#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:48:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179937 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/32/7023273.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_7023273
loop_
_publ_author_name
'Hausmann, David'
'Feldmann, Claus'
_publ_section_title
;
 The chain-like polynuclear coordination compounds (ZnBr2)n(18-crown-6)2
 (n = 4, 6, 8, 10) and [Zn5Br9][N(Tf2)].
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13487
_journal_page_last               13494
_journal_paper_doi               10.1039/c3dt51130h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C24 H48 Br12 O12 Zn6'
_chemical_formula_weight         1879.76
_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-97
_cell_angle_alpha                79.16(3)
_cell_angle_beta                 74.99(3)
_cell_angle_gamma                79.78(3)
_cell_formula_units_Z            1
_cell_length_a                   8.1203(16)
_cell_length_b                   10.887(2)
_cell_length_c                   14.851(3)
_cell_measurement_temperature    200(2)
_cell_volume                     1234.0(5)
_computing_cell_refinement       'CELL, SELECT (STOE)'
_computing_data_collection       'EXPOSE (STOE)'
_computing_data_reduction        'INTEGRATE (STOE)'
_computing_molecular_graphics    'DIAMOND, Crystal Impact'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.918
_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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12074
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    12.66
_exptl_absorpt_correction_T_max  0.28
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         6139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0422P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                4340
_reflns_number_total             6139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51130h.txt
_cod_data_source_block           Compound-2_Zn6Br12(18c6)2
_cod_original_cell_volume        1234.0(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7023273
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br1 Br 1.35516(7) -0.16462(7) 0.41928(4) 0.04765(17) Uani 1 1 d .
Br2 Br 1.16290(12) 0.26691(8) 0.34694(5) 0.0696(2) Uani 1 1 d .
Br3 Br 1.18250(9) 0.05595(6) 0.14077(4) 0.05047(17) Uani 1 1 d .
Br4 Br 1.37812(7) 0.38053(5) 0.08102(4) 0.03964(14) Uani 1 1 d .
Br5 Br 1.11709(7) 0.72157(5) 0.10940(4) 0.03632(13) Uani 1 1 d .
Br6 Br 0.86957(7) 0.43348(5) 0.11298(3) 0.03461(13) Uani 1 1 d .
Zn1 Zn 1.62653(7) -0.20435(6) 0.32203(4) 0.03216(14) Uani 1 1 d .
Zn2 Zn 1.28260(8) 0.20043(6) 0.20190(4) 0.03614(15) Uani 1 1 d .
Zn3 Zn 1.13344(8) 0.53359(6) 0.05571(4) 0.03117(14) Uani 1 1 d .
O1 O 1.5385(5) 0.1230(3) 0.2007(2) 0.0327(8) Uani 1 1 d .
O2 O 1.6639(5) -0.1335(3) 0.1806(2) 0.0320(8) Uani 1 1 d .
O3 O 1.5890(5) -0.3564(3) 0.2590(2) 0.0326(8) Uani 1 1 d .
O4 O 1.6542(5) -0.4517(4) 0.4318(3) 0.0437(10) Uani 1 1 d .
O5 O 1.8576(5) -0.2681(4) 0.3513(3) 0.0426(9) Uani 1 1 d .
O6 O 1.7237(6) -0.0334(4) 0.3371(3) 0.0466(10) Uani 1 1 d .
C1 C 1.6427(7) 0.0853(5) 0.1128(3) 0.0369(12) Uani 1 1 d .
H1A H 1.7111 0.1533 0.0777 0.044 Uiso 1 1 calc R
H1B H 1.5668 0.0726 0.0738 0.044 Uiso 1 1 calc R
C2 C 1.7610(7) -0.0337(5) 0.1297(4) 0.0349(11) Uani 1 1 d .
H2A H 1.8304 -0.0576 0.0686 0.042 Uiso 1 1 calc R
H2B H 1.8407 -0.0204 0.1663 0.042 Uiso 1 1 calc R
C3 C 1.6237(8) -0.2083(5) 0.1217(3) 0.0367(12) Uani 1 1 d .
H3A H 1.7301 -0.2561 0.0881 0.044 Uiso 1 1 calc R
H3B H 1.5660 -0.1537 0.0744 0.044 Uiso 1 1 calc R
C4 C 1.5078(7) -0.2961(6) 0.1843(4) 0.0378(12) Uani 1 1 d .
H4A H 1.3943 -0.2492 0.2100 0.045 Uiso 1 1 calc R
H4B H 1.4907 -0.3596 0.1491 0.045 Uiso 1 1 calc R
C5 C 1.5025(8) -0.4565(5) 0.3186(4) 0.0421(14) Uani 1 1 d .
H5A H 1.4727 -0.5103 0.2800 0.050 Uiso 1 1 calc R
H5B H 1.3950 -0.4214 0.3602 0.050 Uiso 1 1 calc R
C6 C 1.6213(9) -0.5325(5) 0.3764(4) 0.0424(14) Uani 1 1 d .
H6A H 1.5674 -0.6045 0.4173 0.051 Uiso 1 1 calc R
H6B H 1.7300 -0.5659 0.3349 0.051 Uiso 1 1 calc R
C7 C 1.8262(8) -0.4705(6) 0.4405(4) 0.0424(13) Uani 1 1 d .
H7A H 1.8716 -0.5615 0.4448 0.051 Uiso 1 1 calc R
H7B H 1.8318 -0.4409 0.4986 0.051 Uiso 1 1 calc R
C8 C 1.9322(8) -0.3983(6) 0.3561(4) 0.0474(15) Uani 1 1 d .
H8A H 2.0525 -0.4075 0.3622 0.057 Uiso 1 1 calc R
H8B H 1.9321 -0.4308 0.2982 0.057 Uiso 1 1 calc R
C9 C 1.9620(8) -0.1828(7) 0.3586(5) 0.0560(17) Uani 1 1 d .
H9A H 2.0430 -0.1625 0.2971 0.067 Uiso 1 1 calc R
H9B H 2.0301 -0.2212 0.4058 0.067 Uiso 1 1 calc R
C10 C 1.8534(8) -0.0664(7) 0.3873(5) 0.0506(16) Uani 1 1 d .
H10A H 1.8013 -0.0802 0.4558 0.061 Uiso 1 1 calc R
H10B H 1.9246 0.0028 0.3740 0.061 Uiso 1 1 calc R
C11 C 1.6213(10) 0.0869(6) 0.3490(4) 0.0520(16) Uani 1 1 d .
H11A H 1.6636 0.1281 0.3910 0.062 Uiso 1 1 calc R
H11B H 1.5003 0.0746 0.3789 0.062 Uiso 1 1 calc R
C12 C 1.6303(9) 0.1700(6) 0.2555(4) 0.0446(14) Uani 1 1 d .
H12A H 1.5789 0.2574 0.2654 0.053 Uiso 1 1 calc R
H12B H 1.7521 0.1715 0.2210 0.053 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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_3
Zn3 Br4 Zn2 110.34(4) .
Zn3 Br6 Zn3 83.89(4) 2_765
O5 Zn1 O2 108.45(16) .
O5 Zn1 O3 101.31(16) .
O2 Zn1 O3 75.92(13) .
O5 Zn1 O6 75.29(17) .
O2 Zn1 O6 86.26(14) .
O3 Zn1 O6 159.88(14) .
O5 Zn1 Br1 131.54(12) .
O2 Zn1 Br1 118.73(12) .
O3 Zn1 Br1 100.15(10) .
O6 Zn1 Br1 96.56(13) .
O1 Zn2 Br3 103.62(10) .
O1 Zn2 Br2 107.23(10) .
Br3 Zn2 Br2 125.74(4) .
O1 Zn2 Br4 91.03(10) .
Br3 Zn2 Br4 112.48(4) .
Br2 Zn2 Br4 110.43(4) .
Br5 Zn3 Br4 114.65(4) .
Br5 Zn3 Br6 114.29(4) .
Br4 Zn3 Br6 109.54(3) .
Br5 Zn3 Br6 111.75(4) 2_765
Br4 Zn3 Br6 108.92(4) 2_765
Br6 Zn3 Br6 96.11(4) 2_765
C12 O1 C1 114.9(4) .
C12 O1 Zn2 119.3(3) .
C1 O1 Zn2 116.5(3) .
C3 O2 C2 114.0(4) .
C3 O2 Zn1 116.8(3) .
C2 O2 Zn1 127.6(3) .
C4 O3 C5 113.0(4) .
C4 O3 Zn1 104.9(3) .
C5 O3 Zn1 118.5(3) .
C6 O4 C7 113.8(5) .
C9 O5 C8 116.3(5) .
C9 O5 Zn1 120.1(4) .
C8 O5 Zn1 123.3(4) .
C10 O6 C11 115.3(4) .
C10 O6 Zn1 110.4(4) .
C11 O6 Zn1 125.2(4) .
O1 C1 C2 111.3(4) .
O2 C2 C1 110.1(4) .
O2 C3 C4 106.8(4) .
O3 C4 C3 106.7(4) .
O3 C5 C6 107.8(5) .
O4 C6 C5 107.3(5) .
O4 C7 C8 108.9(5) .
O5 C8 C7 107.6(5) .
O5 C9 C10 109.5(5) .
O6 C10 C9 109.2(5) .
O6 C11 C12 110.5(5) .
O1 C12 C11 109.8(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Zn1 2.3189(11) .
Br2 Zn2 2.3153(11) .
Br3 Zn2 2.3091(10) .
Br4 Zn3 2.4170(12) .
Br4 Zn2 2.4827(12) .
Br5 Zn3 2.3031(9) .
Br6 Zn3 2.4573(11) .
Br6 Zn3 2.4690(9) 2_765
Zn1 O5 2.009(4) .
Zn1 O2 2.060(3) .
Zn1 O3 2.149(3) .
Zn1 O6 2.216(4) .
Zn2 O1 2.096(4) .
Zn3 Br6 2.4690(9) 2_765
O1 C12 1.446(7) .
O1 C1 1.447(6) .
O2 C3 1.429(6) .
O2 C2 1.435(6) .
O3 C4 1.431(7) .
O3 C5 1.432(6) .
O4 C6 1.411(7) .
O4 C7 1.412(8) .
O5 C9 1.399(7) .
O5 C8 1.436(7) .
O6 C10 1.401(8) .
O6 C11 1.436(8) .
C1 C2 1.492(8) .
C3 C4 1.483(8) .
C5 C6 1.493(9) .
C7 C8 1.496(7) .
C9 C10 1.475(10) .
C11 C12 1.500(9) .
