#------------------------------------------------------------------------------
#$Date: 2015-09-17 09:17:35 +0300 (Thu, 17 Sep 2015) $
#$Revision: 156723 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/21/7222169.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_7222169
loop_
_publ_author_name
'Easton, Max Eric'
'Turner, Peter'
'Masters, Anthony Frederick'
'Maschmeyer, Thomas'
_publ_section_title
;
 Zinc bromide in aqueous solutions of ionic liquid bromide salts: the
 interplay between complexation and electrochemistry
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA15736F
_journal_year                    2015
_chemical_formula_sum            'C33 H72 Br7 N3 Zn2'
_chemical_formula_weight         1201.04
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      159
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-08-03 deposited with the CCDC.
2015-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.7234(2)
_cell_length_b                   14.7234(2)
_cell_length_c                   12.4759(3)
_cell_measurement_reflns_used    15448
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      73.2910
_cell_measurement_theta_min      4.9290
_cell_volume                     2342.17(7)
_computing_cell_refinement
;
  CrysAlisPro, Agilent Technologies,
;
_computing_data_collection
;
  CrysAlisPro, Agilent Technologies,
;
_computing_data_reduction
;
  CrysAlisPro, Agilent Technologies,
;
_computing_molecular_graphics
;
  ORTEP3 for Windows (Farrugia, L., 1997)
  ORTEPIII  (Burnett, N.M., Johnson,C.K., 1996). 
  WinGX (Farrugia, 1999)
  shelXle (Hbschle,C.B., et al., 2011) 
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014a)'
_computing_structure_solution    'ShelxT (sheldrick, 2013)'
_diffrn_ambient_temperature      150(1)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N to a nylon loop and quenched 
in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. 
;
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            50065
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.846
_diffrn_reflns_theta_min         3.466
_exptl_absorpt_coefficient_mu    8.429
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  CrysAlisPro, Agilent Technologies,
  Version 1.171.36.28
  Empirical absorption correction using spherical 
  harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.00066(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          1.221
_refine_ls_shift/su_mean         0.144
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.08P)²+1.0P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1646
_reflns_Friedel_coverage         0.990
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.997
_reflns_number_gt                2634
_reflns_number_total             3280
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ra15736f2.cif
_cod_data_source_block           afm15pt3_11_P31c
_cod_original_cell_volume        2342.17(8)
_cod_database_code               7222169
_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.6177(4) 0.3131(10) 0.3430(9) 0.1222(18) Uani 0.3333 1 d . U P . .
Br2 Br 0.4884(2) 0.2345(3) 0.5857(3) 0.1020(9) Uani 1 1 d . U . . .
Br3 Br 0.4881(2) 0.2332(3) 0.0988(3) 0.0996(9) Uani 1 1 d . U . . .
Zn1 Zn 0.6667 0.3333 0.5361(5) 0.0703(15) Uani 1 3 d S TU P . .
Zn2 Zn 0.6667 0.3333 0.1497(5) 0.0724(18) Uani 1 3 d S TU P . .
N1 N 0.4839(16) 0.5178(15) 0.3458(19) 0.117(3) Uani 1 1 d G U . . .
C1 C 0.466(3) 0.440(2) 0.2571(19) 0.142(5) Uani 1 1 d G U . . .
H1A H 0.5243 0.4251 0.2530 0.170 Uiso 1 1 calc R U . . .
H1B H 0.4578 0.4663 0.1867 0.170 Uiso 1 1 calc R U . . .
C2 C 0.358(4) 0.338(3) 0.294(3) 0.165(7) Uani 1 1 d . U . . .
H2A H 0.2971 0.3300 0.2532 0.198 Uiso 1 1 calc R U . . .
H2B H 0.3621 0.2728 0.2873 0.198 Uiso 1 1 calc R U . . .
C3 C 0.354(4) 0.365(4) 0.410(4) 0.165(7) Uani 1 1 d . U . . .
H3A H 0.3383 0.3037 0.4546 0.198 Uiso 1 1 calc R U . . .
H3B H 0.2964 0.3804 0.4185 0.198 Uiso 1 1 calc R U . . .
C4 C 0.460(3) 0.463(3) 0.451(2) 0.142(5) Uani 1 1 d . U . . .
H4A H 0.4482 0.5020 0.5089 0.170 Uiso 1 1 calc R U . . .
H4B H 0.5129 0.4442 0.4732 0.170 Uiso 1 1 calc R U . . .
C5 C 0.4229(18) 0.5717(17) 0.335(2) 0.103(4) Uani 1 1 d . U . . .
H5A H 0.3542 0.5235 0.3041 0.155 Uiso 1 1 calc R U . . .
H5B H 0.4605 0.6329 0.2883 0.155 Uiso 1 1 calc R U . . .
H5C H 0.4136 0.5946 0.4060 0.155 Uiso 1 1 calc R U . . .
C6 C 0.600(2) 0.592(2) 0.309(2) 0.151(8) Uani 1 1 d D U . . .
H6A H 0.6366 0.5520 0.3010 0.181 Uiso 1 1 calc R U . . .
H6B H 0.6003 0.6238 0.2385 0.181 Uiso 1 1 calc R U . . .
C7 C 0.654(2) 0.677(3) 0.391(3) 0.180(12) Uani 1 1 d D U . . .
H7A H 0.6251 0.6500 0.4634 0.216 Uiso 1 1 calc R U . A 1
H7B H 0.6435 0.7370 0.3751 0.216 Uiso 1 1 calc R U . A 1
C8A C 0.769(3) 0.712(9) 0.389(6) 0.22(3) Uani 0.4 1 d D U P B 1
H8A1 H 0.7774 0.6494 0.3837 0.266 Uiso 0.4 1 calc R U P B 1
H8A2 H 0.8007 0.7547 0.3233 0.266 Uiso 0.4 1 calc R U P B 1
C9A C 0.827(3) 0.775(7) 0.485(6) 0.246(17) Uani 0.4 1 d D U P B 1
H9A1 H 0.8537 0.7357 0.5269 0.295 Uiso 0.4 1 calc R U P B 1
H9A2 H 0.8887 0.8417 0.4616 0.295 Uiso 0.4 1 calc R U P B 1
C10A C 0.760(4) 0.799(7) 0.557(5) 0.246(17) Uani 0.4 1 d D U P B 1
H10A H 0.7127 0.7360 0.5988 0.295 Uiso 0.4 1 calc R U P B 1
H10B H 0.7158 0.8174 0.5119 0.295 Uiso 0.4 1 calc R U P B 1
C11A C 0.823(8) 0.888(7) 0.633(7) 0.246(17) Uani 0.4 1 d D U P B 1
H11A H 0.7756 0.9010 0.6774 0.369 Uiso 0.4 1 calc R U P B 1
H11B H 0.8658 0.8705 0.6788 0.369 Uiso 0.4 1 calc R U P B 1
H11C H 0.8690 0.9519 0.5918 0.369 Uiso 0.4 1 calc R U P B 1
C8B C 0.766(3) 0.751(3) 0.358(5) 0.203(17) Uani 0.6 1 d D U P B 2
H8B1 H 0.8016 0.7096 0.3469 0.244 Uiso 0.6 1 calc R U P B 2
H8B2 H 0.7660 0.7837 0.2891 0.244 Uiso 0.6 1 calc R U P B 2
C9B C 0.826(3) 0.835(3) 0.440(7) 0.246(17) Uani 0.6 1 d D U P B 2
H9B1 H 0.9017 0.8706 0.4214 0.295 Uiso 0.6 1 calc R U P B 2
H9B2 H 0.8171 0.8023 0.5111 0.295 Uiso 0.6 1 calc R U P B 2
C10B C 0.791(5) 0.915(4) 0.445(5) 0.246(17) Uani 0.6 1 d D U P B 2
H10C H 0.8124 0.9568 0.3778 0.295 Uiso 0.6 1 calc R U P B 2
H10D H 0.7140 0.8786 0.4497 0.295 Uiso 0.6 1 calc R U P B 2
C11B C 0.837(8) 0.988(6) 0.539(6) 0.246(17) Uani 0.6 1 d D U P B 2
H11D H 0.8125 1.0387 0.5385 0.369 Uiso 0.6 1 calc R U P B 2
H11E H 0.8157 0.9477 0.6055 0.369 Uiso 0.6 1 calc R U P B 2
H11F H 0.9142 1.0259 0.5337 0.369 Uiso 0.6 1 calc R U P B 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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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
Br1 Br1 Br1 60.003(4) 2_655 3_665
Br1 Br1 Zn1 77.40(10) 2_655 .
Br1 Br1 Zn1 77.40(10) 3_665 .
Br1 Br1 Zn2 77.41(12) 2_655 .
Br1 Br1 Zn2 77.41(12) 3_665 .
Zn1 Br1 Zn2 150.8(2) . .
Br2 Zn1 Br2 113.38(13) . 2_655
Br2 Zn1 Br2 113.38(13) . 3_665
Br2 Zn1 Br2 113.38(13) 2_655 3_665
Br2 Zn1 Br1 109.9(3) . 2_655
Br2 Zn1 Br1 90.80(17) 2_655 2_655
Br2 Zn1 Br1 114.1(3) 3_665 2_655
Br2 Zn1 Br1 90.80(17) . .
Br2 Zn1 Br1 114.1(3) 2_655 .
Br2 Zn1 Br1 109.9(3) 3_665 .
Br1 Zn1 Br1 25.20(19) 2_655 .
Br2 Zn1 Br1 114.1(3) . 3_665
Br2 Zn1 Br1 109.9(3) 2_655 3_665
Br2 Zn1 Br1 90.80(17) 3_665 3_665
Br1 Zn1 Br1 25.20(19) 2_655 3_665
Br1 Zn1 Br1 25.20(19) . 3_665
Br3 Zn2 Br3 113.09(13) 2_655 3_665
Br3 Zn2 Br3 113.09(13) 2_655 .
Br3 Zn2 Br3 113.09(13) 3_665 .
Br3 Zn2 Br1 91.17(19) 2_655 2_655
Br3 Zn2 Br1 114.5(3) 3_665 2_655
Br3 Zn2 Br1 110.1(3) . 2_655
Br3 Zn2 Br1 114.5(3) 2_655 .
Br3 Zn2 Br1 110.1(3) 3_665 .
Br3 Zn2 Br1 91.17(19) . .
Br1 Zn2 Br1 25.2(2) 2_655 .
Br3 Zn2 Br1 110.1(3) 2_655 3_665
Br3 Zn2 Br1 91.17(19) 3_665 3_665
Br3 Zn2 Br1 114.5(3) . 3_665
Br1 Zn2 Br1 25.2(2) 2_655 3_665
Br1 Zn2 Br1 25.2(2) . 3_665
C5 N1 C4 109(2) . .
C5 N1 C1 114.7(18) . .
C4 N1 C1 109(2) . .
C5 N1 C6 109.9(18) . .
C4 N1 C6 121(2) . .
C1 N1 C6 92(2) . .
N1 C1 C2 102(2) . .
C3 C2 C1 100(4) . .
C2 C3 C4 114(5) . .
N1 C4 C3 94(3) . .
C7 C6 N1 109(2) . .
C6 C7 C8A 108(3) . .
C6 C7 C8B 110(3) . .
C9A C8A C7 112.8(14) . .
C10A C9A C8A 112.6(14) . .
C9A C10A C11A 112.8(15) . .
C9B C8B C7 112.9(14) . .
C8B C9B C10B 112.7(14) . .
C11B C10B C9B 112.8(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Br1 1.086(8) 2_655
Br1 Br1 1.086(8) 3_665
Br1 Zn1 2.490(11) .
Br1 Zn2 2.492(11) .
Br2 Zn1 2.360(3) .
Br3 Zn2 2.369(3) .
Zn1 Br2 2.360(3) 2_655
Zn1 Br2 2.360(3) 3_665
Zn1 Br1 2.490(11) 2_655
Zn1 Br1 2.490(11) 3_665
Zn2 Br3 2.369(3) 2_655
Zn2 Br3 2.369(3) 3_665
Zn2 Br1 2.492(11) 2_655
Zn2 Br1 2.492(11) 3_665
N1 C5 1.471(15) .
N1 C4 1.49(3) .
N1 C1 1.5169 .
N1 C6 1.57(3) .
C1 C2 1.62(6) .
C2 C3 1.50(5) .
C3 C4 1.59(7) .
C6 C7 1.504(7) .
C7 C8A 1.505(10) .
C7 C8B 1.505(10) .
C8A C9A 1.504(10) .
C9A C10A 1.504(10) .
C10A C11A 1.504(10) .
C8B C9B 1.504(10) .
C9B C10B 1.504(10) .
C10B C11B 1.504(10) .
