 . ?
C262 C272 1.393(5) . ?
C272 H272 0.9500 . ?
C282 H28A 0.9800 . ?
C282 H28B 0.9800 . ?
C282 H28C 0.9800 . ?
C292 H29A 0.9800 . ?
C292 H29B 0.9800 . ?
C292 H29C 0.9800 . ?
O1M1 H1M1 0.8400 . ?
O1M1 C1M1 1.397(5) . ?
C1M1 H1MD 0.9800 . ?
C1M1 H1ME 0.9800 . ?
C1M1 H1MF 0.9800 . ?
O1M2 H1M2 0.8400 . ?
O1M2 C1M2 1.395(5) . ?
C1M2 H1MA 0.9800 . ?
C1M2 H1MB 0.9800 . ?
C1M2 H1MC 0.9800 . ?
O1M H1M 0.8400 . ?
O1M C1M 1.391(6) . ?
C1M H1MG 0.9800 . ?
C1M H1MH 0.9800 . ?
C1M H1MI 0.9800 . ?
O2M H2M 0.8400 . ?
O2M C2M 1.403(5) . ?
C2M H2MA 0.9800 . ?
C2M H2MB 0.9800 . ?
C2M H2MC 0.9800 . ?
O3M H3M 0.8400 . ?
O3M C3M 1.430(12) . ?
C3M H3MA 0.9800 . ?
C3M H3MB 0.9800 . ?
C3M H3MC 0.9800 . ?
O3MA H3MD 0.8400 . ?
O3MA C3MA 1.401(14) . ?
C3MA H3ME 0.9800 . ?
C3MA H3MF 0.9800 . ?
C3MA H3MG 0.9800 . ?
O4M H4M 0.8400 . ?
O4M C4M 1.420(13) . ?
C4M H4MA 0.9800 . ?
C4M H4MB 0.9800 . ?
C4M H4MC 0.9800 . ?
O4MA H4MD 0.8400 . ?
O4MA C4MA 1.406(13) . ?
C4MA H4ME 0.9800 . ?
C4MA H4MF 0.9800 . ?
C4MA H4MG 0.9800 . ?

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
O11 V1 O21 96.09(12) . . ?
O11 V1 O31 99.95(12) . . ?
O11 V1 O41 103.43(13) . . ?
O11 V1 N1 93.87(11) . . ?
O11 V1 O1M1 170.18(11) . . ?
O21 V1 N1 81.51(10) . . ?
O21 V1 O1M1 78.46(10) . . ?
O31 V1 O21 155.28(11) . . ?
O31 V1 N1 78.75(10) . . ?
O31 V1 O1M1 82.78(10) . . ?
O41 V1 O21 96.42(11) . . ?
O41 V1 O31 97.99(11) . . ?
O41 V1 N1 162.70(11) . . ?
O41 V1 O1M1 85.40(11) . . ?
N1 V1 O1M1 77.34(9) . . ?
C131 O21 V1 126.4(2) . . ?
C31 O31 V1 116.00(18) . . ?
C281 O41 V1 127.8(3) . . ?
C11 O51 C141 111.5(2) . . ?
C211 O61 C41 109.1(2) . . ?
C11 O71 C51 112.4(2) . . ?
C211 O81 C61 110.9(2) . . ?
C121 O91 C291 116.5(3) . . ?
C21 N1 V1 109.90(19) . . ?
C71 N1 V1 126.9(2) . . ?
C71 N1 C21 123.1(3) . . ?
O51 C11 O71 112.6(2) . . ?
O51 C11 H11 108.8 . . ?
O51 C11 C21 109.7(2) . . ?
O71 C11 H11 108.8 . . ?
O71 C11 C21 108.2(2) . . ?
C21 C11 H11 108.8 . . ?
N1 C21 C11 119.3(3) . . ?
N1 C21 H21 106.7 . . ?
N1 C21 C31 103.0(2) . . ?
C11 C21 H21 106.7 . . ?
C11 C21 C31 113.7(3) . . ?
C31 C21 H21 106.7 . . ?
O31 C31 C21 105.6(2) . . ?
O31 C31 H31 109.7 . . ?
O31 C31 C41 113.9(2) . . ?
C21 C31 H31 109.7 . . ?
C41 C31 C21 108.0(2) . . ?
C41 C31 H31 109.7 . . ?
O61 C41 C31 111.4(2) . . ?
O61 C41 H41 109.7 . . ?
O61 C41 C51 108.6(2) . . ?
C31 C41 H41 109.7 . . ?
C31 C41 C51 107.8(2) . . ?
C51 C41 H41 109.7 . . ?
O71 C51 C41 110.6(2) . . ?
O71 C51 H51 109.4 . . ?
O71 C51 C61 109.0(3) . . ?
C41 C51 H51 109.4 . . ?
C61 C51 C41 109.2(2) . . ?
C61 C51 H51 109.4 . . ?
O81 C61 C51 108.1(2) . . ?
O81 C61 H61A 110.1 . . ?
O81 C61 H61B 110.1 . . ?
C51 C61 H61A 110.1 . . ?
C51 C61 H61B 110.1 . . ?
H61A C61 H61B 108.4 . . ?
N1 C71 H71 118.7 . . ?
N1 C71 C81 122.7(3) . . ?
C81 C71 H71 118.7 . . ?
C91 C81 C71 118.6(3) . . ?
C131 C81 C71 121.3(3) . . ?
C131 C81 C91 120.1(3) . . ?
C81 C91 H91 120.2 . . ?
C101 C91 C81 119.6(4) . . ?
C101 C91 H91 120.2 . . ?
C91 C101 H101 119.6 . . ?
C91 C101 C111 120.7(3) . . ?
C111 C101 H101 119.6 . . ?
C101 C111 H111 119.6 . . ?
C101 C111 C121 120.8(3) . . ?
C121 C111 H111 119.6 . . ?
O91 C121 C111 126.0(3) . . ?
O91 C121 C131 114.6(3) . . ?
C111 C121 C131 119.4(3) . . ?
O21 C131 C81 122.5(3) . . ?
O21 C131 C121 118.2(3) . . ?
C81 C131 C121 119.3(3) . . ?
O51 C141 H14E 109.7 . . ?
O51 C141 H14F 109.7 . . ?
O51 C141 C151 110.0(3) . . ?
H14E C141 H14F 108.2 . . ?
C151 C141 H14E 109.7 . . ?
C151 C141 H14F 109.7 . . ?
C161 C151 C141 119.9(4) . . ?
C161 C151 C201 118.1(4) . . ?
C201 C151 C141 122.0(4) . . ?
C151 C161 H161 119.7 . . ?
C151 C161 C171 120.5(5) . . ?
C171 C161 H161 119.7 . . ?
C161 C171 H171 120.4 . . ?
C181 C171 C161 119.2(5) . . ?
C181 C171 H171 120.4 . . ?
C171 C181 H181 119.5 . . ?
C191 C181 C171 121.0(4) . . ?
C191 C181 H181 119.5 . . ?
C181 C191 H191 120.1 . . ?
C181 C191 C201 119.9(5) . . ?
C201 C191 H191 120.1 . . ?
C151 C201 C191 121.2(4) . . ?
C151 C201 H201 119.4 . . ?
C191 C201 H201 119.4 . . ?
O61 C211 H211 109.5 . . ?
O61 C211 C221 109.8(3) . . ?
O81 C211 O61 111.0(2) . . ?
O81 C211 H211 109.5 . . ?
O81 C211 C221 107.7(3) . . ?
C221 C211 H211 109.5 . . ?
C231 C221 C211 122.3(3) . . ?
C231 C221 C271 119.5(3) . . ?
C271 C221 C211 118.2(3) . . ?
C221 C231 H231 120.1 . . ?
C221 C231 C241 119.8(3) . . ?
C241 C231 H231 120.1 . . ?
C231 C241 H241 119.7 . . ?
C251 C241 C231 120.6(4) . . ?
C251 C241 H241 119.7 . . ?
C241 C251 H251 120.3 . . ?
C241 C251 C261 119.4(4) . . ?
C261 C251 H251 120.3 . . ?
C251 C261 H261 120.0 . . ?
C271 C261 C251 120.1(4) . . ?
C271 C261 H261 120.0 . . ?
C221 C271 H271 119.7 . . ?
C261 C271 C221 120.6(4) . . ?
C261 C271 H271 119.7 . . ?
O41 C281 H28D 109.5 . . ?
O41 C281 H28E 109.5 . . ?
O41 C281 H28F 109.5 . . ?
H28D C281 H28E 109.5 . . ?
H28D C281 H28F 109.5 . . ?
H28E C281 H28F 109.5 . . ?
O91 C291 H29D 109.5 . . ?
O91 C291 H29E 109.5 . . ?
O91 C291 H29F 109.5 . . ?
H29D C291 H29E 109.5 . . ?
H29D C291 H29F 109.5 . . ?
H29E C291 H29F 109.5 . . ?
O12 V2 O22 96.45(11) . . ?
O12 V2 O32 99.04(11) . . ?
O12 V2 O42 103.31(12) . . ?
O12 V2 N2 94.41(11) . . ?
O12 V2 O1M2 171.01(11) . . ?
O22 V2 N2 81.59(10) . . ?
O22 V2 O1M2 78.00(9) . . ?
O32 V2 O22 155.34(10) . . ?
O32 V2 N2 78.20(10) . . ?
O32 V2 O1M2 84.03(10) . . ?
O42 V2 O22 99.03(10) . . ?
O42 V2 O32 95.94(11) . . ?
O42 V2 N2 162.05(11) . . ?
O42 V2 O1M2 84.68(11) . . ?
N2 V2 O1M2 77.87(9) . . ?
C132 O22 V2 125.5(2) . . ?
C32 O32 V2 116.25(18) . . ?
C282 O42 V2 130.2(3) . . ?
C12 O52 C142 111.6(2) . . ?
C212 O62 C42 108.5(2) . . ?
C12 O72 C52 112.1(2) . . ?
C212 O82 C62 111.4(2) . . ?
C122 O92 C292 116.4(3) . . ?
C22 N2 V2 109.67(19) . . ?
C72 N2 V2 126.1(2) . . ?
C72 N2 C22 124.1(3) . . ?
O52 C12 O72 112.2(2) . . ?
O52 C12 H12 108.8 . . ?
O52 C12 C22 110.2(2) . . ?
O72 C12 H12 108.8 . . ?
O72 C12 C22 107.8(2) . . ?
C22 C12 H12 108.8 . . ?
N2 C22 C12 119.5(3) . . ?
N2 C22 H22 106.5 . . ?
N2 C22 C32 102.6(2) . . ?
C12 C22 H22 106.5 . . ?
C12 C22 C32 114.4(2) . . ?
C32 C22 H22 106.5 . . ?
O32 C32 C22 105.2(2) . . ?
O32 C32 H32 109.9 . . ?
O32 C32 C42 113.8(2) . . ?
C22 C32 H32 109.9 . . ?
C42 C32 C22 108.0(2) . . ?
C42 C32 H32 109.9 . . ?
O62 C42 C32 111.1(2) . . ?
O62 C42 H42 109.8 . . ?
O62 C42 C52 108.6(2) . . ?
C32 C42 H42 109.8 . . ?
C32 C42 C52 107.6(2) . . ?
C52 C42 H42 109.8 . . ?
O72 C52 C42 109.9(2) . . ?
O72 C52 H52 109.7 . . ?
O72 C52 C62 107.9(3) . . ?
C42 C52 H52 109.7 . . ?
C62 C52 C42 109.8(3) . . ?
C62 C52 H52 109.7 . . ?
O82 C62 C52 107.5(3) . . ?
O82 C62 H62A 110.2 . . ?
O82 C62 H62B 110.2 . . ?
C52 C62 H62A 110.2 . . ?
C52 C62 H62B 110.2 . . ?
H62A C62 H62B 108.5 . . ?
N2 C72 H72 118.4 . . ?
N2 C72 C82 123.2(3) . . ?
C82 C72 H72 118.4 . . ?
C92 C82 C72 118.4(3) . . ?
C132 C82 C72 120.9(3) . . ?
C132 C82 C92 120.8(3) . . ?
C82 C92 H92 120.3 . . ?
C102 C92 C82 119.4(3) . . ?
C102 C92 H92 120.3 . . ?
C92 C102 H102 119.7 . . ?
C92 C102 C112 120.7(3) . . ?
C112 C102 H102 119.7 . . ?
C102 C112 H112 119.7 . . ?
C102 C112 C122 120.6(3) . . ?
C122 C112 H112 119.7 . . ?
O92 C122 C112 125.0(3) . . ?
O92 C122 C132 115.1(3) . . ?
C112 C122 C132 120.0(3) . . ?
O22 C132 C82 122.2(3) . . ?
O22 C132 C122 119.2(3) . . ?
C82 C132 C122 118.6(3) . . ?
O52 C142 H14A 110.2 . . ?
O52 C142 H14B 110.2 . . ?
O52 C142 H14C 109.7 . . ?
O52 C142 H14D 109.7 . . ?
O52 C142 C152 107.5(6) . . ?
O52 C142 C153 109.9(6) . . ?
H14A C142 H14B 108.5 . . ?
H14C C142 H14D 108.2 . . ?
C152 C142 H14A 110.2 . . ?
C152 C142 H14B 110.2 . . ?
C153 C142 H14C 109.7 . . ?
C153 C142 H14D 109.7 . . ?
C162 C152 C142 120.2(10) . . ?
C202 C152 C142 122.3(10) . . ?
C202 C152 C162 117.6(11) . . ?
C152 C162 H162 119.6 . . ?
C152 C162 C172 120.9(11) . . ?
C172 C162 H162 119.6 . . ?
C162 C172 H172 121.6 . . ?
C182 C172 C162 116.8(10) . . ?
C182 C172 H172 121.6 . . ?
C172 C182 H182 118.7 . . ?
C192 C182 C172 122.7(9) . . ?
C192 C182 H182 118.7 . . ?
C182 C192 H192 120.2 . . ?
C182 C192 C202 119.6(8) . . ?
C202 C192 H192 120.2 . . ?
C152 C202 C192 122.3(11) . . ?
C152 C202 H202 118.8 . . ?
C192 C202 H202 118.8 . . ?
C163 C153 C142 121.1(9) . . ?
C163 C153 C203 117.0(10) . . ?
C203 C153 C142 121.7(10) . . ?
C153 C163 H163 119.9 . . ?
C153 C163 C173 120.2(10) . . ?
C173 C163 H163 119.9 . . ?
C163 C173 H173 118.9 . . ?
C183 C173 C163 122.2(9) . . ?
C183 C173 H173 118.9 . . ?
C173 C183 H183 120.1 . . ?
C193 C183 C173 119.8(8) . . ?
C193 C183 H183 120.1 . . ?
C183 C193 H193 120.9 . . ?
C183 C193 C203 118.2(9) . . ?
C203 C193 H193 120.9 . . ?
C153 C203 C193 122.4(11) . . ?
C153 C203 H203 118.8 . . ?
C193 C203 H203 118.8 . . ?
O62 C212 H212 109.6 . . ?
O62 C212 C222 110.8(3) . . ?
O82 C212 O62 110.7(2) . . ?
O82 C212 H212 109.6 . . ?
O82 C212 C222 106.6(3) . . ?
C222 C212 H212 109.6 . . ?
C232 C222 C212 122.5(3) . . ?
C232 C222 C272 119.8(4) . . ?
C272 C222 C212 117.6(3) . . ?
C222 C232 H232 119.9 . . ?
C222 C232 C242 120.2(4) . . ?
C242 C232 H232 119.9 . . ?
C232 C242 H242 120.1 . . ?
C252 C242 C232 119.8(4) . . ?
C252 C242 H242 120.1 . . ?
C242 C252 H252 119.7 . . ?
C262 C252 C242 120.5(4) . . ?
C262 C252 H252 119.7 . . ?
C252 C262 H262 120.1 . . ?
C252 C262 C272 119.9(4) . . ?
C272 C262 H262 120.1 . . ?
C222 C272 H272 120.1 . . ?
C262 C272 C222 119.7(4) . . ?
C262 C272 H272 120.1 . . ?
O42 C282 H28A 109.5 . . ?
O42 C282 H28B 109.5 . . ?
O42 C282 H28C 109.5 . . ?
H28A C282 H28B 109.5 . . ?
H28A C282 H28C 109.5 . . ?
H28B C282 H28C 109.5 . . ?
O92 C292 H29A 109.5 . . ?
O92 C292 H29B 109.5 . . ?
O92 C292 H29C 109.5 . . ?
H29A C292 H29B 109.5 . . ?
H29A C292 H29C 109.5 . . ?
H29B C292 H29C 109.5 . . ?
V1 O1M1 H1M1 121.0 . . ?
C1M1 O1M1 V1 128.4(3) . . ?
C1M1 O1M1 H1M1 109.5 . . ?
O1M1 C1M1 H1MD 109.5 . . ?
O1M1 C1M1 H1ME 109.5 . . ?
O1M1 C1M1 H1MF 109.5 . . ?
H1MD C1M1 H1ME 109.5 . . ?
H1MD C1M1 H1MF 109.5 . . ?
H1ME C1M1 H1MF 109.5 . . ?
V2 O1M2 H1M2 119.0 . . ?
C1M2 O1M2 V2 129.2(3) . . ?
C1M2 O1M2 H1M2 109.5 . . ?
O1M2 C1M2 H1MA 109.5 . . ?
O1M2 C1M2 H1MB 109.5 . . ?
O1M2 C1M2 H1MC 109.5 . . ?
H1MA C1M2 H1MB 109.5 . . ?
H1MA C1M2 H1MC 109.5 . . ?
H1MB C1M2 H1MC 109.5 . . ?
C1M O1M H1M 109.5 . . ?
O1M C1M H1MG 109.5 . . ?
O1M C1M H1MH 109.5 . . ?
O1M C1M H1MI 109.5 . . ?
H1MG C1M H1MH 109.5 . . ?
H1MG C1M H1MI 109.5 . . ?
H1MH C1M H1MI 109.5 . . ?
C2M O2M H2M 109.5 . . ?
O2M C2M H2MA 109.5 . . ?
O2M C2M H2MB 109.5 . . ?
O2M C2M H2MC 109.5 . . ?
H2MA C2M H2MB 109.5 . . ?
H2MA C2M H2MC 109.5 . . ?
H2MB C2M H2MC 109.5 . . ?
C3M O3M H3M 109.5 . . ?
O3M C3M H3MA 109.5 . . ?
O3M C3M H3MB 109.5 . . ?
O3M C3M H3MC 109.5 . . ?
H3MA C3M H3MB 109.5 . . ?
H3MA C3M H3MC 109.5 . . ?
H3MB C3M H3MC 109.5 . . ?
C3MA O3MA H3MD 109.5 . . ?
O3MA C3MA H3ME 109.5 . . ?
O3MA C3MA H3MF 109.5 . . ?
O3MA C3MA H3MG 109.5 . . ?
H3ME C3MA H3MF 109.5 . . ?
H3ME C3MA H3MG 109.5 . . ?
H3MF C3MA H3MG 109.5 . . ?
C4M O4M H4M 109.5 . . ?
O4M C4M H4MA 109.5 . . ?
O4M C4M H4MB 109.5 . . ?
O4M C4M H4MC 109.5 . . ?
H4MA C4M H4MB 109.5 . . ?
H4MA C4M H4MC 109.5 . . ?
H4MB C4M H4MC 109.5 . . ?
C4MA O4MA H4MD 109.5 . . ?
O4MA C4MA H4ME 109.5 . . ?
O4MA C4MA H4MF 109.5 . . ?
O4MA C4MA H4MG 109.5 . . ?
H4ME C4MA H4MF 109.5 . . ?
H4ME C4MA H4MG 109.5 . . ?
H4MF C4MA H4MG 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1M1 H1M1 O22 0.84 1.99 2.812(3) 167.4 .
O1M2 H1M2 O21 0.84 1.92 2.758(3) 175.8 .
O1M H1M O31 0.84 1.95 2.780(4) 171.0 .
O2M H2M O32 0.84 1.91 2.740(4) 172.3 .
O3M H3M O1M 0.84 2.02 2.844(7) 166.8 .
O3MA H3MD O1M 0.84 2.00 2.677(11) 137.3 .
O4M H4M O2M 0.84 1.91 2.748(10) 171.6 .
O4MA H4MD O2M 0.84 1.82 2.639(11) 165.3 .

_database_code_depnum_ccdc_archive 'CCDC 927423'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_fo4341
_audit_creation_date             2013-05-12
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C29 H30 N O9 V, C H Cl3'
_chemical_formula_sum            'C30 H31 Cl3 N O9 V'
_chemical_formula_weight         706.85
_chemical_absolute_configuration syn
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.10390(10)
_cell_length_b                   18.2392(4)
_cell_length_c                   14.3543(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.1380(10)
_cell_angle_gamma                90
_cell_volume                     1585.68(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10948
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.652
_diffrn_ambient_temperature      133.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.887
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                6681
_reflns_number_total             6790
_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.
;
_reflns_threshold_expression     'I > 2\s(I)'
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 
;
 Flack x determined using 2935 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.014(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6790
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0257
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+0.7800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0607
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H1(0.023) H2(0.02) H3(0.018) H4(0.02) H5(0.022) H6A(0.031)
 H6B(0.031) H7(0.023) H9(0.03) H10(0.035) H11(0.033) H14A(0.035) H14B(0.035)
 H16(0.036) H17(0.045) H18(0.043) H19(0.044) H20(0.037) H21(0.022) H23(0.026)
 H24(0.031) H25(0.036) H26(0.037) H27(0.029) H28A(0.054) H28B(0.054)
 H28C(0.054) H29A(0.046) H29B(0.046) H29C(0.046) H1CL(0.034)
 Fixed X: H1(0.3171) H2(0.1488) H3(-0.1578) H4(0.1655) H5(0.172) H6A(0.4906)
 H6B(0.5169) H7(0.0207) H9(-0.0996) H10(-0.3464) H11(-0.6598) H14A(0.405)
 H14B(0.1986) H16(0.5233) H17(0.4805) H18(0.1639) H19(-0.1108) H20(-0.0712)
 H21(0.1908) H23(-0.3057) H24(-0.5144) H25(-0.3564) H26(0.0105) H27(0.2217)
 H28A(-0.7966) H28B(-0.5952) H28C(-0.7893) H29A(-1.031) H29B(-0.8279) H29C(-
 0.9827) H1CL(-0.2627)
 Fixed Y: H1(-0.3981) H2(-0.3286) H3(-0.4467) H4(-0.3884) H5(-0.5246) H6A(-
 0.4695) H6B(-0.5452) H7(-0.3653) H9(-0.3249) H10(-0.2623) H11(-0.2058) H14A(-
 0.526) H14B(-0.5796) H16(-0.4471) H17(-0.4023) H18(-0.4291) H19(-0.5022) H20(-
 0.5473) H21(-0.4598) H23(-0.4864) H24(-0.5563) H25(-0.6584) H26(-0.689) H27(-
 0.6187) H28A(-0.2081) H28B(-0.163) H28C(-0.1921) H29A(-0.1377) H29B(-0.1153)
 H29C(-0.1829) H1CL(-0.3235)
 Fixed Z: H1(-0.4016) H2(-0.5293) H3(-0.5706) H4(-0.6815) H5(-0.5781) H6A(-
 0.6924) H6B(-0.6347) H7(-0.3308) H9(-0.1816) H10(-0.1002) H11(-0.1804) H14A(-
 0.3676) H14B(-0.3624) H16(-0.2361) H17(-0.0872) H18(-0.0189) H19(-0.0986) H20(-
 0.2478) H21(-0.8219) H23(-0.8693) H24(-0.9837) H25(-1.049) H26(-0.9994) H27(-
 0.8855) H28A(-0.7184) H28B(-0.664) H28C(-0.6084) H29A(-0.3703) H29B(-0.2943)
 H29C(-0.2744) H1CL(-0.7733)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
V V -0.34033(6) -0.28161(2) -0.55691(3) 0.01589(8) Uani 1 1 d . . . . .
O1 O -0.2085(3) -0.20667(10) -0.55811(14) 0.0255(4) Uani 1 1 d . . . . .
O2 O -0.4955(3) -0.27502(11) -0.45464(11) 0.0209(3) Uani 1 1 d . . . . .
O3 O -0.2185(3) -0.34950(10) -0.63046(12) 0.0196(4) Uani 1 1 d . . . . .
O4 O -0.5824(3) -0.26933(10) -0.63844(12) 0.0211(4) Uani 1 1 d . . . . .
O5 O 0.1151(3) -0.48248(10) -0.42340(13) 0.0218(4) Uani 1 1 d . . . . .
O6 O -0.0309(3) -0.47117(10) -0.73176(12) 0.0180(3) Uani 1 1 d . . . . .
O7 O 0.3736(3) -0.44555(10) -0.52241(13) 0.0217(4) Uani 1 1 d . . . . .
O8 O 0.2754(3) -0.54712(10) -0.74297(14) 0.0224(4) Uani 1 1 d . . . . .
O9 O -0.7739(3) -0.20515(11) -0.36650(14) 0.0279(4) Uani 1 1 d . . . . .
N N -0.1071(3) -0.33651(11) -0.45498(14) 0.0163(4) Uani 1 1 d . . . . .
C1 C 0.2294(4) -0.42318(14) -0.45591(18) 0.0195(5) Uani 1 1 d . . . . .
H1 H 0.3171 -0.3981 -0.4016 0.023 Uiso 1 1 calc R U . . .
C2 C 0.0626(4) -0.36977(13) -0.50571(17) 0.0163(5) Uani 1 1 d . . . . .
H2 H 0.1488 -0.3286 -0.5293 0.020 Uiso 1 1 calc R U . . .
C3 C -0.0716(4) -0.40421(13) -0.59103(16) 0.0154(4) Uani 1 1 d . . . . .
H3 H -0.1578 -0.4467 -0.5706 0.018 Uiso 1 1 calc R U . . .
C4 C 0.0874(4) -0.43093(13) -0.65643(17) 0.0169(5) Uani 1 1 d . . . . .
H4 H 0.1655 -0.3884 -0.6815 0.020 Uiso 1 1 calc R U . . .
C5 C 0.2535(4) -0.48219(13) -0.60145(18) 0.0186(5) Uani 1 1 d . . . . .
H5 H 0.1720 -0.5246 -0.5781 0.022 Uiso 1 1 calc R U . . .
C6 C 0.4089(4) -0.51062(16) -0.6678(2) 0.0256(5) Uani 1 1 d . . . . .
H6A H 0.4906 -0.4695 -0.6924 0.031 Uiso 1 1 calc R U . . .
H6B H 0.5169 -0.5452 -0.6347 0.031 Uiso 1 1 calc R U . . .
C7 C -0.0978(4) -0.33930(13) -0.36511(18) 0.0193(5) Uani 1 1 d . . . . .
H7 H 0.0207 -0.3653 -0.3308 0.023 Uiso 1 1 calc R U . . .
C8 C -0.2598(4) -0.30458(13) -0.31364(17) 0.0194(5) Uani 1 1 d . . . . .
C9 C -0.2247(5) -0.30156(15) -0.21489(18) 0.0253(6) Uani 1 1 d . . . . .
H9 H -0.0996 -0.3249 -0.1816 0.030 Uiso 1 1 calc R U . . .
C10 C -0.3720(5) -0.26482(16) -0.16679(19) 0.0289(6) Uani 1 1 d . . . . .
H10 H -0.3464 -0.2623 -0.1002 0.035 Uiso 1 1 calc R U . . .
C11 C -0.5595(5) -0.23102(16) -0.2146(2) 0.0277(6) Uani 1 1 d . . . . .
H11 H -0.6598 -0.2058 -0.1804 0.033 Uiso 1 1 calc R U . . .
C12 C -0.5983(4) -0.23435(14) -0.31119(19) 0.0226(5) Uani 1 1 d . . . . .
C13 C -0.4466(4) -0.27162(13) -0.36179(17) 0.0189(5) Uani 1 1 d . . . . .
C14 C 0.2488(5) -0.52804(16) -0.3556(2) 0.0291(6) Uani 1 1 d . . . . .
H14A H 0.4050 -0.5260 -0.3676 0.035 Uiso 1 1 calc R U . . .
H14B H 0.1986 -0.5796 -0.3624 0.035 Uiso 1 1 calc R U . . .
C15 C 0.2302(4) -0.50184(14) -0.25768(19) 0.0231(5) Uani 1 1 d . . . . .
C16 C 0.3936(5) -0.45848(17) -0.2087(2) 0.0296(6) Uani 1 1 d . . . . .
H16 H 0.5233 -0.4471 -0.2361 0.036 Uiso 1 1 calc R U . . .
C17 C 0.3680(6) -0.43178(19) -0.1201(2) 0.0374(7) Uani 1 1 d . . . . .
H17 H 0.4805 -0.4023 -0.0872 0.045 Uiso 1 1 calc R U . . .
C18 C 0.1808(6) -0.44778(18) -0.0794(2) 0.0359(7) Uani 1 1 d . . . . .
H18 H 0.1639 -0.4291 -0.0189 0.043 Uiso 1 1 calc R U . . .
C19 C 0.0180(6) -0.49086(19) -0.1267(2) 0.0365(7) Uani 1 1 d . . . . .
H19 H -0.1108 -0.5022 -0.0986 0.044 Uiso 1 1 calc R U . . .
C20 C 0.0419(5) -0.51776(17) -0.2155(2) 0.0312(6) Uani 1 1 d . . . . .
H20 H -0.0712 -0.5473 -0.2478 0.037 Uiso 1 1 calc R U . . .
C21 C 0.1158(4) -0.50060(13) -0.79176(18) 0.0187(5) Uani 1 1 d . . . . .
H21 H 0.1908 -0.4598 -0.8219 0.022 Uiso 1 1 calc R U . . .
C22 C -0.0213(4) -0.54538(13) -0.86647(18) 0.0185(5) Uani 1 1 d . . . . .
C23 C -0.2408(4) -0.52750(15) -0.89593(18) 0.0217(5) Uani 1 1 d . . . . .
H23 H -0.3057 -0.4864 -0.8693 0.026 Uiso 1 1 calc R U . . .
C24 C -0.3650(5) -0.56910(16) -0.96373(19) 0.0259(6) Uani 1 1 d . . . . .
H24 H -0.5144 -0.5563 -0.9837 0.031 Uiso 1 1 calc R U . . .
C25 C -0.2714(5) -0.62961(16) -1.0026(2) 0.0299(6) Uani 1 1 d . . . . .
H25 H -0.3564 -0.6584 -1.0490 0.036 Uiso 1 1 calc R U . . .
C26 C -0.0536(5) -0.64764(16) -0.9730(2) 0.0307(6) Uani 1 1 d . . . . .
H26 H 0.0105 -0.6890 -0.9994 0.037 Uiso 1 1 calc R U . . .
C27 C 0.0723(5) -0.60594(15) -0.90526(18) 0.0239(5) Uani 1 1 d . . . . .
H27 H 0.2217 -0.6187 -0.8855 0.029 Uiso 1 1 calc R U . . .
C28 C -0.7000(5) -0.20302(18) -0.6589(2) 0.0358(7) Uani 1 1 d . . . . .
H28A H -0.7966 -0.2081 -0.7184 0.054 Uiso 1 1 calc R U . . .
H28B H -0.5952 -0.1630 -0.6640 0.054 Uiso 1 1 calc R U . . .
H28C H -0.7893 -0.1921 -0.6084 0.054 Uiso 1 1 calc R U . . .
C29 C -0.9151(5) -0.15639(16) -0.3229(2) 0.0304(6) Uani 1 1 d . . . . .
H29A H -1.0310 -0.1377 -0.3703 0.046 Uiso 1 1 calc R U . . .
H29B H -0.8279 -0.1153 -0.2943 0.046 Uiso 1 1 calc R U . . .
H29C H -0.9827 -0.1829 -0.2744 0.046 Uiso 1 1 calc R U . . .
Cl1 Cl -0.58398(12) -0.31482(5) -0.87318(6) 0.03775(18) Uani 1 1 d . . . . .
Cl2 Cl -0.13882(12) -0.33359(4) -0.91759(6) 0.03646(17) Uani 1 1 d . . . . .
Cl3 Cl -0.25583(12) -0.20333(4) -0.81906(5) 0.03451(16) Uani 1 1 d . . . . .
C1CL C -0.3036(5) -0.29814(15) -0.83476(19) 0.0281(6) Uani 1 1 d . . . . .
H1CL H -0.2627 -0.3235 -0.7733 0.034 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V 0.01605(17) 0.01591(18) 0.01544(18) -0.00022(16) 0.00086(14) 0.00221(15)
O1 0.0243(9) 0.0191(9) 0.0327(10) 0.0027(8) 0.0015(8) 0.0001(8)
O2 0.0195(8) 0.0270(9) 0.0162(8) -0.0047(8) 0.0018(6) 0.0036(8)
O3 0.0211(8) 0.0221(9) 0.0152(8) 0.0001(7) 0.0006(7) 0.0073(7)
O4 0.0198(8) 0.0232(9) 0.0197(8) 0.0012(7) 0.0001(7) 0.0053(7)
O5 0.0262(9) 0.0177(8) 0.0201(9) 0.0023(7) -0.0022(7) 0.0004(7)
O6 0.0170(8) 0.0206(8) 0.0165(8) -0.0037(7) 0.0020(7) 0.0010(7)
O7 0.0164(8) 0.0255(9) 0.0223(9) -0.0070(8) -0.0015(7) 0.0030(7)
O8 0.0187(8) 0.0235(9) 0.0243(9) -0.0073(8) 0.0000(7) 0.0034(7)
O9 0.0263(9) 0.0309(10) 0.0271(10) -0.0100(9) 0.0060(8) 0.0076(8)
N 0.0169(9) 0.0143(9) 0.0176(9) -0.0018(8) 0.0016(8) 0.0000(7)
C1 0.0199(12) 0.0191(11) 0.0185(12) -0.0035(10) -0.0012(10) 0.0005(9)
C2 0.0160(11) 0.0160(11) 0.0169(11) -0.0006(9) 0.0019(9) 0.0010(8)
C3 0.0166(10) 0.0140(10) 0.0152(11) 0.0009(9) 0.0000(9) 0.0035(8)
C4 0.0167(11) 0.0168(11) 0.0174(11) -0.0023(9) 0.0027(9) 0.0001(9)
C5 0.0160(11) 0.0193(11) 0.0196(12) -0.0034(10) -0.0012(9) 0.0010(9)
C6 0.0178(11) 0.0318(14) 0.0265(14) -0.0088(12) -0.0004(10) 0.0031(10)
C7 0.0214(11) 0.0163(11) 0.0194(12) -0.0008(9) -0.0007(9) -0.0028(9)
C8 0.0236(11) 0.0170(11) 0.0175(12) -0.0022(9) 0.0024(9) -0.0034(9)
C9 0.0305(13) 0.0268(13) 0.0180(12) 0.0016(10) -0.0003(11) -0.0035(10)
C10 0.0396(15) 0.0309(15) 0.0164(12) -0.0042(10) 0.0045(11) -0.0061(12)
C11 0.0344(15) 0.0257(13) 0.0247(14) -0.0082(11) 0.0108(12) -0.0053(11)
C12 0.0260(12) 0.0179(11) 0.0250(13) -0.0055(10) 0.0080(11) -0.0036(10)
C13 0.0232(11) 0.0169(12) 0.0167(11) -0.0038(9) 0.0035(9) -0.0038(9)
C14 0.0395(15) 0.0215(13) 0.0247(14) 0.0033(11) -0.0020(12) 0.0094(11)
C15 0.0280(13) 0.0197(12) 0.0208(13) 0.0069(10) -0.0004(11) 0.0047(10)
C16 0.0269(14) 0.0371(16) 0.0239(14) 0.0067(12) -0.0007(11) -0.0044(12)
C17 0.0436(18) 0.0408(17) 0.0255(15) 0.0027(13) -0.0053(13) -0.0094(14)
C18 0.0518(19) 0.0349(16) 0.0216(14) 0.0045(12) 0.0071(13) 0.0067(14)
C19 0.0338(15) 0.0439(18) 0.0335(16) 0.0150(14) 0.0113(13) 0.0016(13)
C20 0.0307(14) 0.0301(15) 0.0309(15) 0.0078(12) -0.0033(12) -0.0068(12)
C21 0.0193(11) 0.0186(11) 0.0191(12) -0.0008(10) 0.0060(9) -0.0003(9)
C22 0.0208(11) 0.0192(12) 0.0163(11) 0.0014(9) 0.0048(9) -0.0022(9)
C23 0.0235(12) 0.0218(12) 0.0204(12) -0.0010(10) 0.0056(10) -0.0003(10)
C24 0.0251(13) 0.0299(14) 0.0220(13) 0.0014(11) 0.0006(11) -0.0052(11)
C25 0.0382(16) 0.0293(14) 0.0210(13) -0.0049(11) -0.0009(12) -0.0089(12)
C26 0.0417(16) 0.0250(14) 0.0258(14) -0.0077(12) 0.0065(12) 0.0019(12)
C27 0.0283(13) 0.0238(12) 0.0199(12) -0.0014(10) 0.0046(11) 0.0021(10)
C28 0.0243(13) 0.0329(15) 0.0487(19) 0.0059(15) -0.0012(13) 0.0108(12)
C29 0.0317(15) 0.0248(14) 0.0375(16) -0.0070(12) 0.0159(13) 0.0031(11)
Cl1 0.0281(3) 0.0429(4) 0.0410(4) 0.0014(3) -0.0010(3) -0.0129(3)
Cl2 0.0357(4) 0.0344(4) 0.0399(4) 0.0084(3) 0.0073(3) 0.0004(3)
Cl3 0.0340(4) 0.0345(4) 0.0329(4) 0.0004(3) -0.0043(3) -0.0097(3)
C1CL 0.0290(13) 0.0321(16) 0.0214(12) 0.0082(11) -0.0045(10) -0.0057(11)

_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
V O1 1.5875(19) . ?
V O2 1.8473(16) . ?
V O3 1.8428(17) . ?
V O4 1.7815(18) . ?
V N 2.157(2) . ?
O2 C13 1.331(3) . ?
O3 C3 1.412(3) . ?
O4 C28 1.418(3) . ?
O5 C1 1.398(3) . ?
O5 C14 1.451(3) . ?
O6 C4 1.427(3) . ?
O6 C21 1.423(3) . ?
O7 C1 1.436(3) . ?
O7 C5 1.437(3) . ?
O8 C6 1.433(3) . ?
O8 C21 1.410(3) . ?
O9 C12 1.361(3) . ?
O9 C29 1.435(3) . ?
N C2 1.469(3) . ?
N C7 1.285(3) . ?
C1 H1 1.0000 . ?
C1 C2 1.522(3) . ?
C2 H2 1.0000 . ?
C2 C3 1.522(3) . ?
C3 H3 1.0000 . ?
C3 C4 1.512(3) . ?
C4 H4 1.0000 . ?
C4 C5 1.525(3) . ?
C5 H5 1.0000 . ?
C5 C6 1.516(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.451(3) . ?
C8 C9 1.408(3) . ?
C8 C13 1.394(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.402(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(4) . ?
C12 C13 1.419(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.503(4) . ?
C15 C16 1.393(4) . ?
C15 C20 1.395(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.390(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.378(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.377(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.390(5) . ?
C20 H20 0.9500 . ?
C21 H21 1.0000 . ?
C21 C22 1.515(4) . ?
C22 C23 1.392(4) . ?
C22 C27 1.391(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.384(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.391(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.384(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.389(4) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
Cl1 C1CL 1.758(3) . ?
Cl2 C1CL 1.772(3) . ?
Cl3 C1CL 1.763(3) . ?
C1CL H1CL 1.0000 . ?

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 V O2 105.27(9) . . ?
O1 V O3 109.34(9) . . ?
O1 V O4 105.36(9) . . ?
O1 V N 96.56(9) . . ?
O2 V N 81.46(8) . . ?
O3 V O2 141.47(8) . . ?
O3 V N 78.31(8) . . ?
O4 V O2 92.78(8) . . ?
O4 V O3 93.95(8) . . ?
O4 V N 158.08(8) . . ?
C13 O2 V 136.54(15) . . ?
C3 O3 V 121.77(14) . . ?
C28 O4 V 126.88(18) . . ?
C1 O5 C14 113.8(2) . . ?
C21 O6 C4 110.83(18) . . ?
C1 O7 C5 111.26(18) . . ?
C21 O8 C6 112.79(19) . . ?
C12 O9 C29 117.4(2) . . ?
C2 N V 107.57(15) . . ?
C7 N V 129.97(17) . . ?
C7 N C2 122.4(2) . . ?
O5 C1 O7 112.0(2) . . ?
O5 C1 H1 109.6 . . ?
O5 C1 C2 108.6(2) . . ?
O7 C1 H1 109.6 . . ?
O7 C1 C2 107.4(2) . . ?
C2 C1 H1 109.6 . . ?
N C2 C1 120.2(2) . . ?
N C2 H2 106.9 . . ?
N C2 C3 103.13(18) . . ?
C1 C2 H2 106.9 . . ?
C1 C2 C3 112.1(2) . . ?
C3 C2 H2 106.9 . . ?
O3 C3 C2 106.40(19) . . ?
O3 C3 H3 109.5 . . ?
O3 C3 C4 113.79(19) . . ?
C2 C3 H3 109.5 . . ?
C4 C3 C2 108.04(19) . . ?
C4 C3 H3 109.5 . . ?
O6 C4 C3 109.45(19) . . ?
O6 C4 H4 110.2 . . ?
O6 C4 C5 108.55(19) . . ?
C3 C4 H4 110.2 . . ?
C3 C4 C5 108.2(2) . . ?
C5 C4 H4 110.2 . . ?
O7 C5 C4 111.37(19) . . ?
O7 C5 H5 108.8 . . ?
O7 C5 C6 110.95(19) . . ?
C4 C5 H5 108.8 . . ?
C6 C5 C4 108.2(2) . . ?
C6 C5 H5 108.8 . . ?
O8 C6 C5 106.9(2) . . ?
O8 C6 H6A 110.3 . . ?
O8 C6 H6B 110.3 . . ?
C5 C6 H6A 110.3 . . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.6 . . ?
N C7 H7 118.5 . . ?
N C7 C8 123.1(2) . . ?
C8 C7 H7 118.5 . . ?
C9 C8 C7 120.1(2) . . ?
C13 C8 C7 120.2(2) . . ?
C13 C8 C9 119.6(2) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.9(3) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 H10 119.5 . . ?
C9 C10 C11 120.9(2) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 H11 120.0 . . ?
O9 C12 C11 126.4(2) . . ?
O9 C12 C13 113.9(2) . . ?
C11 C12 C13 119.6(3) . . ?
O2 C13 C8 123.0(2) . . ?
O2 C13 C12 117.1(2) . . ?
C8 C13 C12 119.9(2) . . ?
O5 C14 H14A 109.6 . . ?
O5 C14 H14B 109.6 . . ?
O5 C14 C15 110.1(2) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.6 . . ?
C15 C14 H14B 109.6 . . ?
C16 C15 C14 121.3(3) . . ?
C16 C15 C20 118.4(3) . . ?
C20 C15 C14 120.2(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.5(3) . . ?
C18 C17 H17 119.8 . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.9(3) . . ?
C19 C18 H18 120.1 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.1(3) . . ?
C20 C19 H19 119.9 . . ?
C15 C20 H20 119.6 . . ?
C19 C20 C15 120.7(3) . . ?
C19 C20 H20 119.6 . . ?
O6 C21 H21 109.7 . . ?
O6 C21 C22 107.33(19) . . ?
O8 C21 O6 112.0(2) . . ?
O8 C21 H21 109.7 . . ?
O8 C21 C22 108.3(2) . . ?
C22 C21 H21 109.7 . . ?
C23 C22 C21 121.0(2) . . ?
C27 C22 C21 119.5(2) . . ?
C27 C22 C23 119.5(2) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.5(3) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 120.0(3) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.2 . . ?
C26 C25 C24 119.5(3) . . ?
C26 C25 H25 120.2 . . ?
C25 C26 H26 119.6 . . ?
C25 C26 C27 120.8(3) . . ?
C27 C26 H26 119.6 . . ?
C22 C27 H27 120.1 . . ?
C26 C27 C22 119.7(3) . . ?
C26 C27 H27 120.1 . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O9 C29 H29A 109.5 . . ?
O9 C29 H29B 109.5 . . ?
O9 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Cl1 C1CL Cl2 109.75(16) . . ?
Cl1 C1CL Cl3 110.41(15) . . ?
Cl1 C1CL H1CL 108.8 . . ?
Cl2 C1CL H1CL 108.8 . . ?
Cl3 C1CL Cl2 110.19(14) . . ?
Cl3 C1CL H1CL 108.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1CL H1CL O3 1.00 2.09 3.061(3) 163.4 .

_database_code_depnum_ccdc_archive 'CCDC 927424'
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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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data_fo4351
_audit_creation_date             2013-05-12
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C29 H31 Br N O9 V, 2(C H4 O)'
_chemical_formula_sum            'C31 H39 Br N O11 V'
_chemical_formula_weight         732.48
_chemical_absolute_configuration syn
_chemical_melting_point          ?
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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.5230(3)
_cell_length_b                   11.3226(2)
_cell_length_c                   28.4192(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3386.08(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20740
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.461
_diffrn_reflns_theta_min         2.738
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                5892
_reflns_number_total             7706
_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.
;
_reflns_threshold_expression     'I > 2\s(I)'
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 
;
 Flack x determined using 1971 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.033(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7706
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0552
_refine_ls_restrained_S_all      1.200
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+2.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0949
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H1(0.055) H2(0.048) H3(0.05) H4(0.049) H5(0.051) H6A(0.065)
 H6B(0.065) H7(0.053) H9(0.06) H11(0.062) H12(0.061) H14A(0.084) H14B(0.084)
 H16(0.087) H17(0.114) H18(0.107) H19(0.104) H20(0.087) H21(0.055) H23(0.074)
 H24(0.091) H25(0.086) H26(0.087) H27(0.07) H28A(0.12) H28B(0.12) H28C(0.12)
 H1M(0.082) H1MA(0.147) H1MB(0.147) H1MC(0.147) H2M(0.204) H2MA(0.172)
 H2MB(0.172) H2MC(0.172) H3MA(0.155) H3MB(0.229) H3MC(0.229) H3MD(0.229)
 H3ME(0.168) H3MF(0.122) H3MG(0.122) H3MH(0.122)
 Fixed X: H1(-0.4505) H2(-0.3766) H3(-0.318) H4(-0.504) H5(-0.543) H6A(-0.729)
 H6B(-0.7615) H7(-0.2426) H9(-0.0843) H11(0.28) H12(0.2361) H14A(-0.4914) H14B(-
 0.5633) H16(-0.2422) H17(-0.1442) H18(-0.2627) H19(-0.4753) H20(-0.5724) H21(-
 0.6335) H23(-0.8035) H24(-0.8149) H25(-0.6331) H26(-0.4405) H27(-0.4268)
 H28A(0.0999) H28B(0.0656) H28C(-0.0314) H1M(-0.1537) H1MA(-0.1801) H1MB(-
 0.1374) H1MC(-0.0397) H2M(-0.2951) H2MA(-0.4305) H2MB(-0.3272) H2MC(-0.3039)
 H3MA(-0.2361) H3MB(-0.1497) H3MC(-0.1203) H3MD(-0.0499) H3ME(-0.1894) H3MF(-
 0.2288) H3MG(-0.1641) H3MH(-0.2925)
 Fixed Y: H1(0.2523) H2(0.23) H3(0.475) H4(0.3495) H5(0.5101) H6A(0.3846)
 H6B(0.4698) H7(0.2543) H9(0.2523) H11(0.1945) H12(0.1963) H14A(0.3678)
 H14B(0.4702) H16(0.5202) H17(0.6487) H18(0.7369) H19(0.698) H20(0.5716)
 H21(0.4668) H23(0.6398) H24(0.8105) H25(0.9154) H26(0.8498) H27(0.6807)
 H28A(0.3903) H28B(0.4771) H28C(0.4557) H1M(0.1399) H1MA(-0.0319) H1MB(0.0263)
 H1MC(0.0117) H2M(0.3553) H2MA(0.4294) H2MB(0.4156) H2MC(0.502) H3MA(0.1903)
 H3MB(0.0957) H3MC(-0.0065) H3MD(0.115) H3ME(0.1907) H3MF(-0.0191) H3MG(0.0328)
 H3MH(0.0862)
 Fixed Z: H1(0.2795) H2(0.2029) H3(0.2005) H4(0.1483) H5(0.2241) H6A(0.1708)
 H6B(0.2129) H7(0.2984) H9(0.3583) H11(0.3288) H12(0.2494) H14A(0.3435)
 H14B(0.3174) H16(0.33) H17(0.3819) H18(0.44) H19(0.4464) H20(0.3936)
 H21(0.1007) H23(0.0768) H24(0.0316) H25(0.0154) H26(0.0419) H27(0.0873)
 H28A(0.0736) H28B(0.1146) H28C(0.0737) H1M(0.1225) H1MA(0.1547) H1MB(0.2022)
 H1MC(0.161) H2M(0.0854) H2MA(0.0396) H2MB(0.0003) H2MC(0.0425) H3MA(0.0556)
 H3MB(-0.0025) H3MC(0.0331) H3MD(0.0377) H3ME(0.0554) H3MF(0.0399) H3MG(-
 0.0052) H3MH(0.013)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
V V -0.09160(9) 0.32624(8) 0.17513(3) 0.0444(2) Uani 1 1 d . . . . .
Br Br 0.13857(7) 0.22827(7) 0.41615(2) 0.0755(2) Uani 1 1 d . . . . .
O1 O -0.0486(4) 0.4488(3) 0.19696(15) 0.0560(11) Uani 1 1 d . . . . .
O2 O 0.0226(4) 0.2299(3) 0.20910(13) 0.0503(9) Uani 1 1 d . . . . .
O3 O -0.2547(4) 0.3710(3) 0.15070(13) 0.0476(9) Uani 1 1 d . . . . .
O4 O -0.0217(4) 0.3257(4) 0.11842(13) 0.0549(10) Uani 1 1 d . . . . .
O5 O -0.4064(4) 0.4198(3) 0.28535(12) 0.0477(9) Uani 1 1 d . . . . .
O6 O -0.4846(4) 0.5219(3) 0.13626(13) 0.0452(9) Uani 1 1 d . . . . .
O7 O -0.5679(3) 0.3396(3) 0.23826(13) 0.0483(9) Uani 1 1 d . . . . .
O8 O -0.6970(4) 0.5549(3) 0.15602(14) 0.0524(10) Uani 1 1 d . . . . .
N N -0.2162(4) 0.2844(4) 0.23321(15) 0.0433(11) Uani 1 1 d . . . . .
C1 C -0.4472(5) 0.3219(5) 0.25906(19) 0.0455(13) Uani 1 1 d . . . . .
H1 H -0.4505 0.2523 0.2795 0.055 Uiso 1 1 calc R U . . .
C2 C -0.3499(5) 0.3009(4) 0.22008(17) 0.0403(12) Uani 1 1 d . . . . .
H2 H -0.3766 0.2300 0.2029 0.048 Uiso 1 1 calc R U . . .
C3 C -0.3456(5) 0.4027(4) 0.18452(18) 0.0416(12) Uani 1 1 d . . . . .
H3 H -0.3180 0.4750 0.2005 0.050 Uiso 1 1 calc R U . . .
C4 C -0.4780(5) 0.4196(5) 0.16605(18) 0.0410(13) Uani 1 1 d . . . . .
H4 H -0.5040 0.3495 0.1483 0.049 Uiso 1 1 calc R U . . .
C5 C -0.5682(5) 0.4388(5) 0.20682(18) 0.0429(13) Uani 1 1 d . . . . .
H5 H -0.5430 0.5101 0.2241 0.051 Uiso 1 1 calc R U . . .
C6 C -0.7020(6) 0.4549(6) 0.1875(2) 0.0544(16) Uani 1 1 d . . . . .
H6A H -0.7290 0.3846 0.1708 0.065 Uiso 1 1 calc R U . . .
H6B H -0.7615 0.4698 0.2129 0.065 Uiso 1 1 calc R U . . .
C7 C -0.1807(5) 0.2613(5) 0.27518(18) 0.0444(13) Uani 1 1 d . . . . .
H7 H -0.2426 0.2543 0.2984 0.053 Uiso 1 1 calc R U . . .
C8 C -0.0496(5) 0.2455(5) 0.28855(19) 0.0439(13) Uani 1 1 d . . . . .
C9 C -0.0200(5) 0.2423(5) 0.33619(19) 0.0496(14) Uani 1 1 d . . . . .
H9 H -0.0843 0.2523 0.3583 0.060 Uiso 1 1 calc R U . . .
C10 C 0.1015(6) 0.2249(5) 0.3510(2) 0.0523(14) Uani 1 1 d . . . . .
C11 C 0.1972(5) 0.2074(5) 0.3185(2) 0.0518(15) Uani 1 1 d . . . . .
H11 H 0.2800 0.1945 0.3288 0.062 Uiso 1 1 calc R U . . .
C12 C 0.1710(5) 0.2090(5) 0.2709(2) 0.0509(14) Uani 1 1 d . . . . .
H12 H 0.2361 0.1963 0.2494 0.061 Uiso 1 1 calc R U . . .
C13 C 0.0460(5) 0.2297(5) 0.2548(2) 0.0466(13) Uani 1 1 d . . . . .
C14 C -0.4800(6) 0.4410(6) 0.3263(2) 0.0700(19) Uani 1 1 d . . . . .
H14A H -0.4914 0.3678 0.3435 0.084 Uiso 1 1 calc R U . . .
H14B H -0.5633 0.4702 0.3174 0.084 Uiso 1 1 calc R U . . .
C15 C -0.4151(7) 0.5300(5) 0.3573(2) 0.0543(15) Uani 1 1 d . . . . .
C16 C -0.2898(7) 0.5554(7) 0.3537(2) 0.072(2) Uani 1 1 d . . . . .
H16 H -0.2422 0.5202 0.3300 0.087 Uiso 1 1 calc R U . . .
C17 C -0.2306(9) 0.6328(8) 0.3846(3) 0.095(3) Uani 1 1 d . . . . .
H17 H -0.1442 0.6487 0.3819 0.114 Uiso 1 1 calc R U . . .
C18 C -0.3013(10) 0.6851(7) 0.4190(3) 0.089(2) Uani 1 1 d . . . . .
H18 H -0.2627 0.7369 0.4400 0.107 Uiso 1 1 calc R U . . .
C19 C -0.4277(10) 0.6622(7) 0.4228(3) 0.087(2) Uani 1 1 d . . . . .
H19 H -0.4753 0.6980 0.4464 0.104 Uiso 1 1 calc R U . . .
C20 C -0.4855(8) 0.5856(6) 0.3915(2) 0.073(2) Uani 1 1 d . . . . .
H20 H -0.5724 0.5716 0.3936 0.087 Uiso 1 1 calc R U . . .
C21 C -0.6088(5) 0.5367(5) 0.11886(19) 0.0462(13) Uani 1 1 d . . . . .
H21 H -0.6335 0.4668 0.1007 0.055 Uiso 1 1 calc R U . . .
C22 C -0.6141(5) 0.6443(5) 0.08795(19) 0.0469(13) Uani 1 1 d . . . . .
C23 C -0.7300(6) 0.6825(6) 0.0704(2) 0.0621(17) Uani 1 1 d . . . . .
H23 H -0.8035 0.6398 0.0768 0.074 Uiso 1 1 calc R U . . .
C24 C -0.7369(8) 0.7846(7) 0.0431(2) 0.075(2) Uani 1 1 d . . . . .
H24 H -0.8149 0.8105 0.0316 0.091 Uiso 1 1 calc R U . . .
C25 C -0.6285(8) 0.8466(6) 0.0332(2) 0.072(2) Uani 1 1 d . . . . .
H25 H -0.6331 0.9154 0.0154 0.086 Uiso 1 1 calc R U . . .
C26 C -0.5138(8) 0.8079(6) 0.0493(2) 0.072(2) Uani 1 1 d . . . . .
H26 H -0.4405 0.8498 0.0419 0.087 Uiso 1 1 calc R U . . .
C27 C -0.5055(6) 0.7066(5) 0.0766(2) 0.0585(16) Uani 1 1 d . . . . .
H27 H -0.4268 0.6807 0.0873 0.070 Uiso 1 1 calc R U . . .
C28 C 0.0324(7) 0.4196(6) 0.0931(3) 0.080(2) Uani 1 1 d . . . . .
H28A H 0.0999 0.3903 0.0736 0.120 Uiso 1 1 calc R U . . .
H28B H 0.0656 0.4771 0.1146 0.120 Uiso 1 1 calc R U . . .
H28C H -0.0314 0.4557 0.0737 0.120 Uiso 1 1 calc R U . . .
O1M O -0.1614(5) 0.1393(3) 0.15118(15) 0.0685(13) Uani 1 1 d . . . . .
H1M H -0.1537 0.1399 0.1225 0.082 Uiso 1 1 calc R U . . .
C1M C -0.1269(9) 0.0275(5) 0.1687(3) 0.098(3) Uani 1 1 d . . . . .
H1MA H -0.1801 -0.0319 0.1547 0.147 Uiso 1 1 calc R U . . .
H1MB H -0.1374 0.0263 0.2022 0.147 Uiso 1 1 calc R U . . .
H1MC H -0.0397 0.0117 0.1610 0.147 Uiso 1 1 calc R U . . .
O2M O -0.2878(9) 0.3422(7) 0.0571(2) 0.136(3) Uani 1 1 d . . . . .
H2M H -0.2951 0.3553 0.0854 0.204 Uiso 1 1 calc R U . . .
C2M C -0.3409(12) 0.4280(8) 0.0333(3) 0.115(4) Uani 1 1 d . . . . .
H2MA H -0.4305 0.4294 0.0396 0.172 Uiso 1 1 calc R U . . .
H2MB H -0.3272 0.4156 0.0003 0.172 Uiso 1 1 calc R U . . .
H2MC H -0.3039 0.5020 0.0425 0.172 Uiso 1 1 calc R U . . .
O3MA O -0.226(3) 0.1192(15) 0.0596(6) 0.104(6) Uani 0.65(6) 1 d . . P A 1
H3MA H -0.2361 0.1903 0.0556 0.155 Uiso 0.65(6) 1 calc R U P A 1
C3MA C -0.129(5) 0.078(4) 0.0296(12) 0.15(2) Uani 0.65(6) 1 d . . P A 1
H3MB H -0.1497 0.0957 -0.0025 0.229 Uiso 0.65(6) 1 calc R U P A 1
H3MC H -0.1203 -0.0065 0.0331 0.229 Uiso 0.65(6) 1 calc R U P A 1
H3MD H -0.0499 0.1150 0.0377 0.229 Uiso 0.65(6) 1 calc R U P A 1
O3MB O -0.145(7) 0.132(3) 0.0504(14) 0.112(18) Uani 0.35(6) 1 d . . P A 2
H3ME H -0.1894 0.1907 0.0554 0.168 Uiso 0.35(6) 1 calc R U P A 2
C3MB C -0.213(6) 0.052(3) 0.0223(12) 0.082(12) Uani 0.35(6) 1 d . . P A 2
H3MF H -0.2288 -0.0191 0.0399 0.122 Uiso 0.35(6) 1 calc R U P A 2
H3MG H -0.1641 0.0328 -0.0052 0.122 Uiso 0.35(6) 1 calc R U P A 2
H3MH H -0.2925 0.0862 0.0130 0.122 Uiso 0.35(6) 1 calc R U P A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V 0.0384(5) 0.0428(5) 0.0521(5) 0.0066(4) 0.0056(5) 0.0051(4)
Br 0.0701(5) 0.0896(5) 0.0667(4) 0.0043(4) -0.0209(4) 0.0061(4)
O1 0.053(3) 0.044(2) 0.072(3) 0.0022(19) 0.000(2) -0.0008(19)
O2 0.045(2) 0.050(2) 0.056(2) 0.0077(19) 0.0025(18) 0.0095(18)
O3 0.041(2) 0.054(2) 0.048(2) 0.0042(18) 0.0050(18) 0.0090(18)
O4 0.046(2) 0.060(2) 0.059(2) 0.011(2) 0.011(2) 0.009(2)
O5 0.041(2) 0.060(2) 0.042(2) 0.0022(17) 0.0044(18) -0.006(2)
O6 0.039(2) 0.050(2) 0.047(2) 0.0071(17) -0.0011(17) 0.0056(17)
O7 0.034(2) 0.056(2) 0.055(2) 0.0114(19) -0.0007(17) -0.0058(18)
O8 0.042(2) 0.064(3) 0.051(2) 0.0080(19) 0.0021(19) 0.0129(19)
N 0.042(3) 0.037(2) 0.051(3) 0.008(2) 0.002(2) 0.003(2)
C1 0.039(3) 0.048(3) 0.049(3) 0.009(3) -0.001(2) -0.002(3)
C2 0.033(3) 0.040(3) 0.049(3) 0.005(2) -0.002(2) -0.001(2)
C3 0.040(3) 0.039(3) 0.045(3) 0.002(2) -0.001(3) 0.000(2)
C4 0.037(3) 0.042(3) 0.044(3) 0.004(2) 0.001(2) 0.004(2)
C5 0.037(3) 0.048(3) 0.044(3) 0.005(2) -0.001(2) 0.001(2)
C6 0.039(3) 0.071(4) 0.054(4) 0.008(3) -0.002(3) 0.000(3)
C7 0.040(3) 0.043(3) 0.050(3) 0.011(3) 0.004(2) -0.001(3)
C8 0.037(3) 0.037(3) 0.058(3) 0.010(2) 0.003(2) 0.001(2)
C9 0.045(3) 0.051(3) 0.053(3) 0.012(3) 0.004(3) 0.005(3)
C10 0.054(4) 0.044(3) 0.059(3) 0.006(3) -0.012(3) -0.005(3)
C11 0.039(3) 0.046(3) 0.071(4) 0.005(3) -0.011(3) 0.001(3)
C12 0.038(3) 0.045(3) 0.069(4) 0.004(3) 0.005(3) 0.004(3)
C13 0.046(3) 0.032(3) 0.062(4) 0.010(3) -0.004(3) 0.002(2)
C14 0.054(4) 0.100(5) 0.056(4) -0.005(4) 0.013(4) -0.014(4)
C15 0.055(4) 0.063(4) 0.045(3) 0.005(3) 0.004(3) -0.001(3)
C16 0.067(5) 0.088(5) 0.062(4) -0.007(4) 0.007(4) -0.011(4)
C17 0.096(7) 0.095(6) 0.094(6) -0.014(5) -0.005(5) -0.021(5)
C18 0.130(8) 0.059(4) 0.079(5) -0.003(4) -0.008(6) -0.004(5)
C19 0.125(8) 0.070(5) 0.065(5) -0.006(4) 0.013(5) 0.016(5)
C20 0.066(5) 0.080(5) 0.072(5) -0.003(4) 0.010(4) 0.009(4)
C21 0.041(3) 0.050(3) 0.047(3) -0.004(3) -0.004(3) 0.006(3)
C22 0.049(4) 0.050(3) 0.042(3) -0.004(2) -0.001(3) 0.010(3)
C23 0.053(4) 0.072(4) 0.061(4) 0.005(3) -0.005(3) 0.014(3)
C24 0.075(5) 0.083(5) 0.069(4) 0.009(4) -0.014(4) 0.028(4)
C25 0.092(6) 0.063(4) 0.061(4) 0.010(3) -0.005(4) 0.018(4)
C26 0.078(5) 0.069(5) 0.069(4) 0.015(4) 0.003(4) -0.004(4)
C27 0.053(4) 0.063(4) 0.059(4) 0.004(3) -0.003(3) 0.006(3)
C28 0.074(5) 0.091(5) 0.075(5) 0.027(4) 0.015(4) 0.001(4)
O1M 0.090(4) 0.044(2) 0.072(3) -0.001(2) -0.005(3) 0.006(2)
C1M 0.109(7) 0.043(4) 0.142(8) 0.017(4) -0.017(6) 0.001(4)
O2M 0.184(7) 0.144(6) 0.079(4) -0.031(4) -0.033(5) 0.081(5)
C2M 0.180(11) 0.095(6) 0.069(5) 0.011(5) 0.021(7) 0.014(7)
O3MA 0.114(15) 0.125(10) 0.072(8) -0.014(6) 0.017(8) 0.012(10)
C3MA 0.15(4) 0.17(3) 0.13(2) 0.01(2) 0.06(3) 0.06(4)
O3MB 0.16(5) 0.077(17) 0.10(2) -0.011(12) 0.01(3) 0.03(2)
C3MB 0.09(3) 0.086(18) 0.069(18) 0.006(13) 0.006(18) -0.005(18)

_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
V O1 1.586(4) . ?
V O2 1.888(4) . ?
V O3 1.919(4) . ?
V O4 1.772(4) . ?
V N 2.161(4) . ?
V O1M 2.342(4) . ?
Br C10 1.893(5) . ?
O2 C13 1.322(6) . ?
O3 C3 1.403(6) . ?
O4 C28 1.405(7) . ?
O5 C1 1.404(6) . ?
O5 C14 1.420(7) . ?
O6 C4 1.437(6) . ?
O6 C21 1.407(6) . ?
O7 C1 1.416(6) . ?
O7 C5 1.435(6) . ?
O8 C6 1.445(7) . ?
O8 C21 1.421(6) . ?
N C2 1.468(6) . ?
N C7 1.277(6) . ?
C1 H1 0.9800 . ?
C1 C2 1.527(7) . ?
C2 H2 0.9800 . ?
C2 C3 1.534(7) . ?
C3 H3 0.9800 . ?
C3 C4 1.502(7) . ?
C4 H4 0.9800 . ?
C4 C5 1.514(7) . ?
C5 H5 0.9800 . ?
C5 C6 1.522(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7 0.9300 . ?
C7 C8 1.441(7) . ?
C8 C9 1.390(7) . ?
C8 C13 1.402(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.361(8) . ?
C10 C11 1.380(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.380(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.413(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.501(9) . ?
C15 C16 1.353(9) . ?
C15 C20 1.375(9) . ?
C16 H16 0.9300 . ?
C16 C17 1.389(10) . ?
C17 H17 0.9300 . ?
C17 C18 1.364(11) . ?
C18 H18 0.9300 . ?
C18 C19 1.360(11) . ?
C19 H19 0.9300 . ?
C19 C20 1.384(10) . ?
C20 H20 0.9300 . ?
C21 H21 0.9800 . ?
C21 C22 1.504(7) . ?
C22 C23 1.388(8) . ?
C22 C27 1.381(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.394(9) . ?
C24 H24 0.9300 . ?
C24 C25 1.369(10) . ?
C25 H25 0.9300 . ?
C25 C26 1.362(10) . ?
C26 H26 0.9300 . ?
C26 C27 1.388(8) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
O1M H1M 0.8200 . ?
O1M C1M 1.408(7) . ?
C1M H1MA 0.9600 . ?
C1M H1MB 0.9600 . ?
C1M H1MC 0.9600 . ?
O2M H2M 0.8200 . ?
O2M C2M 1.310(9) . ?
C2M H2MA 0.9600 . ?
C2M H2MB 0.9600 . ?
C2M H2MC 0.9600 . ?
O3MA H3MA 0.8200 . ?
O3MA C3MA 1.42(5) . ?
C3MA H3MB 0.9600 . ?
C3MA H3MC 0.9600 . ?
C3MA H3MD 0.9600 . ?
O3MB H3ME 0.8200 . ?
O3MB C3MB 1.41(7) . ?
C3MB H3MF 0.9600 . ?
C3MB H3MG 0.9600 . ?
C3MB H3MH 0.9600 . ?

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 V O2 97.1(2) . . ?
O1 V O3 99.54(19) . . ?
O1 V O4 103.9(2) . . ?
O1 V N 93.80(19) . . ?
O1 V O1M 173.79(19) . . ?
O2 V O3 155.01(17) . . ?
O2 V N 82.46(16) . . ?
O2 V O1M 79.99(17) . . ?
O3 V N 77.98(16) . . ?
O3 V O1M 81.53(17) . . ?
O4 V O2 101.46(17) . . ?
O4 V O3 92.48(17) . . ?
O4 V N 161.11(19) . . ?
O4 V O1M 82.10(18) . . ?
N V O1M 80.40(17) . . ?
C13 O2 V 128.5(4) . . ?
C3 O3 V 115.4(3) . . ?
C28 O4 V 129.2(4) . . ?
C1 O5 C14 113.8(4) . . ?
C21 O6 C4 110.3(4) . . ?
C1 O7 C5 111.9(4) . . ?
C21 O8 C6 111.8(4) . . ?
C2 N V 111.1(3) . . ?
C7 N V 125.5(4) . . ?
C7 N C2 123.0(4) . . ?
O5 C1 O7 112.6(4) . . ?
O5 C1 H1 109.3 . . ?
O5 C1 C2 107.7(4) . . ?
O7 C1 H1 109.3 . . ?
O7 C1 C2 108.7(4) . . ?
C2 C1 H1 109.3 . . ?
N C2 C1 118.5(4) . . ?
N C2 H2 107.2 . . ?
N C2 C3 103.6(4) . . ?
C1 C2 H2 107.2 . . ?
C1 C2 C3 112.4(4) . . ?
C3 C2 H2 107.2 . . ?
O3 C3 C2 106.2(4) . . ?
O3 C3 H3 109.3 . . ?
O3 C3 C4 115.2(4) . . ?
C2 C3 H3 109.3 . . ?
C4 C3 C2 107.3(4) . . ?
C4 C3 H3 109.3 . . ?
O6 C4 C3 110.7(4) . . ?
O6 C4 H4 109.7 . . ?
O6 C4 C5 107.7(4) . . ?
C3 C4 H4 109.7 . . ?
C3 C4 C5 109.4(4) . . ?
C5 C4 H4 109.7 . . ?
O7 C5 C4 111.2(4) . . ?
O7 C5 H5 109.4 . . ?
O7 C5 C6 108.6(4) . . ?
C4 C5 H5 109.4 . . ?
C4 C5 C6 108.8(5) . . ?
C6 C5 H5 109.4 . . ?
O8 C6 C5 106.4(5) . . ?
O8 C6 H6A 110.4 . . ?
O8 C6 H6B 110.4 . . ?
C5 C6 H6A 110.4 . . ?
C5 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
N C7 H7 118.3 . . ?
N C7 C8 123.5(5) . . ?
C8 C7 H7 118.3 . . ?
C9 C8 C7 118.3(5) . . ?
C9 C8 C13 120.2(5) . . ?
C13 C8 C7 121.5(5) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 C8 121.0(5) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 Br 119.5(5) . . ?
C9 C10 C11 120.0(5) . . ?
C11 C10 Br 120.5(4) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 C10 120.5(5) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.4(5) . . ?
C13 C12 H12 119.8 . . ?
O2 C13 C8 122.5(5) . . ?
O2 C13 C12 119.6(5) . . ?
C8 C13 C12 117.8(5) . . ?
O5 C14 H14A 109.6 . . ?
O5 C14 H14B 109.6 . . ?
O5 C14 C15 110.2(5) . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 H14A 109.6 . . ?
C15 C14 H14B 109.6 . . ?
C16 C15 C14 122.8(6) . . ?
C16 C15 C20 118.7(7) . . ?
C20 C15 C14 118.4(6) . . ?
C15 C16 H16 119.2 . . ?
C15 C16 C17 121.6(8) . . ?
C17 C16 H16 119.2 . . ?
C16 C17 H17 120.6 . . ?
C18 C17 C16 118.8(9) . . ?
C18 C17 H17 120.6 . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.6(9) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.8(8) . . ?
C20 C19 H19 120.1 . . ?
C15 C20 C19 120.4(8) . . ?
C15 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
O6 C21 O8 111.3(4) . . ?
O6 C21 H21 109.6 . . ?
O6 C21 C22 109.6(5) . . ?
O8 C21 H21 109.6 . . ?
O8 C21 C22 107.0(4) . . ?
C22 C21 H21 109.6 . . ?
C23 C22 C21 119.7(5) . . ?
C27 C22 C21 121.3(5) . . ?
C27 C22 C23 119.0(5) . . ?
C22 C23 H23 119.9 . . ?
C22 C23 C24 120.3(6) . . ?
C24 C23 H23 119.9 . . ?
C23 C24 H24 120.1 . . ?
C25 C24 C23 119.7(7) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 119.8 . . ?
C26 C25 C24 120.3(6) . . ?
C26 C25 H25 119.8 . . ?
C25 C26 H26 119.7 . . ?
C25 C26 C27 120.6(7) . . ?
C27 C26 H26 119.7 . . ?
C22 C27 C26 120.1(6) . . ?
C22 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
V O1M H1M 104.5 . . ?
C1M O1M V 129.0(4) . . ?
C1M O1M H1M 109.5 . . ?
O1M C1M H1MA 109.5 . . ?
O1M C1M H1MB 109.5 . . ?
O1M C1M H1MC 109.5 . . ?
H1MA C1M H1MB 109.5 . . ?
H1MA C1M H1MC 109.5 . . ?
H1MB C1M H1MC 109.5 . . ?
C2M O2M H2M 109.5 . . ?
O2M C2M H2MA 109.5 . . ?
O2M C2M H2MB 109.5 . . ?
O2M C2M H2MC 109.5 . . ?
H2MA C2M H2MB 109.5 . . ?
H2MA C2M H2MC 109.5 . . ?
H2MB C2M H2MC 109.5 . . ?
C3MA O3MA H3MA 109.5 . . ?
O3MA C3MA H3MB 109.5 . . ?
O3MA C3MA H3MC 109.5 . . ?
O3MA C3MA H3MD 109.5 . . ?
H3MB C3MA H3MC 109.5 . . ?
H3MB C3MA H3MD 109.5 . . ?
H3MC C3MA H3MD 109.5 . . ?
C3MB O3MB H3ME 109.5 . . ?
O3MB C3MB H3MF 109.5 . . ?
O3MB C3MB H3MG 109.5 . . ?
O3MB C3MB H3MH 109.5 . . ?
H3MF C3MB H3MG 109.5 . . ?
H3MF C3MB H3MH 109.5 . . ?
H3MG C3MB H3MH 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1M H1M O3MA 0.82 1.96 2.699(17) 150.3 .
O1M H1M O3MB 0.82 2.05 2.87(4) 175.7 .
O2M H2M O3 0.82 1.91 2.701(7) 161.2 .
O3MA H3MA O2M 0.82 1.80 2.608(18) 166.0 .
O3MB H3ME O2M 0.82 2.00 2.82(4) 170.5 .

_database_code_depnum_ccdc_archive 'CCDC 927425'