data_4000200 _journal_name_full 'Chemistry of Materials' _journal_year 2002 _chemical_formula_sum 'C21 H25 Br6 O16 V3' _chemical_formula_weight 1165.69 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.967(2) _cell_length_b 12.126(2) _cell_length_c 17.378(3) _cell_angle_alpha 107.372(4) _cell_angle_beta 98.015(4) _cell_angle_gamma 99.125(4) _cell_volume 2134.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 6.313 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3372 _exptl_absorpt_correction_T_max 0.5709 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD Detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 20 _diffrn_standards_decay_% ? _diffrn_reflns_number 7704 _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_av_sigmaI/netI 0.1491 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 21.18 _reflns_number_total 4575 _reflns_number_gt 2068 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4575 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2223 _refine_ls_R_factor_gt 0.1204 _refine_ls_wR_factor_ref 0.3690 _refine_ls_wR_factor_gt 0.3105 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.3599(3) 0.8279(3) 0.7337(2) 0.0504(12) Uani 1 1 d . . . O1 O 0.4956(15) 0.8208(14) 0.6562(9) 0.073(5) Uani 1 1 d . . . V2 V 0.0346(3) 0.7320(3) 0.7241(2) 0.0628(13) Uani 1 1 d . . . C2 C 0.607(3) 0.901(3) 0.6536(19) 0.093(9) Uani 1 1 d . . . H2A H 0.6416 0.9518 0.7114 0.112 Uiso 1 1 calc R . . V3 V 0.2929(3) 0.9044(3) 0.9320(2) 0.0499(12) Uani 1 1 d . . . C3 C 0.702(3) 0.844(3) 0.629(2) 0.127(12) Uani 1 1 d . . . H3A H 0.7743 0.9012 0.6286 0.190 Uiso 1 1 calc R . . H3B H 0.6715 0.7872 0.5737 0.190 Uiso 1 1 calc R . . H3C H 0.7265 0.8024 0.6664 0.190 Uiso 1 1 calc R . . C4 C 0.564(4) 0.981(4) 0.611(3) 0.18(2) Uani 1 1 d . . . H4A H 0.6366 1.0355 0.6081 0.277 Uiso 1 1 calc R . . H4B H 0.5094 1.0242 0.6413 0.277 Uiso 1 1 calc R . . H4C H 0.5185 0.9343 0.5560 0.277 Uiso 1 1 calc R . . O5 O 0.2683(17) 0.8778(16) 0.6497(10) 0.083(5) Uani 1 1 d . . . C6 C 0.156(3) 0.872(2) 0.6281(17) 0.078(8) Uani 1 1 d . . . O7 O 0.0653(18) 0.8256(16) 0.6491(9) 0.080(5) Uani 1 1 d . . . C8 C 0.112(3) 0.943(3) 0.568(2) 0.114(12) Uani 1 1 d . . . Br1A Br 0.1259(8) 0.8647(8) 0.4637(4) 0.153(3) Uani 0.50 1 d P . . C9A C 0.1259(8) 0.8647(8) 0.4637(4) 0.153(3) Uani 0.50 1 d P . . H9A1 H 0.1602 0.9211 0.4386 0.230 Uiso 0.50 1 calc PR . . H9A2 H 0.0434 0.8209 0.4317 0.230 Uiso 0.50 1 calc PR . . H9A3 H 0.1816 0.8103 0.4651 0.230 Uiso 0.50 1 calc PR . . Br1B Br 0.156(3) 1.0772(11) 0.6083(12) 0.57(3) Uani 0.50 1 d P . . C9B C 0.156(3) 1.0772(11) 0.6083(12) 0.57(3) Uani 0.50 1 d P . . H9B1 H 0.0873 1.1152 0.5968 0.848 Uiso 0.50 1 calc PR . . H9B2 H 0.2268 1.1054 0.5865 0.848 Uiso 0.50 1 calc PR . . H9B3 H 0.1811 1.0959 0.6673 0.848 Uiso 0.50 1 calc PR . . O10 O 0.3136(16) 0.6620(14) 0.6634(9) 0.072(5) Uani 1 1 d . . . C11 C 0.211(3) 0.585(2) 0.6476(14) 0.055(6) Uani 1 1 d . . . O12 O 0.1160(16) 0.6078(14) 0.6634(11) 0.078(5) Uani 1 1 d . . . C13 C 0.218(3) 0.463(2) 0.6077(18) 0.104(10) Uani 1 1 d . . . Br2A Br 0.1320(9) 0.3862(8) 0.5172(5) 0.185(4) Uani 0.50 1 d P . . C14A C 0.1320(9) 0.3862(8) 0.5172(5) 0.185(4) Uani 0.50 1 d P . . H14A H 0.0460 0.3617 0.5228 0.277 Uiso 0.50 1 calc PR . . H14B H 0.1653 0.3169 0.4936 0.277 Uiso 0.50 1 calc PR . . H14C H 0.1334 0.4343 0.4815 0.277 Uiso 0.50 1 calc PR . . Br2B Br 0.2397(13) 0.3893(6) 0.6780(6) 0.221(5) Uani 0.50 1 d P . . C14B C 0.2397(13) 0.3893(6) 0.6780(6) 0.221(5) Uani 0.50 1 d P . . H14D H 0.2814 0.4456 0.7314 0.332 Uiso 0.50 1 calc PR . . H14E H 0.2912 0.3321 0.6600 0.332 Uiso 0.50 1 calc PR . . H14F H 0.1584 0.3487 0.6820 0.332 Uiso 0.50 1 calc PR . . O15 O 0.4883(12) 0.7860(13) 0.8018(10) 0.061(4) Uani 1 1 d . . . C16 C 0.505(2) 0.7860(17) 0.8731(19) 0.053(6) Uani 1 1 d . . . O17 O 0.4299(14) 0.8185(12) 0.9208(9) 0.058(4) Uani 1 1 d . . . C18 C 0.616(2) 0.745(2) 0.9061(17) 0.086(8) Uani 1 1 d . . . Br3A Br 0.5552(4) 0.5845(3) 0.8983(3) 0.1053(16) Uani 0.75 1 d P . . C19A C 0.5552(4) 0.5845(3) 0.8983(3) 0.1053(16) Uani 0.25 1 d P . . H19A H 0.4686 0.5739 0.9057 0.158 Uiso 0.25 1 calc PR . . H19B H 0.6070 0.5656 0.9406 0.158 Uiso 0.25 1 calc PR . . H19C H 0.5595 0.5325 0.8446 0.158 Uiso 0.25 1 calc PR . . Br3B Br 0.7418(8) 0.7476(10) 0.8557(7) 0.110(3) Uani 0.25 1 d P . . C19B C 0.7418(8) 0.7476(10) 0.8557(7) 0.110(3) Uani 0.75 1 d P . . H19D H 0.7292 0.6734 0.8113 0.165 Uiso 0.75 1 calc PR . . H19E H 0.8193 0.7585 0.8943 0.165 Uiso 0.75 1 calc PR . . H19F H 0.7473 0.8123 0.8334 0.165 Uiso 0.75 1 calc PR . . O20 O 0.4485(13) 0.9951(13) 0.7863(11) 0.066(4) Uani 1 1 d . . . C21 C 0.440(2) 1.0655(19) 0.8593(19) 0.056(6) Uani 1 1 d . . . O22 O 0.3887(14) 1.0360(12) 0.9077(9) 0.058(4) Uani 1 1 d . . . C23 C 0.513(2) 1.1917(19) 0.8798(18) 0.094(9) Uani 1 1 d . . . Br4A Br 0.3851(5) 1.2697(4) 0.8437(4) 0.141(2) Uani 0.75 1 d P . . C24A C 0.3851(5) 1.2697(4) 0.8437(4) 0.141(2) Uani 0.25 1 d P . . H24A H 0.3791 1.2581 0.7854 0.212 Uiso 0.25 1 calc PR . . H24B H 0.4080 1.3536 0.8744 0.212 Uiso 0.25 1 calc PR . . H24C H 0.3044 1.2362 0.8531 0.212 Uiso 0.25 1 calc PR . . Br4B Br 0.6471(15) 1.2142(12) 0.8380(9) 0.178(6) Uani 0.25 1 d P . . C24B C 0.6471(15) 1.2142(12) 0.8380(9) 0.178(6) Uani 0.75 1 d P . . H24D H 0.7048 1.1673 0.8525 0.267 Uiso 0.75 1 calc PR . . H24E H 0.6882 1.2972 0.8597 0.267 Uiso 0.75 1 calc PR . . H24F H 0.6228 1.1905 0.7786 0.267 Uiso 0.75 1 calc PR . . O25 O -0.1077(12) 0.6717(14) 0.6844(10) 0.084(5) Uani 1 1 d . . . O26 O 0.0510(16) 0.6602(15) 0.8130(13) 0.093(6) Uani 1 1 d . . . C27 C 0.111(3) 0.670(3) 0.880(2) 0.067(7) Uani 1 1 d . . . O28 O 0.1897(17) 0.7549(15) 0.9267(11) 0.079(5) Uani 1 1 d . . . C29 C 0.070(2) 0.564(2) 0.909(2) 0.108(11) Uani 1 1 d . . . Br5A Br 0.2044(8) 0.5042(7) 0.9339(6) 0.158(3) Uani 0.50 1 d P . . C30A C 0.2044(8) 0.5042(7) 0.9339(6) 0.158(3) Uani 0.50 1 d P . . H30A H 0.2034 0.4328 0.8894 0.238 Uiso 0.50 1 calc PR . . H30B H 0.2011 0.4855 0.9842 0.238 Uiso 0.50 1 calc PR . . H30C H 0.2812 0.5618 0.9415 0.238 Uiso 0.50 1 calc PR . . Br5B Br -0.0795(6) 0.4822(7) 0.8756(6) 0.163(3) Uani 0.50 1 d P . . C30B C -0.0795(6) 0.4822(7) 0.8756(6) 0.163(3) Uani 0.50 1 d P . . H30D H -0.1308 0.5125 0.9150 0.244 Uiso 0.50 1 calc PR . . H30E H -0.0790 0.4004 0.8704 0.244 Uiso 0.50 1 calc PR . . H30F H -0.1143 0.4873 0.8226 0.244 Uiso 0.50 1 calc PR . . O31 O 0.0057(15) 0.8784(17) 0.7961(12) 0.079(5) Uani 1 1 d . . . C32 C 0.048(3) 0.961(3) 0.856(2) 0.081(8) Uani 1 1 d . . . O33 O 0.1423(17) 0.9746(14) 0.9097(12) 0.087(6) Uani 1 1 d . . . O34 O 0.3243(13) 0.9610(12) 1.0270(9) 0.064(4) Uani 1 1 d . . . C34 C -0.027(3) 1.068(4) 0.885(3) 0.20(2) Uani 1 1 d . . . Br6A Br -0.0085(7) 1.1243(5) 0.7746(4) 0.124(2) Uani 0.50 1 d P . . C35A C -0.0085(7) 1.1243(5) 0.7746(4) 0.124(2) Uani 0.50 1 d P . . H35A H 0.0498 1.0843 0.7455 0.186 Uiso 0.50 1 calc PR . . H35B H 0.0231 1.2091 0.7922 0.186 Uiso 0.50 1 calc PR . . H35C H -0.0902 1.1039 0.7383 0.186 Uiso 0.50 1 calc PR . . Br6B Br 0.0803(15) 1.2018(10) 0.9510(10) 0.301(9) Uani 0.50 1 d P . . C35B C 0.0803(15) 1.2018(10) 0.9510(10) 0.301(9) Uani 0.50 1 d P . . H35D H 0.1370 1.1837 0.9914 0.451 Uiso 0.50 1 calc PR . . H35E H 0.0331 1.2573 0.9789 0.451 Uiso 0.50 1 calc PR . . H35F H 0.1286 1.2364 0.9181 0.451 Uiso 0.50 1 calc PR . . O36 O 0.2488(11) 0.8215(10) 0.7857(8) 0.045(3) Uani 1 1 d . . . 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 0.051(2) 0.038(2) 0.064(3) 0.0220(19) 0.0068(19) 0.0093(18) O1 0.086(12) 0.077(11) 0.071(11) 0.028(9) 0.039(9) 0.027(10) V2 0.053(3) 0.048(3) 0.084(3) 0.028(2) -0.001(2) 0.004(2) C2 0.063(19) 0.10(2) 0.13(3) 0.05(2) 0.030(18) -0.004(18) V3 0.044(2) 0.039(2) 0.070(3) 0.020(2) 0.0122(19) 0.0118(18) C3 0.10(2) 0.15(3) 0.15(3) 0.06(3) 0.03(2) 0.05(2) C4 0.14(3) 0.20(4) 0.32(6) 0.20(5) 0.09(4) 0.06(3) O5 0.053(11) 0.122(15) 0.096(13) 0.074(11) 0.005(9) 0.018(10) C6 0.06(2) 0.076(19) 0.10(2) 0.041(17) 0.024(18) -0.003(16) O7 0.087(13) 0.094(13) 0.067(11) 0.041(10) 0.002(10) 0.028(11) C8 0.16(3) 0.12(3) 0.15(3) 0.13(2) 0.08(2) 0.07(2) Br1A 0.194(8) 0.182(7) 0.103(5) 0.078(5) 0.022(5) 0.040(6) C9A 0.194(8) 0.182(7) 0.103(5) 0.078(5) 0.022(5) 0.040(6) Br1B 0.87(5) 0.140(10) 0.50(3) 0.168(14) -0.43(3) -0.022(17) C9B 0.87(5) 0.140(10) 0.50(3) 0.168(14) -0.43(3) -0.022(17) O10 0.073(12) 0.050(11) 0.078(11) 0.004(9) 0.009(9) 0.015(10) C11 0.057(18) 0.031(15) 0.064(16) 0.004(12) -0.003(14) 0.011(15) O12 0.053(11) 0.051(11) 0.112(14) 0.010(9) 0.002(10) 0.007(9) C13 0.13(3) 0.06(2) 0.10(2) 0.012(17) 0.012(18) -0.001(18) Br2A 0.221(9) 0.152(7) 0.122(6) -0.019(6) -0.008(6) 0.033(7) C14A 0.221(9) 0.152(7) 0.122(6) -0.019(6) -0.008(6) 0.033(7) Br2B 0.400(16) 0.077(5) 0.179(8) 0.058(5) -0.035(9) 0.079(7) C14B 0.400(16) 0.077(5) 0.179(8) 0.058(5) -0.035(9) 0.079(7) O15 0.047(9) 0.081(12) 0.055(10) 0.024(9) -0.005(8) 0.022(8) C16 0.031(13) 0.030(13) 0.09(2) 0.016(13) -0.010(14) 0.012(11) O17 0.055(10) 0.051(10) 0.081(11) 0.030(8) 0.021(9) 0.030(8) C18 0.066(17) 0.067(17) 0.13(2) 0.024(16) 0.010(16) 0.051(14) Br3A 0.112(3) 0.065(2) 0.163(4) 0.064(3) 0.026(3) 0.037(2) C19A 0.112(3) 0.065(2) 0.163(4) 0.064(3) 0.026(3) 0.037(2) Br3B 0.079(6) 0.141(9) 0.141(8) 0.072(7) 0.036(6) 0.044(6) C19B 0.079(6) 0.141(9) 0.141(8) 0.072(7) 0.036(6) 0.044(6) O20 0.068(10) 0.041(10) 0.088(12) 0.021(10) 0.028(9) -0.003(8) C21 0.049(15) 0.031(15) 0.08(2) 0.014(15) -0.001(14) 0.000(12) O22 0.067(10) 0.046(10) 0.064(11) 0.028(9) 0.011(8) -0.005(8) C23 0.087(19) 0.023(14) 0.15(3) 0.025(15) -0.013(18) 0.001(14) Br4A 0.154(4) 0.062(3) 0.219(5) 0.072(3) 0.000(4) 0.035(3) C24A 0.154(4) 0.062(3) 0.219(5) 0.072(3) 0.000(4) 0.035(3) Br4B 0.196(13) 0.131(11) 0.169(12) 0.039(9) 0.045(10) -0.063(10) C24B 0.196(13) 0.131(11) 0.169(12) 0.039(9) 0.045(10) -0.063(10) O25 0.031(8) 0.085(12) 0.123(14) 0.038(11) 0.006(8) -0.021(8) O26 0.082(12) 0.079(13) 0.118(15) 0.069(12) -0.006(11) -0.032(10) C27 0.08(2) 0.058(19) 0.09(2) 0.054(18) 0.027(18) 0.031(17) O28 0.100(13) 0.046(11) 0.086(12) 0.024(10) 0.023(10) -0.007(10) C29 0.09(2) 0.08(2) 0.19(3) 0.11(2) 0.001(19) -0.001(16) Br5A 0.153(6) 0.113(5) 0.241(9) 0.104(6) 0.022(6) 0.046(5) C30A 0.153(6) 0.113(5) 0.241(9) 0.104(6) 0.022(6) 0.046(5) Br5B 0.107(5) 0.174(7) 0.238(8) 0.155(7) 0.007(5) -0.027(5) C30B 0.107(5) 0.174(7) 0.238(8) 0.155(7) 0.007(5) -0.027(5) O31 0.063(11) 0.075(13) 0.089(13) 0.014(11) -0.003(10) 0.022(10) C32 0.07(2) 0.07(2) 0.11(3) 0.029(19) 0.005(19) 0.036(18) O33 0.072(12) 0.058(11) 0.113(14) -0.005(10) 0.007(11) 0.031(10) O34 0.066(10) 0.049(9) 0.065(11) 0.008(8) 0.004(8) 0.006(8) C34 0.044(17) 0.16(3) 0.43(7) 0.21(4) -0.04(3) -0.02(2) Br6A 0.187(7) 0.089(4) 0.111(5) 0.048(4) 0.011(4) 0.063(4) C35A 0.187(7) 0.089(4) 0.111(5) 0.048(4) 0.011(4) 0.063(4) Br6B 0.299(16) 0.133(9) 0.400(19) 0.002(10) -0.044(13) 0.109(10) C35B 0.299(16) 0.133(9) 0.400(19) 0.002(10) -0.044(13) 0.109(10) O36 0.044(8) 0.033(8) 0.065(9) 0.027(7) 0.016(7) 0.001(6)