#------------------------------------------------------------------------------
#$Date: 2015-12-09 15:53:49 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171150 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/74/7037424.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_7037424
loop_
_publ_author_name
'van Dijkman, Thomas F.'
'Siegler, Maxime A.'
'Bouwman, Elisabeth'
_publ_section_title
;
 Highly tunable fluorinated trispyrazolylborates
 [HB(3-CF3-5-{4-RPh}pz)3](-) (R = NO2, CF3, Cl, F, H, OMe and NMe2) and
 their copper(i) complexes.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              21109
_journal_page_last               21123
_journal_paper_doi               10.1039/c5dt04006j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C30 H18 B F9 N9 Na O7'
_chemical_formula_sum            'C30 H18 B F9 N9 Na O7'
_chemical_formula_weight         821.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-08 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.3724(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.32258(10)
_cell_length_b                   23.3536(3)
_cell_length_c                   15.70665(18)
_cell_measurement_reflns_used    10327
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.96
_cell_measurement_theta_min      3.38
_cell_volume                     3391.32(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20217
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.900
_diffrn_reflns_theta_min         3.410
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6614
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0374
_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/[σ²(Fo²)+(0.0490P)²+1.3075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5643
_reflns_number_total             6614
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt04006j2.cif
_cod_data_source_block           Na4aprime
_cod_depositor_comments
'Adding full bibliography for 7037416--7037425.cif.'
_cod_database_code               7037424
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Na1 Na 0.52769(7) 0.03601(3) 0.77896(4) 0.02181(15) Uani 1 1 d . .
B1 B 0.58689(18) 0.16385(7) 0.68908(11) 0.0166(3) Uani 1 1 d . .
H1 H 0.610(2) 0.2061(8) 0.6615(12) 0.016(5) Uiso 1 1 d . .
O1W O 0.5871(2) -0.00183(7) 0.91108(10) 0.0457(4) Uani 1 1 d D .
H1W1 H 0.650(3) 0.0131(13) 0.9467(19) 0.069 Uiso 1 1 d D U
H1W2 H 0.554(3) -0.0289(12) 0.935(2) 0.069 Uiso 1 1 d D U
N11 N 0.47834(14) 0.17209(6) 0.75528(8) 0.0166(3) Uani 1 1 d . .
N12 N 0.46888(15) 0.13461(6) 0.82031(9) 0.0191(3) Uani 1 1 d . .
C13 C 0.38290(18) 0.16011(7) 0.87053(11) 0.0214(3) Uani 1 1 d . .
C131 C 0.3468(2) 0.13066(8) 0.94904(12) 0.0273(4) Uani 1 1 d . .
F11 F 0.25395(19) 0.16080(8) 0.98805(10) 0.0661(5) Uani 1 1 d . .
F12 F 0.28956(16) 0.07908(6) 0.93265(8) 0.0491(4) Uani 1 1 d . .
F13 F 0.46368(13) 0.12200(5) 1.00767(7) 0.0365(3) Uani 1 1 d . .
C14 C 0.33530(18) 0.21376(7) 0.83951(11) 0.0221(3) Uani 1 1 d . .
H14 H 0.2743 0.2400 0.8640 0.027 Uiso 1 1 calc R U
C15 C 0.39781(16) 0.21971(7) 0.76494(10) 0.0176(3) Uani 1 1 d . .
C151 C 0.37710(16) 0.26519(7) 0.69924(10) 0.0179(3) Uani 1 1 d . .
C152 C 0.40031(18) 0.32238(7) 0.72245(11) 0.0225(3) Uani 1 1 d . .
H152 H 0.4354 0.3319 0.7802 0.027 Uiso 1 1 calc R U
C153 C 0.37253(19) 0.36542(7) 0.66172(11) 0.0239(3) Uani 1 1 d . .
H153 H 0.3870 0.4045 0.6771 0.029 Uiso 1 1 calc R U
C154 C 0.32310(17) 0.34984(7) 0.57800(11) 0.0221(3) Uani 1 1 d . .
C155 C 0.29984(17) 0.29347(8) 0.55260(11) 0.0223(3) Uani 1 1 d . .
H155 H 0.2666 0.2841 0.4945 0.027 Uiso 1 1 calc R U
C156 C 0.32652(17) 0.25105(7) 0.61428(10) 0.0199(3) Uani 1 1 d . .
H156 H 0.3103 0.2121 0.5987 0.024 Uiso 1 1 calc R U
N13 N 0.28786(17) 0.39513(7) 0.51408(10) 0.0277(3) Uani 1 1 d . .
O131 O 0.27881(18) 0.44462(6) 0.54053(10) 0.0407(4) Uani 1 1 d . .
O132 O 0.26694(17) 0.38159(7) 0.43845(9) 0.0373(3) Uani 1 1 d . .
N21 N 0.73207(14) 0.13931(6) 0.73311(8) 0.0165(3) Uani 1 1 d . .
N22 N 0.74972(15) 0.08229(6) 0.74876(9) 0.0181(3) Uani 1 1 d . .
C23 C 0.89034(17) 0.07622(7) 0.77653(10) 0.0197(3) Uani 1 1 d . .
C231 C 0.94936(19) 0.01883(8) 0.80390(12) 0.0252(4) Uani 1 1 d . .
F21 F 1.09182(11) 0.01611(5) 0.79969(8) 0.0327(2) Uani 1 1 d . .
F22 F 0.93128(17) 0.00582(6) 0.88369(9) 0.0561(4) Uani 1 1 d . .
F23 F 0.89065(14) -0.02345(5) 0.75366(10) 0.0490(4) Uani 1 1 d . .
C24 C 0.96545(17) 0.12778(7) 0.77843(11) 0.0219(3) Uani 1 1 d . .
H24 H 1.0659 0.1342 0.7948 0.026 Uiso 1 1 calc R U
C25 C 0.85982(17) 0.16752(7) 0.75100(10) 0.0183(3) Uani 1 1 d . .
C251 C 0.87817(17) 0.23011(7) 0.74339(10) 0.0178(3) Uani 1 1 d . .
C252 C 0.98867(17) 0.25044(7) 0.69934(11) 0.0212(3) Uani 1 1 d . .
H252 H 1.0442 0.2242 0.6708 0.025 Uiso 1 1 calc R U
C253 C 1.01808(17) 0.30851(7) 0.69686(11) 0.0213(3) Uani 1 1 d . .
H253 H 1.0933 0.3225 0.6671 0.026 Uiso 1 1 calc R U
C254 C 0.93534(17) 0.34557(7) 0.73880(10) 0.0184(3) Uani 1 1 d . .
C255 C 0.82164(17) 0.32716(7) 0.78115(11) 0.0212(3) Uani 1 1 d . .
H255 H 0.7646 0.3537 0.8080 0.025 Uiso 1 1 calc R U
C256 C 0.79385(17) 0.26895(7) 0.78313(11) 0.0215(3) Uani 1 1 d . .
H256 H 0.7168 0.2553 0.8117 0.026 Uiso 1 1 calc R U
N23 N 0.97440(15) 0.40647(6) 0.74128(9) 0.0206(3) Uani 1 1 d . .
O231 O 0.90139(15) 0.44022(5) 0.77811(8) 0.0273(3) Uani 1 1 d . .
O232 O 1.07982(14) 0.42195(5) 0.70755(9) 0.0290(3) Uani 1 1 d . .
N31 N 0.52089(14) 0.12331(6) 0.61616(8) 0.0166(3) Uani 1 1 d . .
N32 N 0.43468(14) 0.07866(6) 0.63106(8) 0.0173(3) Uani 1 1 d . .
C33 C 0.38458(16) 0.05682(7) 0.55379(10) 0.0174(3) Uani 1 1 d . .
C331 C 0.27939(16) 0.00966(7) 0.54458(10) 0.0177(3) Uani 1 1 d . .
C332 C 0.21788(18) -0.01084(7) 0.61532(11) 0.0221(3) Uani 1 1 d . .
H332 H 0.2472 0.0050 0.6705 0.027 Uiso 1 1 calc R U
C333 C 0.11484(18) -0.05387(8) 0.60612(11) 0.0228(3) Uani 1 1 d . .
H333 H 0.0739 -0.0679 0.6544 0.027 Uiso 1 1 calc R U
C334 C 0.07276(17) -0.07598(7) 0.52492(11) 0.0203(3) Uani 1 1 d . .
C335 C 0.13118(17) -0.05695(7) 0.45334(11) 0.0218(3) Uani 1 1 d . .
H335 H 0.1006 -0.0728 0.3983 0.026 Uiso 1 1 calc R U
C336 C 0.23517(17) -0.01431(7) 0.46358(11) 0.0213(3) Uani 1 1 d . .
H336 H 0.2771 -0.0011 0.4151 0.026 Uiso 1 1 calc R U
C34 C 0.44105(17) 0.08684(7) 0.48811(10) 0.0194(3) Uani 1 1 d . .
H34 H 0.4239 0.0799 0.4281 0.023 Uiso 1 1 calc R U
C35 C 0.52653(16) 0.12846(7) 0.53028(10) 0.0174(3) Uani 1 1 d . .
C351 C 0.61331(18) 0.17270(7) 0.49118(10) 0.0211(3) Uani 1 1 d . .
F31 F 0.74516(10) 0.18113(4) 0.53471(6) 0.0251(2) Uani 1 1 d . .
F32 F 0.54887(12) 0.22414(5) 0.48379(7) 0.0315(2) Uani 1 1 d . .
F33 F 0.63398(11) 0.15672(5) 0.41127(6) 0.0287(2) Uani 1 1 d . .
N33 N -0.03780(15) -0.12118(6) 0.51429(10) 0.0240(3) Uani 1 1 d . .
O331 O -0.08325(15) -0.14022(6) 0.57870(9) 0.0359(3) Uani 1 1 d . .
O332 O -0.08090(15) -0.13780(6) 0.44128(9) 0.0332(3) Uani 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1W Na1 N22 103.78(6) . .
O1W Na1 N12 99.18(6) . .
N22 Na1 N12 81.98(5) . .
O1W Na1 O231 86.28(6) . 2_646
N22 Na1 O231 93.22(5) . 2_646
N12 Na1 O231 173.43(5) . 2_646
O1W Na1 N32 174.55(7) . .
N22 Na1 N32 81.30(5) . .
N12 Na1 N32 79.42(5) . .
O231 Na1 N32 95.48(5) 2_646 .
O1W Na1 O232 67.35(5) . 2_646
N22 Na1 O232 137.88(5) . 2_646
N12 Na1 O232 139.04(5) . 2_646
O231 Na1 O232 46.64(4) 2_646 2_646
N32 Na1 O232 110.26(5) . 2_646
O1W Na1 N23 72.81(5) . 2_646
N22 Na1 N23 114.54(5) . 2_646
N12 Na1 N23 162.72(5) . 2_646
O231 Na1 N23 23.33(4) 2_646 2_646
N32 Na1 N23 107.08(4) . 2_646
O232 Na1 N23 23.78(4) 2_646 2_646
N21 B1 N31 110.18(13) . .
N21 B1 N11 110.74(13) . .
N31 B1 N11 109.82(12) . .
N21 B1 H1 107.6(10) . .
N31 B1 H1 109.4(10) . .
N11 B1 H1 109.0(10) . .
Na1 O1W H1W1 121(2) . .
Na1 O1W H1W2 132(2) . .
H1W1 O1W H1W2 107(3) . .
N12 N11 C15 110.68(13) . .
N12 N11 B1 122.35(13) . .
C15 N11 B1 126.29(13) . .
C13 N12 N11 105.01(13) . .
C13 N12 Na1 137.80(11) . .
N11 N12 Na1 111.41(10) . .
N12 C13 C14 112.47(15) . .
N12 C13 C131 120.01(15) . .
C14 C13 C131 127.51(16) . .
F11 C131 F12 107.49(17) . .
F11 C131 F13 106.40(16) . .
F12 C131 F13 105.40(15) . .
F11 C131 C13 111.60(16) . .
F12 C131 C13 112.74(15) . .
F13 C131 C13 112.76(15) . .
C15 C14 C13 103.69(14) . .
C15 C14 H14 128.2 . .
C13 C14 H14 128.2 . .
N11 C15 C14 108.13(14) . .
N11 C15 C151 122.31(14) . .
C14 C15 C151 129.34(15) . .
C152 C151 C156 119.89(15) . .
C152 C151 C15 120.31(15) . .
C156 C151 C15 119.71(15) . .
C153 C152 C151 120.37(16) . .
C153 C152 H152 119.8 . .
C151 C152 H152 119.8 . .
C154 C153 C152 118.20(16) . .
C154 C153 H153 120.9 . .
C152 C153 H153 120.9 . .
C155 C154 C153 122.96(16) . .
C155 C154 N13 118.39(15) . .
C153 C154 N13 118.59(16) . .
C154 C155 C156 118.09(15) . .
C154 C155 H155 121.0 . .
C156 C155 H155 121.0 . .
C155 C156 C151 120.49(15) . .
C155 C156 H156 119.8 . .
C151 C156 H156 119.8 . .
O132 N13 O131 124.10(16) . .
O132 N13 C154 118.25(16) . .
O131 N13 C154 117.64(15) . .
C25 N21 N22 110.79(13) . .
C25 N21 B1 127.27(13) . .
N22 N21 B1 121.43(13) . .
C23 N22 N21 104.71(13) . .
C23 N22 Na1 135.46(11) . .
N21 N22 Na1 112.56(9) . .
N22 C23 C24 112.68(14) . .
N22 C23 C231 120.01(15) . .
C24 C23 C231 127.28(15) . .
F22 C231 F23 107.32(17) . .
F22 C231 F21 106.50(15) . .
F23 C231 F21 105.62(15) . .
F22 C231 C23 113.14(15) . .
F23 C231 C23 112.70(15) . .
F21 C231 C23 111.09(14) . .
C25 C24 C23 103.78(14) . .
C25 C24 H24 128.1 . .
C23 C24 H24 128.1 . .
N21 C25 C24 108.03(14) . .
N21 C25 C251 124.77(14) . .
C24 C25 C251 127.18(15) . .
C252 C251 C256 119.56(15) . .
C252 C251 C25 118.48(14) . .
C256 C251 C25 121.85(15) . .
C253 C252 C251 120.55(15) . .
C253 C252 H252 119.7 . .
C251 C252 H252 119.7 . .
C254 C253 C252 118.38(15) . .
C254 C253 H253 120.8 . .
C252 C253 H253 120.8 . .
C253 C254 C255 122.76(15) . .
C253 C254 N23 117.91(14) . .
C255 C254 N23 119.27(14) . .
C256 C255 C254 118.08(15) . .
C256 C255 H255 121.0 . .
C254 C255 H255 121.0 . .
C255 C256 C251 120.60(15) . .
C255 C256 H256 119.7 . .
C251 C256 H256 119.7 . .
O232 N23 O231 122.29(14) . .
O232 N23 C254 118.89(14) . .
O231 N23 C254 118.82(14) . .
O232 N23 Na1 69.95(9) . 2_656
O231 N23 Na1 54.32(8) . 2_656
C254 N23 Na1 164.36(10) . 2_656
N23 O231 Na1 102.36(10) . 2_656
N23 O232 Na1 86.27(9) . 2_656
N32 N31 C35 109.76(13) . .
N32 N31 B1 122.01(12) . .
C35 N31 B1 127.97(13) . .
C33 N32 N31 106.34(13) . .
C33 N32 Na1 134.91(11) . .
N31 N32 Na1 108.37(9) . .
N32 C33 C34 110.75(14) . .
N32 C33 C331 121.58(14) . .
C34 C33 C331 127.61(15) . .
C332 C331 C336 118.76(15) . .
C332 C331 C33 120.99(14) . .
C336 C331 C33 120.21(15) . .
C333 C332 C331 121.00(15) . .
C333 C332 H332 119.5 . .
C331 C332 H332 119.5 . .
C332 C333 C334 118.51(15) . .
C332 C333 H333 120.7 . .
C334 C333 H333 120.7 . .
C335 C334 C333 122.27(15) . .
C335 C334 N33 118.79(15) . .
C333 C334 N33 118.94(15) . .
C334 C335 C336 118.64(15) . .
C334 C335 H335 120.7 . .
C336 C335 H335 120.7 . .
C335 C336 C331 120.81(15) . .
C335 C336 H336 119.6 . .
C331 C336 H336 119.6 . .
C35 C34 C33 104.38(14) . .
C35 C34 H34 127.8 . .
C33 C34 H34 127.8 . .
N31 C35 C34 108.76(14) . .
N31 C35 C351 124.10(14) . .
C34 C35 C351 127.14(15) . .
F32 C351 F31 106.46(14) . .
F32 C351 F33 106.47(13) . .
F31 C351 F33 106.51(13) . .
F32 C351 C35 113.28(13) . .
F31 C351 C35 113.66(14) . .
F33 C351 C35 109.98(14) . .
O332 N33 O331 123.23(15) . .
O332 N33 C334 118.27(15) . .
O331 N33 C334 118.50(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na1 O1W 2.2581(16) .
Na1 N22 2.4351(15) .
Na1 N12 2.4731(15) .
Na1 O231 2.5291(14) 2_646
Na1 N32 2.5737(15) .
Na1 O232 2.8633(14) 2_646
Na1 N23 3.0418(15) 2_646
B1 N21 1.549(2) .
B1 N31 1.551(2) .
B1 N11 1.553(2) .
B1 H1 1.11(2) .
O1W H1W1 0.83(2) .
O1W H1W2 0.82(2) .
N11 N12 1.3566(19) .
N11 C15 1.361(2) .
N12 C13 1.335(2) .
C13 C14 1.396(2) .
C13 C131 1.488(2) .
C131 F11 1.326(2) .
C131 F12 1.329(2) .
C131 F13 1.348(2) .
C14 C15 1.380(2) .
C14 H14 0.9500 .
C15 C151 1.476(2) .
C151 C152 1.394(2) .
C151 C156 1.397(2) .
C152 C153 1.387(2) .
C152 H152 0.9500 .
C153 C154 1.385(2) .
C153 H153 0.9500 .
C154 C155 1.385(3) .
C154 N13 1.466(2) .
C155 C156 1.386(2) .
C155 H155 0.9500 .
C156 H156 0.9500 .
N13 O132 1.221(2) .
N13 O131 1.235(2) .
N21 C25 1.358(2) .
N21 N22 1.3603(18) .
N22 C23 1.335(2) .
C23 C24 1.391(2) .
C23 C231 1.491(2) .
C231 F22 1.321(2) .
C231 F23 1.337(2) .
C231 F21 1.340(2) .
C24 C25 1.381(2) .
C24 H24 0.9500 .
C25 C251 1.478(2) .
C251 C252 1.396(2) .
C251 C256 1.399(2) .
C252 C253 1.385(2) .
C252 H252 0.9500 .
C253 C254 1.381(2) .
C253 H253 0.9500 .
C254 C255 1.390(2) .
C254 N23 1.467(2) .
C255 C256 1.385(2) .
C255 H255 0.9500 .
C256 H256 0.9500 .
N23 O232 1.229(2) .
N23 O231 1.2331(19) .
N23 Na1 3.0416(15) 2_656
O231 Na1 2.5291(14) 2_656
O232 Na1 2.8633(14) 2_656
N31 N32 1.3551(19) .
N31 C35 1.362(2) .
N32 C33 1.344(2) .
C33 C34 1.404(2) .
C33 C331 1.469(2) .
C331 C332 1.399(2) .
C331 C336 1.403(2) .
C332 C333 1.385(2) .
C332 H332 0.9500 .
C333 C334 1.385(2) .
C333 H333 0.9500 .
C334 C335 1.384(2) .
C334 N33 1.470(2) .
C335 C336 1.385(2) .
C335 H335 0.9500 .
C336 H336 0.9500 .
C34 C35 1.372(2) .
C34 H34 0.9500 .
C35 C351 1.492(2) .
C351 F32 1.341(2) .
C351 F31 1.342(2) .
C351 F33 1.3468(19) .
N33 O332 1.228(2) .
N33 O331 1.229(2) .
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
O1W H1W1 O131 0.83(2) 2.03(2) 2.860(2) 172(3) 4_666
O1W H1W2 F13 0.82(2) 2.36(2) 3.1438(19) 159(3) 3_657
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
N21 B1 N11 N12 -37.49(19) .
N31 B1 N11 N12 84.42(17) .
N21 B1 N11 C15 132.16(15) .
N31 B1 N11 C15 -105.93(17) .
C15 N11 N12 C13 -0.70(17) .
B1 N11 N12 C13 170.39(14) .
C15 N11 N12 Na1 157.58(10) .
B1 N11 N12 Na1 -31.33(16) .
N11 N12 C13 C14 0.13(19) .
Na1 N12 C13 C14 -149.01(13) .
N11 N12 C13 C131 179.44(15) .
Na1 N12 C13 C131 30.3(3) .
N12 C13 C131 F11 -176.35(17) .
C14 C13 C131 F11 2.9(3) .
N12 C13 C131 F12 -55.3(2) .
C14 C13 C131 F12 123.9(2) .
N12 C13 C131 F13 64.0(2) .
C14 C13 C131 F13 -116.8(2) .
N12 C13 C14 C15 0.5(2) .
C131 C13 C14 C15 -178.79(17) .
N12 N11 C15 C14 1.01(18) .
B1 N11 C15 C14 -169.65(14) .
N12 N11 C15 C151 -174.09(14) .
B1 N11 C15 C151 15.3(2) .
C13 C14 C15 N11 -0.87(18) .
C13 C14 C15 C151 173.78(16) .
N11 C15 C151 C152 -130.40(17) .
C14 C15 C151 C152 55.6(2) .
N11 C15 C151 C156 53.1(2) .
C14 C15 C151 C156 -120.92(19) .
C156 C151 C152 C153 0.4(2) .
C15 C151 C152 C153 -176.10(15) .
C151 C152 C153 C154 -0.7(3) .
C152 C153 C154 C155 0.3(3) .
C152 C153 C154 N13 177.57(15) .
C153 C154 C155 C156 0.5(2) .
N13 C154 C155 C156 -176.83(15) .
C154 C155 C156 C151 -0.8(2) .
C152 C151 C156 C155 0.3(2) .
C15 C151 C156 C155 176.89(14) .
C155 C154 N13 O132 -14.2(2) .
C153 C154 N13 O132 168.42(16) .
C155 C154 N13 O131 164.63(16) .
C153 C154 N13 O131 -12.8(2) .
N31 B1 N21 C25 131.41(15) .
N11 B1 N21 C25 -106.89(17) .
N31 B1 N21 N22 -39.65(19) .
N11 B1 N21 N22 82.05(17) .
C25 N21 N22 C23 0.03(17) .
B1 N21 N22 C23 172.43(14) .
C25 N21 N22 Na1 155.14(10) .
B1 N21 N22 Na1 -32.46(16) .
N21 N22 C23 C24 -0.74(18) .
Na1 N22 C23 C24 -147.08(13) .
N21 N22 C23 C231 177.39(14) .
Na1 N22 C23 C231 31.0(2) .
N22 C23 C231 F22 -82.7(2) .
C24 C23 C231 F22 95.2(2) .
N22 C23 C231 F23 39.3(2) .
C24 C23 C231 F23 -142.86(18) .
N22 C23 C231 F21 157.62(15) .
C24 C23 C231 F21 -24.6(2) .
N22 C23 C24 C25 1.13(19) .
C231 C23 C24 C25 -176.83(16) .
N22 N21 C25 C24 0.67(18) .
B1 N21 C25 C24 -171.18(14) .
N22 N21 C25 C251 -178.20(14) .
B1 N21 C25 C251 10.0(2) .
C23 C24 C25 N21 -1.05(18) .
C23 C24 C25 C251 177.79(15) .
N21 C25 C251 C252 -131.00(17) .
C24 C25 C251 C252 50.3(2) .
N21 C25 C251 C256 52.8(2) .
C24 C25 C251 C256 -125.88(19) .
C256 C251 C252 C253 1.9(2) .
C25 C251 C252 C253 -174.41(15) .
C251 C252 C253 C254 -0.1(3) .
C252 C253 C254 C255 -1.9(3) .
C252 C253 C254 N23 175.48(15) .
C253 C254 C255 C256 2.0(2) .
N23 C254 C255 C256 -175.34(14) .
C254 C255 C256 C251 -0.1(2) .
C252 C251 C256 C255 -1.8(2) .
C25 C251 C256 C255 174.40(15) .
C253 C254 N23 O232 -1.2(2) .
C255 C254 N23 O232 176.20(15) .
C253 C254 N23 O231 179.70(15) .
C255 C254 N23 O231 -2.9(2) .
C253 C254 N23 Na1 120.0(4) 2_656
C255 C254 N23 Na1 -62.6(4) 2_656
O232 N23 O231 Na1 17.62(17) 2_656
C254 N23 O231 Na1 -163.34(11) 2_656
O231 N23 O232 Na1 -15.17(15) 2_656
C254 N23 O232 Na1 165.79(12) 2_656
N21 B1 N31 N32 87.05(16) .
N11 B1 N31 N32 -35.19(19) .
N21 B1 N31 C35 -99.34(17) .
N11 B1 N31 C35 138.42(15) .
C35 N31 N32 C33 -1.17(16) .
B1 N31 N32 C33 173.48(13) .
C35 N31 N32 Na1 149.59(10) .
B1 N31 N32 Na1 -35.76(15) .
N31 N32 C33 C34 1.19(17) .
Na1 N32 C33 C34 -137.92(13) .
N31 N32 C33 C331 -176.03(13) .
Na1 N32 C33 C331 44.9(2) .
N32 C33 C331 C332 5.7(2) .
C34 C33 C331 C332 -171.02(16) .
N32 C33 C331 C336 -176.49(14) .
C34 C33 C331 C336 6.8(2) .
C336 C331 C332 C333 -0.2(2) .
C33 C331 C332 C333 177.64(15) .
C331 C332 C333 C334 -0.6(3) .
C332 C333 C334 C335 0.7(3) .
C332 C333 C334 N33 -179.27(15) .
C333 C334 C335 C336 0.0(3) .
N33 C334 C335 C336 179.91(15) .
C334 C335 C336 C331 -0.7(2) .
C332 C331 C336 C335 0.9(2) .
C33 C331 C336 C335 -177.00(15) .
N32 C33 C34 C35 -0.75(18) .
C331 C33 C34 C35 176.26(15) .
N32 N31 C35 C34 0.72(17) .
B1 N31 C35 C34 -173.53(14) .
N32 N31 C35 C351 -179.11(14) .
B1 N31 C35 C351 6.6(2) .
C33 C34 C35 N31 0.01(17) .
C33 C34 C35 C351 179.84(15) .
N31 C35 C351 F32 -80.12(19) .
C34 C35 C351 F32 100.08(19) .
N31 C35 C351 F31 41.6(2) .
C34 C35 C351 F31 -138.23(16) .
N31 C35 C351 F33 160.88(14) .
C34 C35 C351 F33 -18.9(2) .
C335 C334 N33 O332 -4.6(2) .
C333 C334 N33 O332 175.37(16) .
C335 C334 N33 O331 175.87(16) .
C333 C334 N33 O331 -4.2(2) .
