#------------------------------------------------------------------------------
#$Date: 2015-12-09 15:53:49 +0200 (Wed, 09 Dec 2015) $
#$Revision: 171150 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/74/7037425.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_7037425
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         'C66 H36 B2 F36 N12 Na2 O2'
_chemical_formula_sum            'C66 H36 B2 F36 N12 Na2 O2'
_chemical_formula_weight         1780.67
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-08 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                109.484(2)
_cell_angle_beta                 104.948(2)
_cell_angle_gamma                102.991(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2747(2)
_cell_length_b                   12.5762(3)
_cell_length_c                   14.4865(3)
_cell_measurement_reflns_used    14448
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.01
_cell_measurement_theta_min      3.44
_cell_volume                     1758.61(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_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  0.0173
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22232
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.884
_diffrn_reflns_theta_min         3.472
_exptl_absorpt_coefficient_mu    1.645
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.752
_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    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0416P)²+0.7774P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6297
_reflns_number_total             6828
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt04006j2.cif
_cod_data_source_block           Na4b
_cod_depositor_comments
'Adding full bibliography for 7037416--7037425.cif.'
_cod_original_cell_volume        1758.61(7)
_cod_database_code               7037425
_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.
;
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_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_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
Na1 Na 0.06955(5) 0.66420(4) 0.04949(4) 0.02950(13) Uani 1 1 d . . . . .
B1 B 0.32447(13) 0.93738(12) 0.18859(11) 0.0212(3) Uani 1 1 d . . . . .
H1 H 0.4016(14) 1.0228(13) 0.2319(11) 0.020(3) Uiso 1 1 d . . . . .
N11 N 0.38395(10) 0.83658(9) 0.17983(8) 0.0215(2) Uani 1 1 d . . . . .
N12 N 0.30805(10) 0.71884(9) 0.12486(9) 0.0240(2) Uani 1 1 d . . . . .
C13 C 0.38888(13) 0.65815(12) 0.13732(11) 0.0267(3) Uani 1 1 d D . . . .
C14 C 0.51677(13) 0.73295(12) 0.20009(12) 0.0290(3) Uani 1 1 d . . . . .
H14 H 0.5911 0.7106 0.2205 0.035 Uiso 1 1 calc R U . . .
C15 C 0.51095(12) 0.84722(11) 0.22595(10) 0.0234(3) Uani 1 1 d . . . . .
C131 C 0.3403(13) 0.5243(6) 0.0877(10) 0.0323(8) Uani 0.41(2) 1 d D U P A 1
F11 F 0.3859(11) 0.4782(6) 0.1526(9) 0.065(2) Uani 0.41(2) 1 d D U P A 1
F12 F 0.3744(10) 0.4846(6) 0.0059(12) 0.064(3) Uani 0.41(2) 1 d D U P A 1
F13 F 0.2101(11) 0.4754(13) 0.0506(15) 0.044(2) Uani 0.41(2) 1 d D U P A 1
C13' C 0.3393(9) 0.5257(4) 0.0733(6) 0.0323(8) Uani 0.59(2) 1 d D U P A 2
F11' F 0.4131(4) 0.4718(3) 0.1118(8) 0.0598(17) Uani 0.59(2) 1 d D U P A 2
F12' F 0.3318(9) 0.4951(4) -0.0260(4) 0.0601(14) Uani 0.59(2) 1 d D U P A 2
F13' F 0.2180(8) 0.4762(9) 0.0687(11) 0.0450(17) Uani 0.59(2) 1 d D U P A 2
C151 C 0.62117(12) 0.96124(11) 0.29178(10) 0.0236(3) Uani 1 1 d . . . . .
C152 C 0.70596(13) 0.97315(13) 0.38691(11) 0.0292(3) Uani 1 1 d . . . . .
H152 H 0.6894 0.9100 0.4091 0.035 Uiso 1 1 calc R U . . .
C153 C 0.81389(14) 1.07610(14) 0.44917(11) 0.0331(3) Uani 1 1 d . . . . .
H153 H 0.8710 1.0832 0.5136 0.040 Uiso 1 1 calc R U . . .
C154 C 0.83883(13) 1.16882(12) 0.41774(11) 0.0304(3) Uani 1 1 d D . . . .
C155 C 0.75669(13) 1.15840(12) 0.32345(11) 0.0296(3) Uani 1 1 d . . . . .
H155 H 0.7740 1.2217 0.3016 0.036 Uiso 1 1 calc R U . . .
C156 C 0.64887(12) 1.05503(12) 0.26091(11) 0.0264(3) Uani 1 1 d . . . . .
H156 H 0.5930 1.0480 0.1960 0.032 Uiso 1 1 calc R U . . .
C157 C 0.95514(18) 1.28109(17) 0.48781(16) 0.0373(4) Uani 0.926(5) 1 d D U P B
1
F14 F 0.96184(18) 1.36781(14) 0.45660(13) 0.0665(6) Uani 0.926(5) 1 d D U P B 1
F15 F 0.95734(19) 1.32428(18) 0.58678(14) 0.0537(5) Uani 0.926(5) 1 d D U P B 1
F16 F 1.06721(11) 1.25787(14) 0.49667(15) 0.0584(6) Uani 0.926(5) 1 d D U P B 1
C15' C 0.9681(14) 1.2659(16) 0.4885(16) 0.0373(4) Uani 0.074(5) 1 d D U P B 2
F14' F 1.014(2) 1.3222(19) 0.4385(13) 0.061(6) Uani 0.074(5) 1 d D U P B 2
F15' F 0.936(2) 1.347(2) 0.5547(19) 0.055(5) Uani 0.074(5) 1 d D U P B 2
F16' F 1.056(2) 1.227(2) 0.535(2) 0.079(6) Uani 0.074(5) 1 d D U P B 2
N21 N 0.25382(10) 0.92947(9) 0.07776(8) 0.0230(2) Uani 1 1 d . . . . .
N22 N 0.14786(11) 0.83263(10) 0.00658(9) 0.0276(2) Uani 1 1 d . . . . .
C23 C 0.11075(14) 0.85634(13) -0.07668(11) 0.0318(3) Uani 1 1 d D . . . .
C24 C 0.19133(14) 0.96607(13) -0.06352(11) 0.0336(3) Uani 1 1 d . . . . .
H24 H 0.1854 1.0014 -0.1124 0.040 Uiso 1 1 calc R U . . .
C25 C 0.28171(13) 1.01152(12) 0.03682(11) 0.0262(3) Uani 1 1 d . . . . .
C231 C -0.0056(4) 0.7641(4) -0.1697(4) 0.0427(6) Uani 0.672(3) 1 d D U P C 1
F21 F -0.0629(4) 0.8140(3) -0.2270(3) 0.0839(15) Uani 0.672(3) 1 d D U P C 1
F22 F 0.0250(3) 0.6778(2) -0.23314(19) 0.0650(6) Uani 0.672(3) 1 d D U P C 1
F23 F -0.0964(3) 0.7069(3) -0.1416(3) 0.0571(9) Uani 0.672(3) 1 d D U P C 1
C23' C -0.0141(11) 0.7784(12) -0.1671(9) 0.0427(6) Uani 0.211(3) 1 d D U P C 2
F21' F -0.0987(9) 0.8323(10) -0.1823(8) 0.061(3) Uani 0.211(3) 1 d D U P C 2
F22' F 0.0061(7) 0.7318(10) -0.2551(5) 0.068(2) Uani 0.211(3) 1 d D U P C 2
F23' F -0.0695(11) 0.6827(11) -0.1534(11) 0.0571(9) Uani 0.211(3) 1 d D U P C 2
C23C C -0.0073(13) 0.7738(15) -0.1720(10) 0.0427(6) Uani 0.117(3) 1 d D U P C 3
F21C F -0.1138(10) 0.7652(16) -0.1507(10) 0.069(3) Uani 0.117(3) 1 d D U P C 3
F22C F -0.0146(14) 0.8010(17) -0.2535(12) 0.039(3) Uani 0.117(3) 1 d D U P C 3
F23C F -0.0124(11) 0.6603(10) -0.2070(11) 0.0571(9) Uani 0.117(3) 1 d D U P C 3
C251 C 0.39146(13) 1.12680(11) 0.09351(10) 0.0250(3) Uani 1 1 d . . . . .
C252 C 0.48188(15) 1.15435(13) 0.04762(11) 0.0326(3) Uani 1 1 d . . . . .
H252 H 0.4710 1.0994 -0.0201 0.039 Uiso 1 1 calc R U . . .
C253 C 0.58746(15) 1.26076(13) 0.09933(12) 0.0350(3) Uani 1 1 d . . . . .
H253 H 0.6485 1.2786 0.0674 0.042 Uiso 1 1 calc R U . . .
C254 C 0.60300(13) 1.34058(12) 0.19792(11) 0.0292(3) Uani 1 1 d D . . . .
C255 C 0.51290(14) 1.31517(12) 0.24406(11) 0.0296(3) Uani 1 1 d . . . . .
H255 H 0.5241 1.3704 0.3118 0.036 Uiso 1 1 calc R U . . .
C256 C 0.40719(13) 1.20992(12) 0.19179(11) 0.0272(3) Uani 1 1 d . . . . .
H256 H 0.3447 1.1939 0.2230 0.033 Uiso 1 1 calc R U . . .
C257 C 0.7167(5) 1.4559(4) 0.2594(5) 0.0382(4) Uani 0.696(16) 1 d D U P D 1
F24 F 0.7728(6) 1.4744(5) 0.3579(3) 0.0796(14) Uani 0.696(16) 1 d D U P D 1
F25 F 0.8100(4) 1.4609(4) 0.2195(5) 0.0764(14) Uani 0.696(16) 1 d D U P D 1
F26 F 0.6827(5) 1.5508(5) 0.2631(6) 0.0712(14) Uani 0.696(16) 1 d D U P D 1
C25' C 0.7152(11) 1.4563(9) 0.2532(11) 0.0382(4) Uani 0.304(16) 1 d D U P D 2
F24' F 0.8040(10) 1.4546(10) 0.3293(13) 0.082(3) Uani 0.304(16) 1 d D U P D 2
F25' F 0.7708(15) 1.4813(10) 0.1910(9) 0.085(3) Uani 0.304(16) 1 d D U P D 2
F26' F 0.6814(14) 1.5470(11) 0.2970(12) 0.076(3) Uani 0.304(16) 1 d D U P D 2
N31 N 0.22682(10) 0.93359(9) 0.24714(8) 0.0228(2) Uani 1 1 d . . . . .
N32 N 0.10824(11) 0.84513(10) 0.20147(9) 0.0265(2) Uani 1 1 d . . . . .
C33 C 0.03696(13) 0.88509(12) 0.25594(12) 0.0290(3) Uani 1 1 d D . . . .
C34 C 0.10536(13) 0.99892(12) 0.33700(11) 0.0289(3) Uani 1 1 d . . . . .
H34 H 0.0750 1.0463 0.3855 0.035 Uiso 1 1 calc R U . . .
C35 C 0.22768(12) 1.02687(11) 0.33031(10) 0.0237(3) Uani 1 1 d . . . . .
C331 C -0.0995(2) 0.8091(2) 0.23116(19) 0.0304(6) Uani 0.793(3) 1 d D U P E 1
F31 F -0.12551(12) 0.80534(16) 0.31393(12) 0.0556(5) Uani 0.793(3) 1 d D U P E
1
F32 F -0.1867(2) 0.8501(2) 0.18687(19) 0.0615(8) Uani 0.793(3) 1 d D U P E 1
F33 F -0.12581(17) 0.69712(14) 0.1656(2) 0.0741(8) Uani 0.793(3) 1 d D U P E 1
C33' C -0.1039(8) 0.8072(10) 0.2033(9) 0.0304(6) Uani 0.207(3) 1 d D U P E 2
F31' F -0.1607(6) 0.7588(6) 0.1013(5) 0.076(2) Uani 0.207(3) 1 d D U P E 2
F32' F -0.1737(11) 0.8658(10) 0.2342(11) 0.104(4) Uani 0.207(3) 1 d D U P E 2
F33' F -0.1198(7) 0.7198(8) 0.2327(9) 0.083(3) Uani 0.207(3) 1 d D U P E 2
C351 C 0.34477(12) 1.13178(11) 0.40380(10) 0.0237(3) Uani 1 1 d . . . . .
C352 C 0.33568(13) 1.24613(12) 0.43985(11) 0.0279(3) Uani 1 1 d . . . . .
H352 H 0.2545 1.2567 0.4149 0.033 Uiso 1 1 calc R U . . .
C353 C 0.44452(14) 1.34444(12) 0.51189(11) 0.0318(3) Uani 1 1 d . . . . .
H353 H 0.4378 1.4222 0.5363 0.038 Uiso 1 1 calc R U . . .
C354 C 0.56341(14) 1.32936(13) 0.54845(11) 0.0314(3) Uani 1 1 d D . . . .
C355 C 0.57303(14) 1.21567(13) 0.51468(11) 0.0309(3) Uani 1 1 d . . . . .
H355 H 0.6541 1.2053 0.5406 0.037 Uiso 1 1 calc R U . . .
C356 C 0.46421(13) 1.11758(12) 0.44310(10) 0.0274(3) Uani 1 1 d . . . . .
H356 H 0.4708 1.0397 0.4204 0.033 Uiso 1 1 calc R U . . .
C357 C 0.6819(8) 1.4332(8) 0.6277(9) 0.0422(7) Uani 0.35(2) 1 d D U P F 1
F34 F 0.7420(15) 1.4888(14) 0.5812(12) 0.074(3) Uani 0.35(2) 1 d D U P F 1
F35 F 0.6506(7) 1.5113(14) 0.6966(11) 0.068(3) Uani 0.35(2) 1 d D U P F 1
F36 F 0.7693(17) 1.4015(16) 0.6845(13) 0.060(3) Uani 0.35(2) 1 d D U P F 1
C35' C 0.6840(4) 1.4374(4) 0.6178(4) 0.0422(7) Uani 0.65(2) 1 d D U P F 2
F34' F 0.7594(7) 1.4635(7) 0.5659(5) 0.0677(13) Uani 0.65(2) 1 d D U P F 2
F35' F 0.6605(3) 1.5382(3) 0.6621(6) 0.0554(13) Uani 0.65(2) 1 d D U P F 2
F36' F 0.7587(9) 1.4195(9) 0.6959(7) 0.0580(14) Uani 0.65(2) 1 d D U P F 2
O1W O -0.00255(11) 0.51253(10) 0.11307(8) 0.0353(2) Uani 1 1 d D . . G 2
H1W1 H -0.0621(18) 0.5197(19) 0.1359(16) 0.053 Uiso 1 1 d D U . H 2
H1W2 H 0.0579(18) 0.5153(19) 0.1633(16) 0.053 Uiso 1 1 d D U . I 2
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 N32 171.97(5) 2_565 .
O1W Na1 N22 104.57(4) 2_565 .
N32 Na1 N22 73.79(4) . .
O1W Na1 O1W 82.03(4) 2_565 .
N32 Na1 O1W 99.69(4) . .
N22 Na1 O1W 173.40(4) . .
O1W Na1 N12 104.30(4) 2_565 .
N32 Na1 N12 83.15(4) . .
N22 Na1 N12 77.63(4) . .
O1W Na1 N12 100.89(4) . .
N32 Na1 F13 109.9(3) . 2_565
N22 Na1 F13 117.2(3) . 2_565
N12 Na1 F13 162.1(3) . 2_565
O1W Na1 Na1 41.26(3) 2_565 2_565
N32 Na1 Na1 139.91(4) . 2_565
N22 Na1 Na1 145.83(4) . 2_565
O1W Na1 Na1 40.77(3) . 2_565
N12 Na1 Na1 106.78(3) . 2_565
F13 Na1 Na1 55.3(3) 2_565 2_565
N11 B1 N31 112.44(10) . .
N11 B1 N21 110.63(10) . .
N31 B1 N21 109.12(10) . .
N11 B1 H1 109.0(8) . .
N31 B1 H1 107.7(8) . .
N21 B1 H1 107.8(8) . .
N12 N11 C15 110.29(10) . .
N12 N11 B1 121.33(10) . .
C15 N11 B1 128.32(10) . .
C13 N12 N11 105.28(10) . .
C13 N12 Na1 134.70(9) . .
N11 N12 Na1 119.46(8) . .
N12 C13 C14 112.56(12) . .
N12 C13 C131 121.0(5) . .
C14 C13 C131 126.5(5) . .
N12 C13 C13' 118.5(4) . .
C14 C13 C13' 128.3(4) . .
C15 C14 C13 104.12(12) . .
C15 C14 H14 127.9 . .
C13 C14 H14 127.9 . .
N11 C15 C14 107.74(11) . .
N11 C15 C151 125.69(11) . .
C14 C15 C151 126.57(12) . .
F12 C131 F11 107.8(8) . .
F12 C131 F13 105.1(10) . .
F11 C131 F13 106.8(11) . .
F12 C131 C13 110.4(8) . .
F11 C131 C13 112.8(7) . .
F13 C131 C13 113.6(10) . .
C131 F13 Na1 171.5(10) . 2_565
F11' C13' F12' 106.0(5) . .
F11' C13' F13' 107.6(7) . .
F12' C13' F13' 106.0(7) . .
F11' C13' C13 112.5(5) . .
F12' C13' C13 113.6(5) . .
F13' C13' C13 110.6(7) . .
C156 C151 C152 118.33(12) . .
C156 C151 C15 123.16(12) . .
C152 C151 C15 118.41(12) . .
C153 C152 C151 120.63(13) . .
C153 C152 H152 119.7 . .
C151 C152 H152 119.7 . .
C152 C153 C154 120.16(13) . .
C152 C153 H153 119.9 . .
C154 C153 H153 119.9 . .
C155 C154 C153 120.11(13) . .
C155 C154 C15' 127.1(9) . .
C153 C154 C15' 112.3(9) . .
C155 C154 C157 120.62(15) . .
C153 C154 C157 119.27(14) . .
C154 C155 C156 119.69(13) . .
C154 C155 H155 120.2 . .
C156 C155 H155 120.2 . .
C155 C156 C151 121.07(12) . .
C155 C156 H156 119.5 . .
C151 C156 H156 119.5 . .
F14 C157 F16 107.62(18) . .
F14 C157 F15 107.69(18) . .
F16 C157 F15 104.35(17) . .
F14 C157 C154 114.33(16) . .
F16 C157 C154 110.97(15) . .
F15 C157 C154 111.33(17) . .
F14' C15' F16' 110.1(18) . .
F14' C15' F15' 103.5(18) . .
F16' C15' F15' 114(2) . .
F14' C15' C154 111.0(14) . .
F16' C15' C154 113.9(16) . .
F15' C15' C154 103.3(16) . .
N22 N21 C25 110.22(10) . .
N22 N21 B1 121.05(10) . .
C25 N21 B1 128.72(10) . .
C23 N22 N21 105.32(10) . .
C23 N22 Na1 134.61(9) . .
N21 N22 Na1 120.07(8) . .
N22 C23 C24 112.65(12) . .
N22 C23 C23' 121.6(7) . .
C24 C23 C23' 125.4(7) . .
N22 C23 C23C 122.4(8) . .
C24 C23 C23C 124.9(8) . .
N22 C23 C231 117.6(3) . .
C24 C23 C231 129.7(3) . .
C25 C24 C23 103.96(12) . .
C25 C24 H24 128.0 . .
C23 C24 H24 128.0 . .
N21 C25 C24 107.85(11) . .
N21 C25 C251 124.15(12) . .
C24 C25 C251 128.00(12) . .
F21 C231 F23 107.1(4) . .
F21 C231 F22 107.5(4) . .
F23 C231 F22 105.8(4) . .
F21 C231 C23 110.9(4) . .
F23 C231 C23 112.4(4) . .
F22 C231 C23 112.8(4) . .
F21' C23' F22' 108.6(11) . .
F21' C23' F23' 108.4(12) . .
F22' C23' F23' 103.3(12) . .
F21' C23' C23 114.0(10) . .
F22' C23' C23 111.8(10) . .
F23' C23' C23 110.1(11) . .
F21C C23C F22C 112.1(14) . .
F21C C23C F23C 101.5(14) . .
F22C C23C F23C 104.4(14) . .
F21C C23C C23 111.3(12) . .
F22C C23C C23 113.3(13) . .
F23C C23C C23 113.5(13) . .
C256 C251 C252 118.68(12) . .
C256 C251 C25 121.90(12) . .
C252 C251 C25 119.41(12) . .
C253 C252 C251 121.02(13) . .
C253 C252 H252 119.5 . .
C251 C252 H252 119.5 . .
C254 C253 C252 119.32(13) . .
C254 C253 H253 120.3 . .
C252 C253 H253 120.3 . .
C253 C254 C255 120.34(13) . .
C253 C254 C25' 119.6(6) . .
C255 C254 C25' 120.1(6) . .
C253 C254 C257 122.2(3) . .
C255 C254 C257 117.5(3) . .
C256 C255 C254 120.13(13) . .
C256 C255 H255 119.9 . .
C254 C255 H255 119.9 . .
C255 C256 C251 120.46(12) . .
C255 C256 H256 119.8 . .
C251 C256 H256 119.8 . .
F24 C257 F26 106.0(5) . .
F24 C257 F25 106.2(4) . .
F26 C257 F25 105.8(5) . .
F24 C257 C254 112.9(4) . .
F26 C257 C254 112.5(5) . .
F25 C257 C254 112.9(4) . .
F24' C25' F26' 105.0(11) . .
F24' C25' F25' 107.6(11) . .
F26' C25' F25' 107.3(11) . .
F24' C25' C254 111.3(10) . .
F26' C25' C254 112.6(11) . .
F25' C25' C254 112.7(10) . .
N32 N31 C35 110.03(10) . .
N32 N31 B1 120.82(10) . .
C35 N31 B1 126.73(10) . .
C33 N32 N31 105.48(11) . .
C33 N32 Na1 135.09(9) . .
N31 N32 Na1 119.41(8) . .
N32 C33 C34 112.59(12) . .
N32 C33 C331 121.04(15) . .
C34 C33 C331 126.32(16) . .
N32 C33 C33' 111.7(5) . .
C34 C33 C33' 134.5(5) . .
C35 C34 C33 103.78(12) . .
C35 C34 H34 128.1 . .
C33 C34 H34 128.1 . .
N31 C35 C34 108.09(11) . .
N31 C35 C351 124.15(11) . .
C34 C35 C351 127.52(12) . .
F31 C331 F33 107.1(2) . .
F31 C331 F32 104.6(2) . .
F33 C331 F32 107.6(2) . .
F31 C331 C33 114.33(18) . .
F33 C331 C33 111.3(2) . .
F32 C331 C33 111.5(2) . .
F32' C33' F33' 107.0(12) . .
F32' C33' F31' 103.3(10) . .
F33' C33' F31' 106.5(9) . .
F32' C33' C33 109.8(10) . .
F33' C33' C33 108.1(8) . .
F31' C33' C33 121.2(8) . .
C352 C351 C356 119.04(12) . .
C352 C351 C35 120.13(12) . .
C356 C351 C35 120.72(12) . .
C353 C352 C351 120.32(13) . .
C353 C352 H352 119.8 . .
C351 C352 H352 119.8 . .
C352 C353 C354 120.00(13) . .
C352 C353 H353 120.0 . .
C354 C353 H353 120.0 . .
C355 C354 C353 120.18(13) . .
C355 C354 C357 118.5(4) . .
C353 C354 C357 121.3(4) . .
C355 C354 C35' 119.9(2) . .
C353 C354 C35' 119.8(2) . .
C356 C355 C354 119.75(13) . .
C356 C355 H355 120.1 . .
C354 C355 H355 120.1 . .
C355 C356 C351 120.68(12) . .
C355 C356 H356 119.7 . .
C351 C356 H356 119.7 . .
F34 C357 F35 108.8(8) . .
F34 C357 F36 106.9(9) . .
F35 C357 F36 105.8(8) . .
F34 C357 C354 110.6(10) . .
F35 C357 C354 111.1(6) . .
F36 C357 C354 113.3(12) . .
F34' C35' F35' 105.0(4) . .
F34' C35' F36' 106.0(5) . .
F35' C35' F36' 107.1(4) . .
F34' C35' C354 112.4(5) . .
F35' C35' C354 114.4(4) . .
F36' C35' C354 111.3(6) . .
Na1 O1W Na1 97.97(4) 2_565 .
Na1 O1W H1W1 114.0(15) 2_565 .
Na1 O1W H1W1 113.7(14) . .
Na1 O1W H1W2 114.1(14) 2_565 .
Na1 O1W H1W2 112.5(14) . .
H1W1 O1W H1W2 104.9(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na1 O1W 2.4274(12) 2_565
Na1 N32 2.4355(12) .
Na1 N22 2.4440(12) .
Na1 O1W 2.4512(12) .
Na1 N12 2.4595(12) .
Na1 F13 2.930(12) 2_565
Na1 Na1 3.6810(10) 2_565
B1 N11 1.5465(17) .
B1 N31 1.5553(17) .
B1 N21 1.5557(17) .
B1 H1 1.073(15) .
N11 N12 1.3605(14) .
N11 C15 1.3694(16) .
N12 C13 1.3287(17) .
C13 C14 1.3907(19) .
C13 C131 1.491(6) .
C13 C13' 1.494(5) .
C14 C15 1.3805(18) .
C14 H14 0.9500 .
C15 C151 1.4783(17) .
C131 F12 1.315(11) .
C131 F11 1.316(11) .
C131 F13 1.337(12) .
F13 Na1 2.930(12) 2_565
C13' F11' 1.315(8) .
C13' F12' 1.333(7) .
C13' F13' 1.343(8) .
C151 C156 1.3953(18) .
C151 C152 1.3978(19) .
C152 C153 1.385(2) .
C152 H152 0.9500 .
C153 C154 1.385(2) .
C153 H153 0.9500 .
C154 C155 1.383(2) .
C154 C15' 1.503(10) .
C154 C157 1.506(2) .
C155 C156 1.3872(19) .
C155 H155 0.9500 .
C156 H156 0.9500 .
C157 F14 1.307(2) .
C157 F16 1.344(2) .
C157 F15 1.344(2) .
C15' F14' 1.293(18) .
C15' F16' 1.325(18) .
C15' F15' 1.333(18) .
N21 N22 1.3589(15) .
N21 C25 1.3689(16) .
N22 C23 1.3245(18) .
C23 C24 1.3920(19) .
C23 C23' 1.493(8) .
C23 C23C 1.493(8) .
C23 C231 1.498(3) .
C24 C25 1.3776(19) .
C24 H24 0.9500 .
C25 C251 1.4773(17) .
C231 F21 1.324(6) .
C231 F23 1.345(6) .
C231 F22 1.345(6) .
C23' F21' 1.304(14) .
C23' F22' 1.317(15) .
C23' F23' 1.328(15) .
C23C F21C 1.305(16) .
C23C F22C 1.323(16) .
C23C F23C 1.328(17) .
C251 C256 1.3946(19) .
C251 C252 1.3948(19) .
C252 C253 1.387(2) .
C252 H252 0.9500 .
C253 C254 1.383(2) .
C253 H253 0.9500 .
C254 C255 1.388(2) .
C254 C25' 1.494(7) .
C254 C257 1.501(4) .
C255 C256 1.3793(19) .
C255 H255 0.9500 .
C256 H256 0.9500 .
C257 F24 1.318(6) .
C257 F26 1.323(6) .
C257 F25 1.324(6) .
C25' F24' 1.294(14) .
C25' F26' 1.299(14) .
C25' F25' 1.302(14) .
N31 N32 1.3590(15) .
N31 C35 1.3689(17) .
N32 C33 1.3286(18) .
C33 C34 1.3922(19) .
C33 C331 1.495(2) .
C33 C33' 1.497(8) .
C34 C35 1.3815(19) .
C34 H34 0.9500 .
C35 C351 1.4737(18) .
C331 F31 1.319(3) .
C331 F33 1.322(3) .
C331 F32 1.330(3) .
C33' F32' 1.259(13) .
C33' F33' 1.297(12) .
C33' F31' 1.304(12) .
C351 C352 1.3944(18) .
C351 C356 1.3964(19) .
C352 C353 1.3856(19) .
C352 H352 0.9500 .
C353 C354 1.389(2) .
C353 H353 0.9500 .
C354 C355 1.388(2) .
C354 C357 1.494(7) .
C354 C35' 1.503(4) .
C355 C356 1.383(2) .
C355 H355 0.9500 .
C356 H356 0.9500 .
C357 F34 1.319(7) .
C357 F35 1.330(7) .
C357 F36 1.336(7) .
C35' F34' 1.328(4) .
C35' F35' 1.336(4) .
C35' F36' 1.343(4) .
O1W Na1 2.4273(12) 2_565
O1W H1W1 0.831(18) .
O1W H1W2 0.844(18) .
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
N31 B1 N11 N12 63.37(14)
N21 B1 N11 N12 -58.92(14)
N31 B1 N11 C15 -113.43(13)
N21 B1 N11 C15 124.28(13)
C15 N11 N12 C13 -0.19(14)
B1 N11 N12 C13 -177.52(11)
C15 N11 N12 Na1 172.45(8)
B1 N11 N12 Na1 -4.88(14)
N11 N12 C13 C14 0.48(15)
Na1 N12 C13 C14 -170.49(10)
N11 N12 C13 C131 180.0(6)
Na1 N12 C13 C131 9.0(7)
N11 N12 C13 C13' -171.1(4)
Na1 N12 C13 C13' 18.0(4)
N12 C13 C14 C15 -0.58(16)
C131 C13 C14 C15 180.0(7)
C13' C13 C14 C15 170.0(4)
N12 N11 C15 C14 -0.16(14)
B1 N11 C15 C14 176.93(12)
N12 N11 C15 C151 180.00(12)
B1 N11 C15 C151 -2.9(2)
C13 C14 C15 N11 0.42(15)
C13 C14 C15 C151 -179.74(12)
N12 C13 C131 F12 104.9(11)
C14 C13 C131 F12 -75.7(10)
C13' C13 C131 F12 30(5)
N12 C13 C131 F11 -134.5(9)
C14 C13 C131 F11 44.9(12)
C13' C13 C131 F11 150(7)
N12 C13 C131 F13 -12.9(16)
C14 C13 C131 F13 166.5(11)
C13' C13 C131 F13 -88(6)
N12 C13 C13' F11' -162.4(6)
C14 C13 C13' F11' 27.6(9)
C131 C13 C13' F11' -53(6)
N12 C13 C13' F12' 77.1(8)
C14 C13 C13' F12' -92.9(7)
C131 C13 C13' F12' -173(7)
N12 C13 C13' F13' -42.0(10)
C14 C13 C13' F13' 148.0(7)
C131 C13 C13' F13' 67(6)
N11 C15 C151 C156 -50.63(19)
C14 C15 C151 C156 129.57(15)
N11 C15 C151 C152 133.01(14)
C14 C15 C151 C152 -46.80(19)
C156 C151 C152 C153 0.6(2)
C15 C151 C152 C153 177.16(13)
C151 C152 C153 C154 0.1(2)
C152 C153 C154 C155 -0.7(2)
C152 C153 C154 C15' -173.1(10)
C152 C153 C154 C157 178.67(15)
C153 C154 C155 C156 0.4(2)
C15' C154 C155 C156 171.6(11)
C157 C154 C155 C156 -178.93(15)
C154 C155 C156 C151 0.4(2)
C152 C151 C156 C155 -0.9(2)
C15 C151 C156 C155 -177.26(12)
C155 C154 C157 F14 6.4(2)
C153 C154 C157 F14 -172.91(18)
C15' C154 C157 F14 138(6)
C155 C154 C157 F16 -115.5(2)
C153 C154 C157 F16 65.2(2)
C15' C154 C157 F16 16(5)
C155 C154 C157 F15 128.7(2)
C153 C154 C157 F15 -50.6(3)
C15' C154 C157 F15 -99(5)
C155 C154 C15' F14' -19(2)
C153 C154 C15' F14' 153.2(16)
C157 C154 C15' F14' -72(5)
C155 C154 C15' F16' -143.4(17)
C153 C154 C15' F16' 28(2)
C157 C154 C15' F16' 163(7)
C155 C154 C15' F15' 92(2)
C153 C154 C15' F15' -96(2)
C157 C154 C15' F15' 38(5)
N11 B1 N21 N22 63.55(15)
N31 B1 N21 N22 -60.66(14)
N11 B1 N21 C25 -117.58(14)
N31 B1 N21 C25 118.22(14)
C25 N21 N22 C23 -0.67(15)
B1 N21 N22 C23 178.40(12)
C25 N21 N22 Na1 178.91(9)
B1 N21 N22 Na1 -2.03(15)
N21 N22 C23 C24 1.22(17)
Na1 N22 C23 C24 -178.26(11)
N21 N22 C23 C23' -171.6(7)
Na1 N22 C23 C23' 8.9(7)
N21 N22 C23 C23C -177.3(9)
Na1 N22 C23 C23C 3.2(9)
N21 N22 C23 C231 179.8(3)
Na1 N22 C23 C231 0.4(3)
N22 C23 C24 C25 -1.29(19)
C23' C23 C24 C25 171.2(7)
C23C C23 C24 C25 177.2(10)
C231 C23 C24 C25 -179.7(3)
N22 N21 C25 C24 -0.12(16)
B1 N21 C25 C24 -179.09(13)
N22 N21 C25 C251 -179.65(12)
B1 N21 C25 C251 1.4(2)
C23 C24 C25 N21 0.80(17)
C23 C24 C25 C251 -179.68(14)
N22 C23 C231 F21 154.9(4)
C24 C23 C231 F21 -26.7(7)
C23' C23 C231 F21 35(6)
C23C C23 C231 F21 2(9)
N22 C23 C231 F23 35.1(5)
C24 C23 C231 F23 -146.5(3)
C23' C23 C231 F23 -85(6)
C23C C23 C231 F23 -118(10)
N22 C23 C231 F22 -84.4(5)
C24 C23 C231 F22 93.9(5)
C23' C23 C231 F22 156(6)
C23C C23 C231 F22 122(10)
N22 C23 C23' F21' 116.6(11)
C24 C23 C23' F21' -55.3(15)
C23C C23 C23' F21' -141(12)
C231 C23 C23' F21' -179(100)
N22 C23 C23' F22' -119.7(12)
C24 C23 C23' F22' 68.4(14)
C23C C23 C23' F22' -18(11)
C231 C23 C23' F22' -55(5)
N22 C23 C23' F23' -5.5(15)
C24 C23 C23' F23' -177.4(8)
C23C C23 C23' F23' 96(12)
C231 C23 C23' F23' 59(5)
N22 C23 C23C F21C 64.6(18)
C24 C23 C23C F21C -113.7(15)
C23' C23 C23C F21C -16(11)
C231 C23 C23C F21C 93(10)
N22 C23 C23C F22C -168.0(12)
C24 C23 C23C F22C 14(2)
C23' C23 C23C F22C 111(12)
C231 C23 C23C F22C -140(11)
N22 C23 C23C F23C -49.1(17)
C24 C23 C23C F23C 132.6(13)
C23' C23 C23C F23C -130(13)
C231 C23 C23C F23C -21(9)
N21 C25 C251 C256 -55.32(19)
C24 C25 C251 C256 125.24(17)
N21 C25 C251 C252 125.12(15)
C24 C25 C251 C252 -54.3(2)
C256 C251 C252 C253 1.6(2)
C25 C251 C252 C253 -178.83(13)
C251 C252 C253 C254 0.0(2)
C252 C253 C254 C255 -0.8(2)
C252 C253 C254 C25' -178.9(7)
C252 C253 C254 C257 178.5(3)
C253 C254 C255 C256 0.1(2)
C25' C254 C255 C256 178.1(7)
C257 C254 C255 C256 -179.3(3)
C254 C255 C256 C251 1.6(2)
C252 C251 C256 C255 -2.4(2)
C25 C251 C256 C255 178.05(12)
C253 C254 C257 F24 -132.8(5)
C255 C254 C257 F24 46.5(7)
C25' C254 C257 F24 -174(15)
C253 C254 C257 F26 107.3(6)
C255 C254 C257 F26 -73.3(6)
C25' C254 C257 F26 66(14)
C253 C254 C257 F25 -12.3(7)
C255 C254 C257 F25 167.0(5)
C25' C254 C257 F25 -54(14)
C253 C254 C25' F24' -106.3(12)
C255 C254 C25' F24' 75.6(15)
C257 C254 C25' F24' 34(14)
C253 C254 C25' F26' 136.2(12)
C255 C254 C25' F26' -41.9(16)
C257 C254 C25' F26' -84(14)
C253 C254 C25' F25' 14.7(16)
C255 C254 C25' F25' -163.4(11)
C257 C254 C25' F25' 155(15)
N11 B1 N31 N32 -71.15(14)
N21 B1 N31 N32 51.99(14)
N11 B1 N31 C35 128.36(12)
N21 B1 N31 C35 -108.50(13)
C35 N31 N32 C33 0.66(14)
B1 N31 N32 C33 -162.79(11)
C35 N31 N32 Na1 179.67(8)
B1 N31 N32 Na1 16.23(14)
N31 N32 C33 C34 0.27(16)
Na1 N32 C33 C34 -178.51(10)
N31 N32 C33 C331 -177.44(15)
Na1 N32 C33 C331 3.8(2)
N31 N32 C33 C33' 169.7(5)
Na1 N32 C33 C33' -9.1(5)
N32 C33 C34 C35 -1.06(16)
C331 C33 C34 C35 176.50(17)
C33' C33 C34 C35 -167.3(6)
N32 N31 C35 C34 -1.35(14)
B1 N31 C35 C34 160.88(12)
N32 N31 C35 C351 173.40(11)
B1 N31 C35 C351 -24.38(19)
C33 C34 C35 N31 1.41(15)
C33 C34 C35 C351 -173.10(13)
N32 C33 C331 F31 132.9(2)
C34 C33 C331 F31 -44.5(3)
C33' C33 C331 F31 -173(2)
N32 C33 C331 F33 11.3(3)
C34 C33 C331 F33 -166.1(2)
C33' C33 C331 F33 65(2)
N32 C33 C331 F32 -108.7(2)
C34 C33 C331 F32 73.9(3)
C33' C33 C331 F32 -55(2)
N32 C33 C33' F32' -157.6(10)
C34 C33 C33' F32' 8.7(14)
C331 C33 C33' F32' 71(2)
N32 C33 C33' F33' 86.0(10)
C34 C33 C33' F33' -107.7(10)
C331 C33 C33' F33' -45.8(19)
N32 C33 C33' F31' -37.3(12)
C34 C33 C33' F31' 129.0(9)
C331 C33 C33' F31' -169(3)
N31 C35 C351 C352 140.20(13)
C34 C35 C351 C352 -46.1(2)
N31 C35 C351 C356 -43.63(18)
C34 C35 C351 C356 130.07(15)
C356 C351 C352 C353 1.4(2)
C35 C351 C352 C353 177.65(13)
C351 C352 C353 C354 0.1(2)
C352 C353 C354 C355 -1.3(2)
C352 C353 C354 C357 -178.8(7)
C352 C353 C354 C35' 173.7(3)
C353 C354 C355 C356 1.1(2)
C357 C354 C355 C356 178.6(6)
C35' C354 C355 C356 -174.0(3)
C354 C355 C356 C351 0.4(2)
C352 C351 C356 C355 -1.7(2)
C35 C351 C356 C355 -177.89(13)
C355 C354 C357 F34 97.3(13)
C353 C354 C357 F34 -85.1(10)
C35' C354 C357 F34 -6(4)
C355 C354 C357 F35 -141.7(11)
C353 C354 C357 F35 35.8(12)
C35' C354 C357 F35 115(5)
C355 C354 C357 F36 -22.8(13)
C353 C354 C357 F36 154.8(9)
C35' C354 C357 F36 -127(5)
C355 C354 C35' F34' 73.1(6)
C353 C354 C35' F34' -101.9(5)
C357 C354 C35' F34' 153(5)
C355 C354 C35' F35' -167.3(5)
C353 C354 C35' F35' 17.7(7)
C357 C354 C35' F35' -87(5)
C355 C354 C35' F36' -45.7(6)
C353 C354 C35' F36' 139.3(5)
C357 C354 C35' F36' 34(5)
