#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:38:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179254 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/74/4317444.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_4317444
loop_
_publ_author_name
'Clare Kimblin'
'Xianhui Bu'
'Alison Butler'
_publ_section_title
;
 Modeling the Catalytic Site of Vanadium Bromoperoxidase: Synthesis and
 Structural Characterization of Intramolecularly H-bonded Vanadium(V)
 Oxoperoxo Complexes, [VO(O2)(NH2pyg2)]K and [VO(O2)(BrNH2pyg2)]K
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              161
_journal_page_last               163
_journal_paper_doi               10.1021/ic010892j
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C10 H12 Br K N3 O8 V'
_chemical_formula_weight         472.18
_chemical_name_systematic
;
  ?
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                103.680(5)
_cell_angle_beta                 102.750(5)
_cell_angle_gamma                91.286(5)
_cell_formula_units_Z            4
_cell_length_a                   7.563(3)
_cell_length_b                   14.446(5)
_cell_length_c                   14.600(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1507.0(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14373
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    3.634
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_F_000             936
_refine_diff_density_max         1.549
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.229
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         5872
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.228
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_obs          0.0499
_refine_ls_shift/esd_max         0.160
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1332
_refine_ls_wR_factor_obs         0.1227
_reflns_number_observed          3780
_reflns_number_total             5873
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010892j_2.cif
_cod_data_source_block           datam
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1506.9(9)
_cod_database_code               4317444
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Br1 Br -0.83397(10) 0.09788(6) 0.52183(6) 0.0385(2) Uani 1 d . .
V1 V -0.30531(13) -0.09077(7) 0.75113(7) 0.0170(2) Uani 1 d . .
K1 K -0.2150(2) 0.25501(11) 0.94084(13) 0.0385(4) Uani 1 d . .
O1 O -0.6075(6) -0.2824(3) 0.8288(3) 0.0342(12) Uani 1 d . .
C1 C -0.2418(8) 0.1105(4) 0.6960(4) 0.0217(14) Uani 1 d . .
N1 N -0.0785(7) 0.1265(4) 0.7597(4) 0.0298(13) Uani 1 d D .
C2 C -0.2873(9) 0.1708(4) 0.6337(4) 0.0241(15) Uani 1 d . .
H2 H -0.1998(9) 0.2156(4) 0.6308(4) 0.029 Uiso 1 calc R .
Br2 Br 0.35055(9) 0.60120(5) 0.51188(5) 0.0320(2) Uani 1 d . .
V2 V 0.05082(13) 0.40860(7) 0.75452(7) 0.0153(2) Uani 1 d . .
K2 K -0.6741(2) 0.24688(10) 1.00283(10) 0.0224(3) Uani 1 d . .
O2 O -0.3808(5) -0.1881(3) 0.8187(3) 0.0225(10) Uani 1 d . .
N2 N -0.3606(6) 0.0395(3) 0.6964(3) 0.0183(11) Uani 1 d . .
O3 O -0.4344(6) 0.1083(3) 0.9792(3) 0.0237(10) Uani 1 d . .
N3 N -0.5915(6) -0.0681(3) 0.7481(3) 0.0146(10) Uani 1 d . .
C3 C -0.4602(8) 0.1644(4) 0.5767(4) 0.0231(14) Uani 1 d . .
H3 H -0.4913(8) 0.2022(4) 0.5330(4) 0.028 Uiso 1 calc R .
O4 O -0.2871(5) 0.0098(3) 0.8841(3) 0.0207(9) Uani 1 d . .
C4 C -0.5887(8) 0.0973(4) 0.5875(4) 0.0212(14) Uani 1 d . .
N4 N -0.1865(8) 0.6178(4) 0.7583(4) 0.0314(14) Uani 1 d D .
N5 N 0.0494(6) 0.5394(3) 0.6991(3) 0.0176(11) Uani 1 d . .
O5 O -0.3717(5) -0.1586(3) 0.6437(3) 0.0221(10) Uani 1 d . .
C5 C -0.5377(8) 0.0376(4) 0.6461(4) 0.0182(13) Uani 1 d . .
N6 N 0.3289(6) 0.4369(3) 0.7443(3) 0.0137(10) Uani 1 d . .
O6 O -0.0820(6) -0.1331(3) 0.8022(3) 0.0270(10) Uani 1 d . .
C6 C -0.6670(8) -0.0362(4) 0.6593(4) 0.0212(14) Uani 1 d . .
H6A H -0.7821(8) -0.0093(4) 0.6636(4) 0.025 Uiso 1 calc R .
H6B H -0.6893(8) -0.0906(4) 0.6035(4) 0.025 Uiso 1 calc R .
O7 O -0.0601(5) -0.0560(3) 0.7587(3) 0.0261(10) Uani 1 d . .
C7 C -0.6779(8) -0.1626(4) 0.7420(5) 0.0219(14) Uani 1 d . .
H7A H -0.7102(8) -0.1990(4) 0.6749(5) 0.026 Uiso 1 calc R .
H7B H -0.7886(8) -0.1544(4) 0.7652(5) 0.026 Uiso 1 calc R .
C8 C -0.5513(9) -0.2165(4) 0.8015(4) 0.0235(14) Uani 1 d . .
O8 O 0.4326(6) 0.2261(3) 0.8256(3) 0.0240(10) Uani 1 d . .
O9 O 0.1914(5) 0.3118(3) 0.8186(3) 0.0194(9) Uani 1 d . .
C9 C -0.6100(7) 0.0031(4) 0.8381(4) 0.0189(13) Uani 1 d . .
H9A H -0.6763(7) 0.0550(4) 0.8195(4) 0.023 Uiso 1 calc R .
H9B H -0.6813(7) -0.0276(4) 0.8719(4) 0.023 Uiso 1 calc R .
C10 C -0.4329(8) 0.0439(4) 0.9062(4) 0.0192(13) Uani 1 d . .
O10 O 0.4047(5) 0.6012(3) 0.9837(3) 0.0228(10) Uani 1 d . .
O11 O 0.1647(5) 0.5066(3) 0.8897(3) 0.0195(9) Uani 1 d . .
C11 C -0.0737(8) 0.6079(4) 0.6977(4) 0.0210(14) Uani 1 d . .
O12 O 0.0156(5) 0.3418(3) 0.6464(3) 0.0201(9) Uani 1 d . .
C12 C -0.0865(8) 0.6664(4) 0.6330(4) 0.0219(14) Uani 1 d . .
H12 H -0.1770(8) 0.7089(4) 0.6298(4) 0.026 Uiso 1 calc R .
O13 O -0.1196(5) 0.3618(3) 0.8103(3) 0.0230(10) Uani 1 d . .
C13 C 0.0317(8) 0.6619(4) 0.5750(4) 0.0201(14) Uani 1 d . .
H13 H 0.0209(8) 0.6987(4) 0.5300(4) 0.024 Uiso 1 calc R .
O14 O -0.1824(5) 0.4394(3) 0.7691(3) 0.0224(10) Uani 1 d . .
C14 C 0.1703(8) 0.6003(4) 0.5847(4) 0.0192(13) Uani 1 d . .
C15 C 0.1777(7) 0.5416(4) 0.6447(4) 0.0162(13) Uani 1 d . .
O15 O 0.0915(6) 0.3902(3) 1.0241(3) 0.0279(10) Uani 1 d . .
C16 C 0.3190(8) 0.4712(4) 0.6559(4) 0.0196(13) Uani 1 d . .
H16A H 0.2906(8) 0.4171(4) 0.5997(4) 0.024 Uiso 1 calc R .
H16B H 0.4367(8) 0.5011(4) 0.6585(4) 0.024 Uiso 1 calc R .
O16 O 0.0333(6) 0.1215(3) 0.9904(3) 0.0361(12) Uani 1 d . .
C17 C 0.4074(8) 0.3423(4) 0.7319(4) 0.0174(13) Uani 1 d . .
H17A H 0.5392(8) 0.3513(4) 0.7479(4) 0.021 Uiso 1 calc R .
H17B H 0.3675(8) 0.3059(4) 0.6650(4) 0.021 Uiso 1 calc R .
C18 C 0.3448(8) 0.2886(4) 0.7983(4) 0.0195(13) Uani 1 d . .
C19 C 0.4369(7) 0.5061(4) 0.8328(4) 0.0170(13) Uani 1 d . .
H19A H 0.4827(7) 0.5604(4) 0.8140(4) 0.020 Uiso 1 calc R .
H19B H 0.5408(7) 0.4757(4) 0.8613(4) 0.020 Uiso 1 calc R .
C20 C 0.3285(8) 0.5419(4) 0.9089(4) 0.0151(12) Uani 1 d . .
H1A H -0.0424(59) 0.0911(30) 0.7981(31) 0.004(14) Uiso 1 d D .
H1B H 0.0157(49) 0.1640(38) 0.7694(47) 0.049(24) Uiso 1 d D .
H4A H -0.1430(91) 0.5981(51) 0.8087(33) 0.046(24) Uiso 1 d D .
H4B H -0.2391(81) 0.6688(26) 0.7714(48) 0.036(21) Uiso 1 d D .
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'
K K 0.2009 0.2494 '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'
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
O5 V1 O6 105.0(2) . . ?
O5 V1 O7 103.1(2) . . ?
O6 V1 O7 44.8(2) . . ?
O5 V1 O2 95.1(2) . . ?
O6 V1 O2 78.0(2) . . ?
O7 V1 O2 122.5(2) . . ?
O5 V1 O4 165.1(2) . . ?
O6 V1 O4 89.8(2) . . ?
O7 V1 O4 88.9(2) . . ?
O2 V1 O4 85.5(2) . . ?
O5 V1 N3 87.6(2) . . ?
O6 V1 N3 152.4(2) . . ?
O7 V1 N3 156.4(2) . . ?
O2 V1 N3 76.5(2) . . ?
O4 V1 N3 78.1(2) . . ?
O5 V1 N2 91.4(2) . . ?
O6 V1 N2 128.9(2) . . ?
O7 V1 N2 84.6(2) . . ?
O2 V1 N2 149.4(2) . . ?
O4 V1 N2 80.8(2) . . ?
N3 V1 N2 74.0(2) . . ?
O10 K1 O8 72.53(13) 2_567 1_455 ?
O10 K1 O16 143.2(2) 2_567 . ?
O8 K1 O16 130.28(14) 1_455 . ?
O10 K1 O15 84.50(13) 2_567 . ?
O8 K1 O15 144.26(13) 1_455 . ?
O16 K1 O15 84.06(13) . . ?
O10 K1 O3 93.93(13) 2_567 . ?
O8 K1 O3 67.00(12) 1_455 . ?
O16 K1 O3 75.53(13) . . ?
O15 K1 O3 143.44(13) . . ?
O10 K1 O13 91.17(13) 2_567 . ?
O8 K1 O13 87.78(13) 1_455 . ?
O16 K1 O13 115.07(14) . . ?
O15 K1 O13 65.22(12) . . ?
O3 K1 O13 151.26(13) . . ?
O10 K1 N1 150.95(15) 2_567 . ?
O8 K1 N1 88.71(14) 1_455 . ?
O16 K1 N1 65.66(15) . . ?
O15 K1 N1 99.77(14) . . ?
O3 K1 N1 98.95(14) . . ?
O13 K1 N1 65.54(14) . . ?
O10 K1 C10 111.38(15) 2_567 . ?
O8 K1 C10 63.26(14) 1_455 . ?
O16 K1 C10 69.71(14) . . ?
O15 K1 C10 152.45(14) . . ?
O3 K1 C10 21.77(13) . . ?
O13 K1 C10 133.43(15) . . ?
N1 K1 C10 77.47(15) . . ?
O10 K1 C20 18.12(13) 2_567 2_567 ?
O8 K1 C20 90.64(14) 1_455 2_567 ?
O16 K1 C20 128.55(15) . 2_567 ?
O15 K1 C20 69.00(13) . 2_567 ?
O3 K1 C20 100.76(13) . 2_567 ?
O13 K1 C20 92.74(13) . 2_567 ?
N1 K1 C20 158.28(15) . 2_567 ?
C10 K1 C20 121.24(15) . 2_567 ?
O10 K1 K2 49.82(9) 2_567 . ?
O8 K1 K2 48.15(9) 1_455 . ?
O16 K1 K2 118.93(11) . . ?
O15 K1 K2 130.13(10) . . ?
O3 K1 K2 46.18(9) . . ?
O13 K1 K2 124.75(9) . . ?
N1 K1 K2 129.65(11) . . ?
C10 K1 K2 61.57(11) . . ?
C20 K1 K2 62.16(10) 2_567 . ?
O10 K1 K2 126.42(10) 2_567 1_655 ?
O8 K1 K2 157.00(11) 1_455 1_655 ?
O16 K1 K2 43.89(10) . 1_655 ?
O15 K1 K2 43.64(9) . 1_655 ?
O3 K1 K2 118.64(10) . 1_655 ?
O13 K1 K2 79.61(9) . 1_655 ?
N1 K1 K2 68.59(10) . 1_655 ?
C10 K1 K2 112.84(11) . 1_655 ?
C20 K1 K2 108.98(11) 2_567 1_655 ?
K2 K1 K2 152.66(7) . 1_655 ?
C8 O1 K2 93.1(4) . 2_457 ?
N1 C1 N2 119.7(6) . . ?
N1 C1 C2 119.0(6) . . ?
N2 C1 C2 121.3(6) . . ?
C1 N1 K1 96.6(4) . . ?
C1 N1 H1A 123.0(32) . . ?
K1 N1 H1A 84.4(37) . . ?
C1 N1 H1B 134.7(34) . . ?
K1 N1 H1B 93.2(52) . . ?
H1A N1 H1B 101.9(24) . . ?
C3 C2 C1 120.6(6) . . ?
C3 C2 H2 119.7(4) . . ?
C1 C2 H2 119.7(4) . . ?
O12 V2 O13 105.3(2) . . ?
O12 V2 O14 103.8(2) . . ?
O13 V2 O14 45.2(2) . . ?
O12 V2 O9 94.9(2) . . ?
O13 V2 O9 77.8(2) . . ?
O14 V2 O9 122.7(2) . . ?
O12 V2 O11 164.7(2) . . ?
O13 V2 O11 89.4(2) . . ?
O14 V2 O11 89.6(2) . . ?
O9 V2 O11 83.8(2) . . ?
O12 V2 N6 87.2(2) . . ?
O13 V2 N6 152.2(2) . . ?
O14 V2 N6 156.0(2) . . ?
O9 V2 N6 76.5(2) . . ?
O11 V2 N6 77.6(2) . . ?
O12 V2 N5 91.0(2) . . ?
O13 V2 N5 128.7(2) . . ?
O14 V2 N5 84.0(2) . . ?
O9 V2 N5 150.0(2) . . ?
O11 V2 N5 82.9(2) . . ?
N6 V2 N5 74.4(2) . . ?
O3 K2 O15 178.06(13) . 1_455 ?
O3 K2 O16 95.11(14) . 1_455 ?
O15 K2 O16 86.63(14) 1_455 1_455 ?
O3 K2 O1 71.51(13) . 2_457 ?
O15 K2 O1 108.44(14) 1_455 2_457 ?
O16 K2 O1 117.66(14) 1_455 2_457 ?
O3 K2 O8 68.43(12) . 1_455 ?
O15 K2 O8 110.08(13) 1_455 1_455 ?
O16 K2 O8 113.31(14) 1_455 1_455 ?
O1 K2 O8 116.35(14) 2_457 1_455 ?
O3 K2 O2 77.12(12) . 2_457 ?
O15 K2 O2 104.28(13) 1_455 2_457 ?
O16 K2 O2 71.81(13) 1_455 2_457 ?
O1 K2 O2 45.93(12) 2_457 2_457 ?
O8 K2 O2 145.42(13) 1_455 2_457 ?
O3 K2 O10 93.00(13) . 2_567 ?
O15 K2 O10 85.25(13) 1_455 2_567 ?
O16 K2 O10 171.84(14) 1_455 2_567 ?
O1 K2 O10 65.94(13) 2_457 2_567 ?
O8 K2 O10 69.04(12) 1_455 2_567 ?
O2 K2 O10 111.01(13) 2_457 2_567 ?
O3 K2 O9 111.71(12) . 1_455 ?
O15 K2 O9 67.08(12) 1_455 1_455 ?
O16 K2 O9 99.71(13) 1_455 1_455 ?
O1 K2 O9 142.34(13) 2_457 1_455 ?
O8 K2 O9 44.47(11) 1_455 1_455 ?
O2 K2 O9 168.69(12) 2_457 1_455 ?
O10 K2 O9 76.39(11) 2_567 1_455 ?
O3 K2 C8 66.75(15) . 2_457 ?
O15 K2 C8 114.0(2) 1_455 2_457 ?
O16 K2 C8 95.2(2) 1_455 2_457 ?
O1 K2 C8 22.93(14) 2_457 2_457 ?
O8 K2 C8 128.3(2) 1_455 2_457 ?
O2 K2 C8 24.54(14) 2_457 2_457 ?
O10 K2 C8 88.82(15) 2_567 2_457 ?
O9 K2 C8 165.11(15) 1_455 2_457 ?
O3 K2 C18 90.60(14) . 1_455 ?
O15 K2 C18 87.91(14) 1_455 1_455 ?
O16 K2 C18 113.34(15) 1_455 1_455 ?
O1 K2 C18 126.89(15) 2_457 1_455 ?
O8 K2 C18 22.17(13) 1_455 1_455 ?
O2 K2 C18 167.24(14) 2_457 1_455 ?
O10 K2 C18 65.63(13) 2_567 1_455 ?
O9 K2 C18 23.64(12) 1_455 1_455 ?
C8 K2 C18 145.4(2) 2_457 1_455 ?
O3 K2 K1 49.56(9) . . ?
O15 K2 K1 128.53(10) 1_455 . ?
O16 K2 K1 142.00(12) 1_455 . ?
O1 K2 K1 69.23(11) 2_457 . ?
O8 K2 K1 47.12(9) 1_455 . ?
O2 K2 K1 106.68(9) 2_457 . ?
O10 K2 K1 45.48(9) 2_567 . ?
O9 K2 K1 84.62(8) 1_455 . ?
C8 K2 K1 83.73(13) 2_457 . ?
C18 K2 K1 61.78(11) 1_455 . ?
O3 K2 K1 136.01(10) . 1_455 ?
O15 K2 K1 45.32(10) 1_455 1_455 ?
O16 K2 K1 44.95(10) 1_455 1_455 ?
O1 K2 K1 136.49(11) 2_457 1_455 ?
O8 K2 K1 106.38(10) 1_455 1_455 ?
O2 K2 K1 100.27(9) 2_457 1_455 ?
O10 K2 K1 127.13(10) 2_567 1_455 ?
O9 K2 K1 68.51(8) 1_455 1_455 ?
C8 K2 K1 123.60(13) 2_457 1_455 ?
C18 K2 K1 90.94(11) 1_455 1_455 ?
K1 K2 K1 152.66(7) . 1_455 ?
C8 O2 V1 119.1(4) . . ?
C8 O2 K2 88.4(3) . 2_457 ?
V1 O2 K2 145.7(2) . 2_457 ?
C1 N2 C5 118.2(5) . . ?
C1 N2 V1 128.8(4) . . ?
C5 N2 V1 112.4(4) . . ?
C10 O3 K2 128.9(4) . . ?
C10 O3 K1 98.4(3) . . ?
K2 O3 K1 84.26(12) . . ?
C7 N3 C6 110.3(4) . . ?
C7 N3 C9 110.9(5) . . ?
C6 N3 C9 112.2(4) . . ?
C7 N3 V1 105.3(3) . . ?
C6 N3 V1 107.1(3) . . ?
C9 N3 V1 110.8(3) . . ?
C2 C3 C4 116.8(6) . . ?
C2 C3 H3 121.6(4) . . ?
C4 C3 H3 121.6(4) . . ?
C10 O4 V1 119.7(4) . . ?
C5 C4 C3 120.8(6) . . ?
C5 C4 Br1 121.6(5) . . ?
C3 C4 Br1 117.6(5) . . ?
C11 N4 H4A 112.1(51) . . ?
C11 N4 H4B 120.6(47) . . ?
H4A N4 H4B 112.2(70) . . ?
C11 N5 C15 116.4(5) . . ?
C11 N5 V2 130.1(4) . . ?
C15 N5 V2 112.6(4) . . ?
C4 C5 N2 121.5(5) . . ?
C4 C5 C6 123.3(5) . . ?
N2 C5 C6 115.2(5) . . ?
C16 N6 C19 112.2(4) . . ?
C16 N6 C17 109.2(4) . . ?
C19 N6 C17 110.6(4) . . ?
C16 N6 V2 107.3(3) . . ?
C19 N6 V2 112.0(3) . . ?
C17 N6 V2 105.2(3) . . ?
O7 O6 V1 68.2(2) . . ?
N3 C6 C5 110.8(5) . . ?
N3 C6 H6A 109.5(3) . . ?
C5 C6 H6A 109.5(3) . . ?
N3 C6 H6B 109.5(3) . . ?
C5 C6 H6B 109.5(3) . . ?
H6A C6 H6B 108.1 . . ?
O6 O7 V1 67.0(2) . . ?
N3 C7 C8 110.7(5) . . ?
N3 C7 H7A 109.5(3) . . ?
C8 C7 H7A 109.5(3) . . ?
N3 C7 H7B 109.5(3) . . ?
C8 C7 H7B 109.5(3) . . ?
H7A C7 H7B 108.1 . . ?
O1 C8 O2 123.9(6) . . ?
O1 C8 C7 121.6(6) . . ?
O2 C8 C7 114.4(5) . . ?
O1 C8 K2 64.0(4) . 2_457 ?
O2 C8 K2 67.1(3) . 2_457 ?
C7 C8 K2 152.9(4) . 2_457 ?
C18 O8 K1 125.0(4) . 1_655 ?
C18 O8 K2 96.9(4) . 1_655 ?
K1 O8 K2 84.73(13) 1_655 1_655 ?
C18 O9 V2 118.8(4) . . ?
C18 O9 K2 86.3(3) . 1_655 ?
V2 O9 K2 147.1(2) . 1_655 ?
C10 C9 N3 114.1(5) . . ?
C10 C9 H9A 108.7(3) . . ?
N3 C9 H9A 108.7(3) . . ?
C10 C9 H9B 108.7(3) . . ?
N3 C9 H9B 108.7(3) . . ?
H9A C9 H9B 107.6 . . ?
O3 C10 O4 124.3(6) . . ?
O3 C10 C9 118.5(5) . . ?
O4 C10 C9 117.2(5) . . ?
O3 C10 K1 59.9(3) . . ?
O4 C10 K1 84.9(3) . . ?
C9 C10 K1 128.8(4) . . ?
C20 O10 K1 118.7(4) . 2_567 ?
C20 O10 K2 125.5(4) . 2_567 ?
K1 O10 K2 84.70(12) 2_567 2_567 ?
C20 O11 V2 120.3(3) . . ?
N4 C11 N5 119.5(6) . . ?
N4 C11 C12 119.3(5) . . ?
N5 C11 C12 121.2(5) . . ?
C13 C12 C11 120.6(6) . . ?
C13 C12 H12 119.7(4) . . ?
C11 C12 H12 119.7(3) . . ?
O14 O13 V2 67.8(2) . . ?
O14 O13 K1 138.9(3) . . ?
V2 O13 K1 151.0(2) . . ?
C12 C13 C14 118.1(6) . . ?
C12 C13 H13 121.0(4) . . ?
C14 C13 H13 121.0(3) . . ?
O13 O14 V2 67.0(2) . . ?
C15 C14 C13 120.9(5) . . ?
C15 C14 Br2 120.5(5) . . ?
C13 C14 Br2 118.6(4) . . ?
C14 C15 N5 122.1(5) . . ?
C14 C15 C16 123.6(5) . . ?
N5 C15 C16 114.3(5) . . ?
K2 O15 K1 91.05(13) 1_655 . ?
N6 C16 C15 112.0(5) . . ?
N6 C16 H16A 109.2(3) . . ?
C15 C16 H16A 109.2(3) . . ?
N6 C16 H16B 109.2(3) . . ?
C15 C16 H16B 109.2(3) . . ?
H16A C16 H16B 107.9 . . ?
K2 O16 K1 91.15(14) 1_655 . ?
N6 C17 C18 108.9(4) . . ?
N6 C17 H17A 109.9(3) . . ?
C18 C17 H17A 109.9(3) . . ?
N6 C17 H17B 109.9(3) . . ?
C18 C17 H17B 109.9(3) . . ?
H17A C17 H17B 108.3 . . ?
O8 C18 O9 124.5(6) . . ?
O8 C18 C17 120.9(5) . . ?
O9 C18 C17 114.6(5) . . ?
O8 C18 K2 60.9(3) . 1_655 ?
O9 C18 K2 70.1(3) . 1_655 ?
C17 C18 K2 155.7(4) . 1_655 ?
N6 C19 C20 113.4(4) . . ?
N6 C19 H19A 108.9(3) . . ?
C20 C19 H19A 108.9(3) . . ?
N6 C19 H19B 108.9(3) . . ?
C20 C19 H19B 108.9(3) . . ?
H19A C19 H19B 107.7 . . ?
O10 C20 O11 125.1(5) . . ?
O10 C20 C19 118.4(5) . . ?
O11 C20 C19 116.5(5) . . ?
O10 C20 K1 43.1(3) . 2_567 ?
O11 C20 K1 89.6(3) . 2_567 ?
C19 C20 K1 144.2(4) . 2_567 ?
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
Br1 C4 1.892(6) . ?
V1 O5 1.605(4) . ?
V1 O6 1.868(4) . ?
V1 O7 1.883(4) . ?
V1 O2 2.036(4) . ?
V1 O4 2.106(4) . ?
V1 N3 2.189(5) . ?
V1 N2 2.227(5) . ?
K1 O10 2.708(4) 2_567 ?
K1 O8 2.783(5) 1_455 ?
K1 O16 2.827(5) . ?
K1 O15 2.845(5) . ?
K1 O3 2.893(4) . ?
K1 O13 2.912(4) . ?
K1 N1 3.237(6) . ?
K1 C10 3.309(6) . ?
K1 C20 3.473(6) 2_567 ?
K1 K2 3.782(2) . ?
K1 K2 4.001(2) 1_655 ?
O1 C8 1.217(7) . ?
O1 K2 2.808(5) 2_457 ?
C1 N1 1.349(8) . ?
C1 N2 1.350(7) . ?
C1 C2 1.399(9) . ?
N1 H1A 0.853(10) . ?
N1 H1B 0.850(10) . ?
C2 C3 1.374(9) . ?
C2 H2 0.93 . ?
Br2 C14 1.907(6) . ?
V2 O12 1.605(4) . ?
V2 O13 1.861(4) . ?
V2 O14 1.873(4) . ?
V2 O9 2.052(4) . ?
V2 O11 2.125(4) . ?
V2 N6 2.177(5) . ?
V2 N5 2.223(5) . ?
K2 O3 2.743(4) . ?
K2 O15 2.762(4) 1_455 ?
K2 O16 2.775(5) 1_455 ?
K2 O1 2.808(5) 2_457 ?
K2 O8 2.829(4) 1_455 ?
K2 O2 2.875(4) 2_457 ?
K2 O10 2.902(4) 2_567 ?
K2 O9 3.029(4) 1_455 ?
K2 C8 3.120(7) 2_457 ?
K2 C18 3.214(6) 1_455 ?
K2 K1 4.001(2) 1_455 ?
O2 C8 1.296(7) . ?
O2 K2 2.875(4) 2_457 ?
N2 C5 1.374(7) . ?
O3 C10 1.241(7) . ?
N3 C7 1.474(7) . ?
N3 C6 1.480(7) . ?
N3 C9 1.501(7) . ?
C3 C4 1.417(8) . ?
C3 H3 0.93 . ?
O4 C10 1.292(7) . ?
C4 C5 1.357(8) . ?
N4 C11 1.346(8) . ?
N4 H4A 0.852(10) . ?
N4 H4B 0.848(10) . ?
N5 C11 1.374(7) . ?
N5 C15 1.387(7) . ?
C5 C6 1.504(8) . ?
N6 C16 1.476(7) . ?
N6 C19 1.490(7) . ?
N6 C17 1.489(7) . ?
O6 O7 1.430(6) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C7 C8 1.506(9) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C8 K2 3.120(7) 2_457 ?
O8 C18 1.222(7) . ?
O8 K1 2.783(4) 1_655 ?
O8 K2 2.829(4) 1_655 ?
O9 C18 1.292(7) . ?
O9 K2 3.029(4) 1_655 ?
C9 C10 1.493(8) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
O10 C20 1.232(7) . ?
O10 K1 2.708(4) 2_567 ?
O10 K2 2.902(4) 2_567 ?
O11 C20 1.274(7) . ?
C11 C12 1.400(8) . ?
C12 C13 1.353(8) . ?
C12 H12 0.93 . ?
O13 O14 1.435(6) . ?
C13 C14 1.394(8) . ?
C13 H13 0.93 . ?
C14 C15 1.351(8) . ?
C15 C16 1.501(8) . ?
O15 K2 2.762(4) 1_655 ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
O16 K2 2.775(5) 1_655 ?
C17 C18 1.520(8) . ?
C17 H17A 0.97 . ?
C17 H17B 0.97 . ?
C18 K2 3.214(6) 1_655 ?
C19 C20 1.524(8) . ?
C19 H19A 0.97 . ?
C19 H19B 0.97 . ?
C20 K1 3.473(6) 2_567 ?
