#------------------------------------------------------------------------------
#$Date: 2014-07-11 19:04:56 +0300 (Fri, 11 Jul 2014) $
#$Revision: 120072 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/23/45/2234566.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2234566
loop_
_publ_author_name
'Wang, Cheng'
'Wen, Bo'
'Sun, Zhi-Yao'
'Yan, Peng-Fei'
'Gao, Jin-Sheng'
_publ_section_title
;
catena-Poly[(dichloridozinc)-\m-1-{4-[(1H-imidazol-1-yl)methyl]benzyl}-1H-imidazole-\k^2^N^3^:N^3'^]
;
_journal_coeditor_code CV5275
_journal_issue 5
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first m621
_journal_volume 68
_journal_year 2012
_chemical_formula_iupac '[Zn Cl2 (C14 H14 N4)]'
_chemical_formula_moiety 'C14 H14 Cl2 N4 Zn'
_chemical_formula_sum 'C14 H14 Cl2 N4 Zn'
_chemical_formula_weight 374.56
_chemical_name_systematic
;
catena-Poly[(dichloridozinc)-\m-1-{4-[(1H-imidazol-1-
yl)methyl]benzyl}-1H-imidazole-\k^2^N^3^:N^3'^]
;
_space_group_IT_number 60
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2n 2ab'
_symmetry_space_group_name_H-M 'P b c n'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.327(2)
_cell_length_b 10.207(2)
_cell_length_c 14.452(3)
_cell_measurement_reflns_used 13075
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 3.03
_cell_volume 1670.9(6)
_computing_cell_refinement 'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection 'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC, 2002)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPID'
_diffrn_measurement_method '\w scan'
_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 0.0221
_diffrn_reflns_av_sigmaI/netI 0.0131
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 15231
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_min 3.03
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 1.787
_exptl_absorpt_correction_T_max 0.4771
_exptl_absorpt_correction_T_min 0.4212
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.489
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 760
_exptl_crystal_size_max 0.58
_exptl_crystal_size_mid 0.55
_exptl_crystal_size_min 0.49
_refine_diff_density_max 0.204
_refine_diff_density_min -0.293
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.081
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 96
_refine_ls_number_reflns 1916
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.081
_refine_ls_R_factor_all 0.0263
_refine_ls_R_factor_gt 0.0231
_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/[\s^2^(Fo^2^)+(0.0339P)^2^+0.4633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0616
_refine_ls_wR_factor_ref 0.0629
_reflns_number_gt 1718
_reflns_number_total 1916
_reflns_threshold_expression I>2sigma(I)
_iucr_refine_instructions_details
;
TITL in Pbcn
CELL 0.71073 11.3272 10.2066 14.4521 90.000 90.000 90.000
ZERR 4.00 0.0023 0.0020 0.0029 0.000 0.000 0.000
LATT 1
SYMM 0.5-X, 0.5-Y, 0.5+Z
SYMM -X, Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C H N Zn Cl
UNIT 56 56 16 4 8
L.S. 4
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.486 0.550 0.585
WGHT 0.033900 0.463300
FVAR 0.30133
MOLE 1
C1 1 0.835188 0.158166 0.398233 11.00000 0.03463 0.03952 =
0.03085 0.00155 0.00402 0.00667
AFIX 43
H1 2 0.872313 0.102776 0.440233 11.00000 -1.20000
AFIX 0
C2 1 0.793813 0.266162 0.276314 11.00000 0.08350 0.09786 =
0.04481 0.03157 0.01782 0.05001
AFIX 43
H2 2 0.797607 0.300402 0.216754 11.00000 -1.20000
AFIX 0
C3 1 0.708470 0.292617 0.338759 11.00000 0.07367 0.08703 =
0.05924 0.02506 0.01654 0.05107
AFIX 43
H3 2 0.643568 0.347158 0.330410 11.00000 -1.20000
AFIX 0
C4 1 0.666391 0.216801 0.501580 11.00000 0.04391 0.04995 =
0.04367 -0.01253 0.01634 -0.00233
AFIX 23
H4A 2 0.623662 0.298322 0.509865 11.00000 -1.20000
H4B 2 0.719545 0.206535 0.553702 11.00000 -1.20000
AFIX 0
C5 1 0.599833 -0.004847 0.554342 11.00000 0.04080 0.06085 =
0.06028 0.00749 -0.00975 -0.00044
AFIX 43
H5 2 0.666682 -0.008817 0.591597 11.00000 -1.20000
AFIX 0
C6 1 0.579406 0.104172 0.500834 11.00000 0.03457 0.04392 =
0.04024 -0.00744 0.00957 0.00346
C7 1 0.478712 0.108758 0.447007 11.00000 0.04889 0.05069 =
0.06735 0.01458 -0.00555 0.00177
AFIX 43
H7 2 0.463491 0.182580 0.411222 11.00000 -1.20000
AFIX 0
CL1 5 1.082047 -0.037727 0.366085 11.00000 0.03671 0.04778 =
0.03686 0.00531 -0.00610 0.00320
N1 3 0.873719 0.181412 0.314013 11.00000 0.04067 0.04467 =
0.03191 0.00479 0.00782 0.01200
N2 3 0.736012 0.224192 0.415753 11.00000 0.03603 0.03901 =
0.03714 -0.00170 0.00788 0.00639
ZN1 4 1.000000 0.079509 0.250000 10.50000 0.02814 0.03731 =
0.02650 0.00000 0.00440 0.00000
HKLF 4
REM in Pbcn
REM R1 = 0.0231 for 1718 Fo > 4sig(Fo) and 0.0263 for all 1916 data
REM 96 parameters refined using 0 restraints
END
WGHT 0.0319 0.4717
REM Highest difference peak 0.204, deepest hole -0.293, 1-sigma level 0.058
Q1 1 0.9325 0.1882 0.3127 11.00000 0.05 0.20
Q2 1 0.9271 0.1571 0.2967 11.00000 0.05 0.19
Q3 1 0.6087 0.1586 0.5045 11.00000 0.05 0.19
Q4 1 0.5945 0.3304 0.4698 11.00000 0.05 0.17
Q5 1 0.5235 0.1296 0.4930 11.00000 0.05 0.15
Q6 1 0.8593 0.2240 0.2967 11.00000 0.05 0.15
Q7 1 0.9001 0.1541 0.4583 11.00000 0.05 0.14
Q8 1 0.8661 0.2910 0.2904 11.00000 0.05 0.14
Q9 1 0.8575 0.3342 0.2234 11.00000 0.05 0.14
Q10 1 0.8743 0.1808 0.3522 11.00000 0.05 0.14
Q11 1 1.1287 0.0090 0.3511 11.00000 0.05 0.14
Q12 1 0.5346 0.0772 0.4334 11.00000 0.05 0.14
Q13 1 0.9476 0.3061 0.3219 11.00000 0.05 0.14
Q14 1 1.0000 0.2940 0.2500 10.50000 0.05 0.14
Q15 1 0.7036 -0.0356 0.5562 11.00000 0.05 0.13
Q16 1 0.5564 0.0914 0.4464 11.00000 0.05 0.13
Q17 1 0.8432 0.1345 0.3432 11.00000 0.05 0.13
Q18 1 0.8437 0.4930 0.2729 11.00000 0.05 0.12
Q19 1 0.5604 0.1145 0.3687 11.00000 0.05 0.12
Q20 1 0.5433 0.2057 0.3701 11.00000 0.05 0.12
;
_[local]_cod_data_source_file cv5275.cif
_[local]_cod_data_source_block global
_cod_original_cell_volume 1670.8(6)
_cod_database_code 2234566
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.83519(13) 0.15817(15) 0.39823(10) 0.0350(3) Uani d . 1 1
H H1 0.8723 0.1028 0.4402 0.042 Uiso calc R 1 1
C C2 0.7938(2) 0.2662(3) 0.27631(15) 0.0754(8) Uani d . 1 1
H H2 0.7976 0.3004 0.2168 0.090 Uiso calc R 1 1
C C3 0.7085(2) 0.2926(3) 0.33876(15) 0.0733(7) Uani d . 1 1
H H3 0.6436 0.3472 0.3304 0.088 Uiso calc R 1 1
C C4 0.66639(15) 0.21680(18) 0.50158(12) 0.0458(4) Uani d . 1 1
H H4A 0.6237 0.2983 0.5099 0.055 Uiso calc R 1 1
H H4B 0.7195 0.2065 0.5537 0.055 Uiso calc R 1 1
C C5 0.59983(16) -0.0048(2) 0.55434(14) 0.0540(5) Uani d . 1 1
H H5 0.6667 -0.0088 0.5916 0.065 Uiso calc R 1 1
C C6 0.57941(13) 0.10417(16) 0.50083(11) 0.0396(4) Uani d . 1 1
C C7 0.47871(17) 0.1088(2) 0.44701(16) 0.0556(5) Uani d . 1 1
H H7 0.4635 0.1826 0.4112 0.067 Uiso calc R 1 1
Cl Cl1 1.08205(3) -0.03773(4) 0.36609(3) 0.04045(11) Uani d . 1 1
N N1 0.87372(11) 0.18141(14) 0.31401(9) 0.0391(3) Uani d . 1 1
N N2 0.73601(11) 0.22419(13) 0.41575(9) 0.0374(3) Uani d . 1 1
Zn Zn1 1.0000 0.07951(2) 0.2500 0.03065(9) Uani d S 1 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0346(7) 0.0395(8) 0.0308(7) 0.0067(6) 0.0040(6) 0.0015(6)
C2 0.0835(16) 0.0979(19) 0.0448(10) 0.0500(14) 0.0178(10) 0.0316(11)
C3 0.0737(14) 0.0870(16) 0.0592(12) 0.0511(13) 0.0165(10) 0.0251(11)
C4 0.0439(9) 0.0499(10) 0.0437(9) -0.0023(7) 0.0163(7) -0.0125(8)
C5 0.0408(9) 0.0609(12) 0.0603(11) -0.0004(8) -0.0097(8) 0.0075(10)
C6 0.0346(8) 0.0439(9) 0.0402(8) 0.0035(6) 0.0096(6) -0.0074(7)
C7 0.0489(10) 0.0507(11) 0.0674(13) 0.0018(8) -0.0055(9) 0.0146(10)
Cl1 0.0367(2) 0.0478(2) 0.0369(2) 0.00320(16) -0.00610(14) 0.00531(16)
N1 0.0407(7) 0.0447(8) 0.0319(6) 0.0120(6) 0.0078(5) 0.0048(6)
N2 0.0360(6) 0.0390(7) 0.0371(7) 0.0064(5) 0.0079(5) -0.0017(5)
Zn1 0.02814(14) 0.03731(15) 0.02650(14) 0.000 0.00440(8) 0.000
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'
N N 0.0061 0.0033 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 N2 . . 111.35(14)
N1 C1 H1 . . 124.3
N2 C1 H1 . . 124.3
C3 C2 N1 . . 109.55(17)
C3 C2 H2 . . 125.2
N1 C2 H2 . . 125.2
C2 C3 N2 . . 106.38(16)
C2 C3 H3 . . 126.8
N2 C3 H3 . . 126.8
N2 C4 C6 . . 112.43(13)
N2 C4 H4A . . 109.1
C6 C4 H4A . . 109.1
N2 C4 H4B . . 109.1
C6 C4 H4B . . 109.1
H4A C4 H4B . . 107.8
C6 C5 C7 . 5_656 120.26(17)
C6 C5 H5 . . 119.9
C7 C5 H5 5_656 . 119.9
C5 C6 C7 . . 118.89(16)
C5 C6 C4 . . 120.07(16)
C7 C6 C4 . . 121.04(17)
C6 C7 C5 . 5_656 120.84(19)
C6 C7 H7 . . 119.6
C5 C7 H7 5_656 . 119.6
C1 N1 C2 . . 105.29(14)
C1 N1 Zn1 . . 124.96(11)
C2 N1 Zn1 . . 128.33(12)
C1 N2 C3 . . 107.42(14)
C1 N2 C4 . . 125.82(14)
C3 N2 C4 . . 126.67(15)
N1 Zn1 N1 3_755 . 117.19(8)
N1 Zn1 Cl1 3_755 3_755 103.09(4)
N1 Zn1 Cl1 . 3_755 108.98(4)
N1 Zn1 Cl1 3_755 . 108.98(4)
N1 Zn1 Cl1 . . 103.09(4)
Cl1 Zn1 Cl1 3_755 . 116.08(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.3146(19)
C1 N2 . 1.3343(19)
C1 H1 . 0.9300
C2 C3 . 1.350(3)
C2 N1 . 1.365(2)
C2 H2 . 0.9300
C3 N2 . 1.350(2)
C3 H3 . 0.9300
C4 N2 . 1.4718(19)
C4 C6 . 1.514(2)
C4 H4A . 0.9700
C4 H4B . 0.9700
C5 C6 . 1.375(3)
C5 C7 5_656 1.384(3)
C5 H5 . 0.9300
C6 C7 . 1.381(3)
C7 C5 5_656 1.384(3)
C7 H7 . 0.9300
Cl1 Zn1 . 2.2606(5)
N1 Zn1 . 1.9959(13)
Zn1 N1 3_755 1.9959(13)
Zn1 Cl1 3_755 2.2606(5)
_journal_paper_doi 10.1107/S1600536812015395