#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:42:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180445 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/14/7211443.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_7211443
loop_
_publ_author_name
'Waidmann, Thomas'
'Fritsch, Nico'
'Tucher, Johannes'
'Rudolf, Marc'
'Glaser, Felix'
'Guldi, Dirk M.'
'Burzlaff, Nicolai'
_publ_section_title
;
 Battlement-shaped 1D coordination polymer based on a
 bis(N-methylimidazole-2-yl)butadiyne ligand
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              10157
_journal_paper_doi               10.1039/c3ce41652f
_journal_volume                  15
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H50 N8 O20 Zn5'
_chemical_formula_sum            'C44 H50 N8 O20 Zn5'
_chemical_formula_weight         1337.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2013-06-28T11:26:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                98.594(8)
_cell_angle_beta                 94.875(9)
_cell_angle_gamma                93.583(9)
_cell_formula_units_Z            1
_cell_length_a                   8.0568(10)
_cell_length_b                   10.3125(10)
_cell_length_c                   16.0151(16)
_cell_measurement_reflns_used    51
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      6
_cell_measurement_wavelength     0.71073
_cell_volume                     1307.1(2)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 φ- and ω-rotations with 1.60 ° and 192 sec per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13144
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         6.24
_exptl_absorpt_coefficient_mu    2.344
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.053
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+0.3497P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                3632
_reflns_number_total             5321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41652f.txt
_cod_data_source_block           compound8
_cod_database_code               7211443
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
C1 C -0.2924(7) 0.0679(4) -0.0085(3) 0.0273(12) Uani 1 1 d .
C2 C -0.2285(7) 0.0445(5) 0.0570(3) 0.0289(12) Uani 1 1 d .
C3 C -0.1527(7) 0.0174(5) 0.1313(3) 0.0301(13) Uani 1 1 d .
C4 C -0.0839(7) -0.0095(5) 0.1954(3) 0.0290(13) Uani 1 1 d .
C11 C -0.3618(7) 0.0880(5) -0.0896(3) 0.0257(12) Uani 1 1 d .
C12 C -0.4466(7) 0.0376(5) -0.2248(3) 0.0350(14) Uani 1 1 d .
H12 H -0.4729 -0.0079 -0.2794 0.042 Uiso 1 1 calc R
C13 C -0.4657(7) 0.1675(5) -0.1979(3) 0.0331(14) Uani 1 1 d .
H13 H -0.5082 0.226 -0.2316 0.04 Uiso 1 1 calc R
C14 C -0.3425(9) -0.1474(5) -0.1560(4) 0.0456(17) Uani 1 1 d .
H14A H -0.3336 -0.1896 -0.2129 0.068 Uiso 1 1 calc R
H14B H -0.4291 -0.1935 -0.1319 0.068 Uiso 1 1 calc R
H14C H -0.2381 -0.1483 -0.1224 0.068 Uiso 1 1 calc R
C21 C -0.0062(6) -0.0549(4) 0.2665(3) 0.0247(12) Uani 1 1 d .
C22 C 0.0972(7) -0.1947(5) 0.3456(3) 0.0303(13) Uani 1 1 d .
H22 H 0.1315 -0.2709 0.3642 0.036 Uiso 1 1 calc R
C23 C 0.1109(7) -0.0718(5) 0.3911(3) 0.0305(13) Uani 1 1 d .
H23 H 0.1577 -0.0497 0.447 0.037 Uiso 1 1 calc R
C24 C -0.0127(8) -0.2894(5) 0.1940(3) 0.0388(15) Uani 1 1 d .
H24A H 0.086 -0.3008 0.1649 0.058 Uiso 1 1 calc R
H24B H -0.1007 -0.2661 0.1561 0.058 Uiso 1 1 calc R
H24C H -0.0466 -0.37 0.2132 0.058 Uiso 1 1 calc R
C31 C -0.2753(7) 0.2680(5) 0.4119(3) 0.0280(12) Uani 1 1 d .
C32 C -0.4198(7) 0.3415(5) 0.4422(4) 0.0385(14) Uani 1 1 d .
H32A H -0.4247 0.4206 0.4175 0.058 Uiso 1 1 calc R
H32B H -0.4052 0.3635 0.5029 0.058 Uiso 1 1 calc R
H32C H -0.5219 0.2872 0.4255 0.058 Uiso 1 1 calc R
C41 C 0.1878(6) 0.4301(5) 0.3324(3) 0.0232(11) Uani 1 1 d .
C42 C 0.2989(8) 0.4903(5) 0.2755(3) 0.0337(13) Uani 1 1 d .
H42A H 0.3228 0.5823 0.2966 0.051 Uiso 1 1 calc R
H42B H 0.2435 0.4795 0.2192 0.051 Uiso 1 1 calc R
H42C H 0.4013 0.4475 0.2744 0.051 Uiso 1 1 calc R
C51 C 0.2205(6) 0.2859(5) 0.5539(3) 0.0253(12) Uani 1 1 d .
C52 C 0.3286(7) 0.2456(5) 0.6245(3) 0.0376(14) Uani 1 1 d .
H52A H 0.4426 0.2483 0.6111 0.056 Uiso 1 1 calc R
H52B H 0.2927 0.1578 0.6318 0.056 Uiso 1 1 calc R
H52C H 0.3201 0.3048 0.6759 0.056 Uiso 1 1 calc R
C61 C -0.2172(6) 0.6081(5) -0.0299(3) 0.0240(11) Uani 1 1 d .
C62 C -0.0508(7) 0.6690(5) -0.0461(4) 0.0408(15) Uani 1 1 d .
H62A H -0.0411 0.7607 -0.0227 0.061 Uiso 1 1 calc R
H62B H -0.0423 0.6592 -0.1061 0.061 Uiso 1 1 calc R
H62C H 0.037 0.6258 -0.0198 0.061 Uiso 1 1 calc R
C71 C -0.6428(6) 0.5574(5) -0.1406(3) 0.0254(12) Uani 1 1 d .
C72 C -0.7324(7) 0.6002(5) -0.2173(3) 0.0339(13) Uani 1 1 d .
H72A H -0.8472 0.6107 -0.2079 0.051 Uiso 1 1 calc R
H72B H -0.7267 0.5348 -0.2662 0.051 Uiso 1 1 calc R
H72C H -0.6803 0.6824 -0.2268 0.051 Uiso 1 1 calc R
N11 N -0.4123(5) 0.1978(4) -0.1133(2) 0.0233(9) Uani 1 1 d .
N12 N -0.3829(6) -0.0115(4) -0.1571(3) 0.0284(10) Uani 1 1 d .
N21 N 0.0454(6) 0.0156(4) 0.3423(3) 0.0269(10) Uani 1 1 d .
N22 N 0.0228(5) -0.1844(4) 0.2672(3) 0.0263(10) Uani 1 1 d .
O31 O -0.1287(4) 0.3186(3) 0.4409(2) 0.0280(8) Uani 1 1 d .
O32 O -0.2938(5) 0.1667(4) 0.3607(3) 0.0561(13) Uani 1 1 d .
O41 O 0.1475(4) 0.5001(3) 0.3967(2) 0.0271(8) Uani 1 1 d .
O42 O 0.1411(5) 0.3074(3) 0.3098(2) 0.0295(9) Uani 1 1 d .
O51 O 0.1637(4) 0.3980(3) 0.5654(2) 0.0273(8) Uani 1 1 d .
O52 O 0.1937(5) 0.2030(3) 0.4867(2) 0.0297(9) Uani 1 1 d .
O61 O -0.2545(4) 0.4906(3) -0.0621(2) 0.0308(9) Uani 1 1 d .
O62 O -0.3080(5) 0.6768(3) 0.0159(2) 0.0348(9) Uani 1 1 d .
O71 O -0.5851(5) 0.4467(3) -0.1482(2) 0.0313(9) Uani 1 1 d .
O72 O -0.6335(5) 0.6366(3) -0.0725(2) 0.0329(9) Uani 1 1 d .
Zn1 Zn 0 0.5 0.5 0.0213(2) Uani 1 2 d S
Zn2 Zn -0.46055(7) 0.37417(5) -0.04817(3) 0.02167(17) Uani 1 1 d .
Zn3 Zn 0.03528(8) 0.20684(5) 0.38644(4) 0.02283(17) 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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
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
C2 C1 C11 175.6(5) . .
C1 C2 C3 178.9(6) . .
C4 C3 C2 178.1(6) . .
C3 C4 C21 174.0(5) . .
N11 C11 N12 109.9(4) . .
N11 C11 C1 128.4(4) . .
N12 C11 C1 121.6(4) . .
N12 C12 C13 106.8(4) . .
C12 C13 N11 109.2(5) . .
N21 C21 N22 109.7(4) . .
N21 C21 C4 127.3(4) . .
N22 C21 C4 122.9(4) . .
C23 C22 N22 106.4(4) . .
C22 C23 N21 110.0(4) . .
O32 C31 O31 120.5(5) . .
O32 C31 C32 122.7(5) . .
O31 C31 C32 116.8(4) . .
O41 C41 O42 124.9(5) . .
O41 C41 C42 119.1(4) . .
O42 C41 C42 116.0(4) . .
O51 C51 O52 125.4(5) . .
O51 C51 C52 118.4(4) . .
O52 C51 C52 116.1(4) . .
O61 C61 O62 124.3(5) . .
O61 C61 C62 117.3(5) . .
O62 C61 C62 118.4(4) . .
O71 C71 O72 124.6(5) . .
O71 C71 C72 118.9(4) . .
O72 C71 C72 116.5(4) . .
C11 N11 C13 106.2(4) . .
C11 N11 Zn2 133.3(3) . .
C13 N11 Zn2 119.3(3) . .
C12 N12 C11 107.9(4) . .
C12 N12 C14 126.0(4) . .
C11 N12 C14 126.1(5) . .
C21 N21 C23 106.0(4) . .
C21 N21 Zn3 131.1(3) . .
C23 N21 Zn3 122.9(3) . .
C22 N22 C21 107.8(4) . .
C22 N22 C24 127.3(4) . .
C21 N22 C24 124.8(4) . .
C31 O31 Zn3 108.0(3) . .
C31 O31 Zn1 141.3(3) . .
Zn3 O31 Zn1 108.16(16) . .
C31 O32 Zn3 77.8(3) . .
C41 O41 Zn1 143.2(3) . .
C41 O42 Zn3 121.1(3) . .
C51 O51 Zn1 136.6(3) . .
C51 O52 Zn3 128.7(3) . .
C61 O61 Zn2 128.1(3) . .
C61 O62 Zn2 128.2(3) . 2_465
C71 O71 Zn2 123.2(3) . .
C71 O72 Zn2 132.8(3) . 2_465
O51 Zn1 O51 180.00(16) 2_566 .
O51 Zn1 O41 86.43(14) 2_566 .
O51 Zn1 O41 93.57(14) . .
O51 Zn1 O41 93.57(14) 2_566 2_566
O51 Zn1 O41 86.43(14) . 2_566
O41 Zn1 O41 180.0000(10) . 2_566
O51 Zn1 O31 90.50(13) 2_566 .
O51 Zn1 O31 89.50(13) . .
O41 Zn1 O31 90.54(13) . .
O41 Zn1 O31 89.46(13) 2_566 .
O51 Zn1 O31 89.50(13) 2_566 2_566
O51 Zn1 O31 90.50(13) . 2_566
O41 Zn1 O31 89.46(13) . 2_566
O41 Zn1 O31 90.54(13) 2_566 2_566
O31 Zn1 O31 180.00(18) . 2_566
O51 Zn1 Zn3 109.54(8) 2_566 .
O51 Zn1 Zn3 70.46(8) . .
O41 Zn1 Zn3 64.42(8) . .
O41 Zn1 Zn3 115.58(8) 2_566 .
O31 Zn1 Zn3 34.41(9) . .
O31 Zn1 Zn3 145.59(9) 2_566 .
N11 Zn2 O61 102.06(15) . .
N11 Zn2 O62 98.77(15) . 2_465
O61 Zn2 O62 158.97(14) . 2_465
N11 Zn2 O72 102.81(15) . 2_465
O61 Zn2 O72 89.47(15) . 2_465
O62 Zn2 O72 88.74(16) 2_465 2_465
N11 Zn2 O71 97.71(14) . .
O61 Zn2 O71 88.53(15) . .
O62 Zn2 O71 85.82(15) 2_465 .
O72 Zn2 O71 159.35(14) 2_465 .
N11 Zn2 Zn2 178.24(12) . 2_465
O61 Zn2 Zn2 79.68(10) . 2_465
O62 Zn2 Zn2 79.51(10) 2_465 2_465
O72 Zn2 Zn2 76.86(10) 2_465 2_465
O71 Zn2 Zn2 82.56(9) . 2_465
O42 Zn3 O52 108.98(16) . .
O42 Zn3 O31 106.70(15) . .
O52 Zn3 O31 99.03(14) . .
O42 Zn3 N21 108.03(16) . .
O52 Zn3 N21 93.80(15) . .
O31 Zn3 N21 136.42(16) . .
O42 Zn3 O32 116.02(16) . .
O52 Zn3 O32 132.16(16) . .
O31 Zn3 O32 53.72(12) . .
N21 Zn3 O32 87.35(15) . .
O42 Zn3 Zn1 84.41(9) . .
O52 Zn3 Zn1 78.36(9) . .
O31 Zn3 Zn1 37.43(9) . .
N21 Zn3 Zn1 167.06(12) . .
O32 Zn3 Zn1 90.35(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.193(7) .
C1 C11 1.420(7) .
C2 C3 1.365(8) .
C3 C4 1.202(7) .
C4 C21 1.407(7) .
C11 N11 1.323(6) .
C11 N12 1.366(6) .
C12 N12 1.340(7) .
C12 C13 1.366(7) .
C13 N11 1.369(6) .
C14 N12 1.460(6) .
C21 N21 1.338(6) .
C21 N22 1.371(6) .
C22 C23 1.357(6) .
C22 N22 1.367(6) .
C23 N21 1.379(6) .
C24 N22 1.467(6) .
C31 O32 1.221(5) .
C31 O31 1.281(6) .
C31 C32 1.503(7) .
C41 O41 1.245(5) .
C41 O42 1.286(5) .
C41 C42 1.501(7) .
C51 O51 1.263(6) .
C51 O52 1.264(5) .
C51 C52 1.493(7) .
C61 O61 1.251(5) .
C61 O62 1.255(6) .
C61 C62 1.503(7) .
C71 O71 1.252(6) .
C71 O72 1.255(5) .
C71 C72 1.510(7) .
N11 Zn2 2.034(4) .
N21 Zn3 2.002(4) .
O31 Zn3 1.980(3) .
O31 Zn1 2.129(3) .
O32 Zn3 2.645(4) .
O41 Zn1 2.118(3) .
O42 Zn3 1.938(4) .
O51 Zn1 2.052(3) .
O52 Zn3 1.971(3) .
O61 Zn2 2.035(3) .
O62 Zn2 2.036(4) 2_465
O71 Zn2 2.077(4) .
O72 Zn2 2.036(3) 2_465
Zn1 O51 2.052(3) 2_566
Zn1 O41 2.118(3) 2_566
Zn1 O31 2.129(3) 2_566
Zn1 Zn3 3.3287(6) .
Zn2 O62 2.036(4) 2_465
Zn2 O72 2.036(3) 2_465
Zn2 Zn2 2.9489(10) 2_465
