#------------------------------------------------------------------------------
#$Date: 2017-06-28 09:15:53 +0300 (Wed, 28 Jun 2017) $
#$Revision: 198199 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/85/7228574.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_7228574
loop_
_publ_author_name
'Carreras, Lucas'
'Rovira, Laura'
'Vaquero, Mónica'
'Mon, Ignasi'
'Martin, Eddy'
'Benet-Buchholz, Jordi'
'Vidal-Ferran, Anton'
_publ_section_title
;
 Syntheses, characterisation and solid-state study of alkali and ammonium
 BArF salts
;
_journal_issue                   52
_journal_name_full               'RSC Adv.'
_journal_page_first              32833
_journal_paper_doi               10.1039/C7RA05928K
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C32 H18.76 B Cl0 F24 Na O2.38'
_chemical_formula_weight         931.11
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-25 deposited with the CCDC.
2017-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5537(7)
_cell_length_b                   13.5537(7)
_cell_length_c                   9.7850(7)
_cell_measurement_reflns_used    2165
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.57
_cell_volume                     1797.53(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9218
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.503
_diffrn_reflns_theta_min         2.081
_diffrn_source                   'Microfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2249
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0986P)²+1.6780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1726
_refine_ls_wR_factor_ref         0.1984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1544
_reflns_number_total             2249
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ra05928k2.cif
_cod_data_source_block           mo_MV198_0m
_cod_original_cell_volume        1797.5(2)
_cod_database_code               7228574
_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. 
;
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.980
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -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 0.2500 1.2500 0.1608(2) 0.0423(6) Uani 1 4 d S T P . .
O1 O 0.2500 1.2500 -0.0633(4) 0.0417(9) Uani 1 4 d DS T P . .
H1O H 0.212(3) 1.284(4) -0.115(3) 0.063 Uiso 1 1 d D U . . .
B1 B 0.2500 0.7500 0.5000 0.0242(10) Uani 1 4 d S T P . .
C1 C 0.1829(4) 0.8220(7) 0.4006(8) 0.0207(9) Uani 0.7 1 d D U P A 1
C6 C 0.2297(4) 0.8733(7) 0.2943(8) 0.0277(10) Uani 0.7 1 d D U P A 1
H6 H 0.2984 0.8639 0.2798 0.033 Uiso 0.7 1 calc R U P A 1
C5 C 0.1783(4) 0.9375(5) 0.2094(6) 0.0329(9) Uani 0.7 1 d D U P A 1
C4 C 0.0782(4) 0.9524(6) 0.2233(7) 0.0331(10) Uani 0.7 1 d D U P A 1
H4 H 0.0436 0.9960 0.1644 0.040 Uiso 0.7 1 calc R U P A 1
C3 C 0.0299(4) 0.9015(9) 0.3262(10) 0.0298(9) Uani 0.7 1 d D U P A 1
C2 C 0.0815(5) 0.8382(9) 0.4127(10) 0.0241(10) Uani 0.7 1 d D U P A 1
H2 H 0.0463 0.8047 0.4827 0.029 Uiso 0.7 1 calc R U P A 1
C8 C 0.2350(3) 0.9964(3) 0.1057(4) 0.0421(9) Uani 0.7 1 d D U P A 1
C7 C -0.0788(4) 0.9139(5) 0.3438(7) 0.0420(11) Uani 0.7 1 d D U P A 1
F4 F 0.27958(17) 1.07577(15) 0.1596(2) 0.0422(6) Uani 0.7 1 d D U P A 1
F5 F 0.1750(3) 1.0295(3) 0.0037(4) 0.0685(11) Uani 0.7 1 d D U P A 1
F6 F 0.3055(4) 0.9437(3) 0.0462(4) 0.0802(13) Uani 0.7 1 d D U P A 1
F1 F -0.1096(6) 1.0001(3) 0.2949(6) 0.0635(14) Uani 0.7 1 d D U P A 1
F2 F -0.1077(5) 0.9092(4) 0.4730(5) 0.0647(15) Uani 0.7 1 d D U P A 1
F3 F -0.1248(5) 0.8447(4) 0.2735(6) 0.0827(18) Uani 0.7 1 d D U P A 1
C1' C 0.1911(12) 0.822(3) 0.400(3) 0.039(3) Uani 0.3 1 d D U P A 2
C6' C 0.2374(11) 0.871(2) 0.291(3) 0.046(3) Uani 0.3 1 d D U P A 2
H6' H 0.3063 0.8622 0.2776 0.055 Uiso 0.3 1 calc R U P A 2
C5' C 0.1859(9) 0.9322(18) 0.2013(19) 0.054(2) Uani 0.3 1 d D U P A 2
C4' C 0.0858(9) 0.947(2) 0.217(2) 0.048(3) Uani 0.3 1 d D U P A 2
H4' H 0.0507 0.9886 0.1553 0.058 Uiso 0.3 1 calc R U P A 2
C3' C 0.0378(10) 0.900(3) 0.323(3) 0.041(2) Uani 0.3 1 d D U P A 2
C2' C 0.0894(12) 0.837(3) 0.410(3) 0.039(3) Uani 0.3 1 d D U P A 2
H2' H 0.0541 0.8028 0.4793 0.046 Uiso 0.3 1 calc R U P A 2
C8' C 0.2385(7) 0.9659(8) 0.0737(11) 0.072(2) Uani 0.3 1 d D U P A 2
C7' C -0.0718(8) 0.9078(10) 0.3403(13) 0.042(2) Uani 0.3 1 d D U P A 2
F4' F 0.2049(8) 1.0544(6) 0.0327(13) 0.088(3) Uani 0.3 1 d D U P A 2
F5' F 0.2297(7) 0.9107(6) -0.0430(9) 0.092(2) Uani 0.3 1 d D U P A 2
F6' F 0.3371(6) 0.9714(8) 0.0852(13) 0.084(3) Uani 0.3 1 d D U P A 2
F1' F -0.1201(14) 0.9742(7) 0.2629(13) 0.067(3) Uani 0.3 1 d D U P A 2
F2' F -0.0983(12) 0.9337(8) 0.4712(10) 0.046(3) Uani 0.3 1 d D U P A 2
F3' F -0.1271(11) 0.8233(6) 0.3255(10) 0.050(2) Uani 0.3 1 d D U P A 2
O2' O 0.2500 1.2500 0.3915(7) 0.053(2) Uani 0.620(12) 4 d S T P A 2
H2A' H 0.2634 1.3076 0.4205 0.080 Uiso 0.310(6) 1 d R U P A 2
O2 O 0.1384(13) 1.2385(16) 0.334(2) 0.104(8) Uani 0.190(6) 1 d . . P A 1
H1A H 0.1253 1.1690 0.3616 0.156 Uiso 0.190(6) 1 d R U P A 1
H2B H 0.0974 1.3002 0.3643 0.156 Uiso 0.190(6) 1 d R U P A 1
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
Cl Cl 0.1484 0.1585 '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
O1 Na1 O2' 180.0 . .
O1 Na1 O2 138.0(5) . .
O1 Na1 O2 138.0(5) . 2_575
O2 Na1 O2 83.9(11) . 2_575
O1 Na1 O2 138.0(5) . 4_465
O2 Na1 O2 56.4(6) . 4_465
O2 Na1 O2 56.4(6) 2_575 4_465
O1 Na1 O2 138.0(5) . 3_665
O2 Na1 O2 56.4(6) . 3_665
O2 Na1 O2 56.4(6) 2_575 3_665
O2 Na1 O2 83.9(10) 4_465 3_665
O1 Na1 F4 89.71(8) . .
O2 Na1 F4 92.7(6) . .
O2 Na1 F4 87.7(6) 2_575 .
O2 Na1 F4 132.1(5) 4_465 .
O2 Na1 F4 48.4(5) 3_665 .
O1 Na1 F4 89.71(8) . 3_665
O2 Na1 F4 132.1(5) . 3_665
O2 Na1 F4 48.4(5) 2_575 3_665
O2 Na1 F4 87.7(6) 4_465 3_665
O2 Na1 F4 92.7(6) 3_665 3_665
F4 Na1 F4 89.998(2) . 3_665
O1 Na1 F4 89.71(8) . 4_465
O2 Na1 F4 48.4(5) . 4_465
O2 Na1 F4 132.1(5) 2_575 4_465
O2 Na1 F4 92.7(6) 4_465 4_465
O2 Na1 F4 87.7(6) 3_665 4_465
F4 Na1 F4 89.999(2) . 4_465
F4 Na1 F4 179.43(16) 3_665 4_465
O1 Na1 F4 89.71(8) . 2_575
O2 Na1 F4 87.7(6) . 2_575
O2 Na1 F4 92.7(6) 2_575 2_575
O2 Na1 F4 48.4(5) 4_465 2_575
O2 Na1 F4 132.1(5) 3_665 2_575
F4 Na1 F4 179.43(16) . 2_575
F4 Na1 F4 89.999(1) 3_665 2_575
F4 Na1 F4 89.999(1) 4_465 2_575
O1 Na1 F4' 65.3(2) . .
O2' Na1 F4' 114.7(2) . .
O1 Na1 F4' 65.3(2) . 4_465
O2' Na1 F4' 114.7(2) . 4_465
F4' Na1 F4' 79.90(18) . 4_465
C1' B1 C1' 112.1(13) 7_566 2_565
C1' B1 C1' 104(2) 7_566 8_666
C1' B1 C1' 112.1(13) 2_565 8_666
C1' B1 C1' 112.1(13) 7_566 .
C1' B1 C1' 104(2) 2_565 .
C1' B1 C1' 112.1(13) 8_666 .
C1 B1 C1 110.3(3) 7_566 2_565
C1 B1 C1 107.8(7) 7_566 8_666
C1 B1 C1 110.3(3) 2_565 8_666
C1 B1 C1 110.3(3) 7_566 .
C1 B1 C1 107.8(7) 2_565 .
C1 B1 C1 110.3(3) 8_666 .
C2 C1 C6 115.4(3) . .
C2 C1 B1 125.8(3) . .
C6 C1 B1 118.8(3) . .
C5 C6 C1 121.8(3) . .
C4 C5 C6 121.7(3) . .
C4 C5 C8 119.5(3) . .
C6 C5 C8 118.6(4) . .
C5 C4 C3 117.7(3) . .
C4 C3 C2 120.7(3) . .
C4 C3 C7 119.6(3) . .
C2 C3 C7 119.6(3) . .
C3 C2 C1 122.6(3) . .
F6 C8 F4 106.2(4) . .
F6 C8 F5 106.6(4) . .
F4 C8 F5 107.0(3) . .
F6 C8 C5 112.3(4) . .
F4 C8 C5 113.0(4) . .
F5 C8 C5 111.4(4) . .
F3 C7 F2 108.8(5) . .
F3 C7 F1 106.8(4) . .
F2 C7 F1 107.0(5) . .
F3 C7 C3 109.0(8) . .
F2 C7 C3 113.4(6) . .
F1 C7 C3 111.6(6) . .
C8 F4 Na1 135.8(2) . .
C2' C1' C6' 115.5(5) . .
C2' C1' B1 122.3(8) . .
C6' C1' B1 122.1(9) . .
C5' C6' C1' 122.3(6) . .
C4' C5' C6' 120.8(5) . .
C4' C5' C8' 120.6(7) . .
C6' C5' C8' 117.6(7) . .
C5' C4' C3' 118.5(5) . .
C4' C3' C2' 120.3(6) . .
C4' C3' C7' 121.2(6) . .
C2' C3' C7' 118.2(6) . .
C3' C2' C1' 122.5(5) . .
F6' C8' F4' 108.2(8) . .
F6' C8' F5' 100.7(8) . .
F4' C8' F5' 102.1(8) . .
F6' C8' C5' 114.7(10) . .
F4' C8' C5' 111.0(11) . .
F5' C8' C5' 118.9(14) . .
F1' C7' F2' 103.1(9) . .
F1' C7' F3' 103.4(8) . .
F2' C7' F3' 99.7(7) . .
F1' C7' C3' 117.8(11) . .
F2' C7' C3' 112.3(17) . .
F3' C7' C3' 118.2(19) . .
C8' F4' Na1 126.6(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na1 O1 2.193(5) .
Na1 O2' 2.258(7) .
Na1 O2 2.274(17) .
Na1 O2 2.274(17) 2_575
Na1 O2 2.274(17) 4_465
Na1 O2 2.274(17) 3_665
Na1 F4 2.395(2) .
Na1 F4 2.395(2) 3_665
Na1 F4 2.395(2) 4_465
Na1 F4 2.395(2) 2_575
Na1 F4' 2.995(10) .
Na1 F4' 2.995(10) 4_465
B1 C1' 1.601(12) 7_566
B1 C1' 1.601(12) 2_565
B1 C1' 1.601(12) 8_666
B1 C1' 1.601(12) .
B1 C1 1.650(4) 7_566
B1 C1 1.650(4) 2_565
B1 C1 1.650(4) 8_666
B1 C1 1.650(4) .
C1 C2 1.397(4) .
C1 C6 1.404(4) .
C6 C5 1.390(4) .
C5 C4 1.378(5) .
C5 C8 1.502(5) .
C4 C3 1.385(4) .
C3 C2 1.393(4) .
C3 C7 1.493(4) .
C8 F6 1.327(5) .
C8 F4 1.342(4) .
C8 F5 1.363(5) .
C7 F3 1.320(5) .
C7 F2 1.325(6) .
C7 F1 1.329(5) .
C1' C2' 1.396(5) .
C1' C6' 1.402(5) .
C6' C5' 1.392(5) .
C5' C4' 1.380(6) .
C5' C8' 1.509(7) .
C4' C3' 1.386(6) .
C3' C2' 1.396(5) .
C3' C7' 1.497(5) .
C8' F6' 1.344(9) .
C8' F4' 1.345(9) .
C8' F5' 1.371(9) .
C7' F1' 1.347(9) .
C7' F2' 1.376(9) .
C7' F3' 1.377(9) .
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_1
C1 B1 C1 C2 -108.6(15) 7_566
C1 B1 C1 C2 130.9(14) 2_565
C1 B1 C1 C2 10.4(12) 8_666
C1 B1 C1 C6 70.8(7) 7_566
C1 B1 C1 C6 -49.7(8) 2_565
C1 B1 C1 C6 -170.2(10) 8_666
C2 C1 C6 C5 1.5(17) .
B1 C1 C6 C5 -178.0(9) .
C1 C6 C5 C4 -1.5(15) .
C1 C6 C5 C8 174.8(9) .
C6 C5 C4 C3 0.5(14) .
C8 C5 C4 C3 -175.8(9) .
C5 C4 C3 C2 0.4(18) .
C5 C4 C3 C7 -179.0(9) .
C4 C3 C2 C1 0(2) .
C7 C3 C2 C1 179.0(12) .
C6 C1 C2 C3 -0.5(19) .
B1 C1 C2 C3 178.9(11) .
C4 C5 C8 F6 -143.1(7) .
C6 C5 C8 F6 40.5(9) .
C4 C5 C8 F4 96.8(7) .
C6 C5 C8 F4 -79.6(8) .
C4 C5 C8 F5 -23.7(9) .
C6 C5 C8 F5 159.9(7) .
C4 C3 C7 F3 92.6(12) .
C2 C3 C7 F3 -86.8(13) .
C4 C3 C7 F2 -146.0(10) .
C2 C3 C7 F2 34.6(14) .
C4 C3 C7 F1 -25.1(14) .
C2 C3 C7 F1 155.5(11) .
F6 C8 F4 Na1 132.5(3) .
F5 C8 F4 Na1 19.0(6) .
C5 C8 F4 Na1 -103.9(4) .
C1' B1 C1' C2' -111(5) 7_566
C1' B1 C1' C2' 127(4) 2_565
C1' B1 C1' C2' 6(4) 8_666
C1' B1 C1' C6' 72(2) 7_566
C1' B1 C1' C6' -50(3) 2_565
C1' B1 C1' C6' -171(4) 8_666
C2' C1' C6' C5' 1(6) .
B1 C1' C6' C5' 178(3) .
C1' C6' C5' C4' 0(5) .
C1' C6' C5' C8' -169(3) .
C6' C5' C4' C3' 0(5) .
C8' C5' C4' C3' 169(3) .
C5' C4' C3' C2' -2(6) .
C5' C4' C3' C7' -176(3) .
C4' C3' C2' C1' 4(7) .
C7' C3' C2' C1' 178(4) .
C6' C1' C2' C3' -3(6) .
B1 C1' C2' C3' 180(4) .
C4' C5' C8' F6' 163(2) .
C6' C5' C8' F6' -28(3) .
C4' C5' C8' F4' 40(3) .
C6' C5' C8' F4' -151(2) .
C4' C5' C8' F5' -78(3) .
C6' C5' C8' F5' 91(3) .
C4' C3' C7' F1' -11(4) .
C2' C3' C7' F1' 175(3) .
C4' C3' C7' F2' -130(3) .
C2' C3' C7' F2' 56(4) .
C4' C3' C7' F3' 114(3) .
C2' C3' C7' F3' -59(4) .
F6' C8' F4' Na1 -51.7(13) .
F5' C8' F4' Na1 -157.4(7) .
C5' C8' F4' Na1 74.9(14) .
