#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/02/4000200.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4000200
_journal_name_full               'Chemistry of Materials'
_journal_year                    2002
_chemical_formula_sum            'C21 H25 Br6 O16 V3'
_chemical_formula_weight         1165.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                107.372(4)
_cell_angle_beta                 98.015(4)
_cell_angle_gamma                99.125(4)
_cell_formula_units_Z            2
_cell_length_a                   10.967(2)
_cell_length_b                   12.126(2)
_cell_length_c                   17.378(3)
_cell_measurement_temperature    213(2)
_cell_volume                     2134.5(7)
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device       'Siemens SMART CCD Detector'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_sigmaI/netI    0.1491
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7704
_diffrn_reflns_theta_max         21.18
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  20
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    6.313
_exptl_absorpt_correction_T_max  0.5709
_exptl_absorpt_correction_T_min  0.3372
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_ls_extinction_coef       0.0045(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         4575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.2223
_refine_ls_R_factor_gt           0.1204
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3105
_refine_ls_wR_factor_ref         0.3690
_reflns_number_gt                2068
_reflns_number_total             4575
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4000200
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 . . .
