#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/29/4332996.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4332996
loop_
_publ_author_name
'Sun, Jinyu'
'Zhou, Yaming'
'Fang, Qianrong'
'Chen, Zhenxia'
'Weng, Linhong'
'Zhu, Guangshan'
'Qiu, Shilun'
'Zhao, Dongyuan'
_publ_section_title
;
 Construction of 3D Layer-Pillared Homoligand Coordination Polymers from a
 2D Layered Precursor
;
_journal_issue                   21
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8677
_journal_page_last               8684
_journal_paper_doi               10.1021/ic0612303
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C18 H22 N2 O9 Zn1.50'
_chemical_formula_sum            'C18 H22 N2 O9 Zn1.5'
_chemical_formula_weight         508.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 106.892(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.045(5)
_cell_length_b                   9.655(3)
_cell_length_c                   18.462(6)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      1.63
_cell_volume                     2225.0(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10275
_diffrn_reflns_theta_full        26.51
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0344
_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)+(0.0500P)²+0.7398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                3815
_reflns_number_total             4612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0612303sup1.cif
_cod_data_source_block           f10522a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C18 H22 N2 O9 Zn1.50'
_cod_database_code               4332996
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.25781(2) 0.54356(3) 0.048316(15) 0.02537(10) Uani 1 1 d .
Zn2 Zn 0.0000 0.5000 0.0000 0.02425(11) Uani 1 2 d S
O1 O 0.08369(15) 0.3638(2) 0.07916(10) 0.0357(4) Uani 1 1 d .
O2 O 0.25245(15) 0.4275(2) 0.13458(10) 0.0385(5) Uani 1 1 d .
O3 O 0.06891(16) 0.0617(2) 0.41741(10) 0.0390(5) Uani 1 1 d .
O4 O 0.24782(15) 0.0607(2) 0.45674(10) 0.0382(5) Uani 1 1 d .
O5 O 0.12607(14) 0.65678(18) 0.04104(10) 0.0313(4) Uani 1 1 d .
O6 O 0.22136(18) 0.7789(2) -0.01674(15) 0.0557(6) Uani 1 1 d .
O7 O 0.40263(18) 0.6119(3) 0.09157(16) 0.0515(6) Uani 1 1 d .
H7W1 H 0.430(3) 0.652(5) 0.067(2) 0.069(14) Uiso 1 1 d .
H7W2 H 0.454(4) 0.563(5) 0.124(3) 0.088(15) Uiso 1 1 d .
C1 C 0.1666(2) 0.3661(3) 0.13360(14) 0.0293(5) Uani 1 1 d .
C2 C 0.1660(2) 0.2904(3) 0.20465(14) 0.0302(6) Uani 1 1 d .
C3 C 0.2581(2) 0.2810(3) 0.26486(15) 0.0392(7) Uani 1 1 d .
H3A H 0.3218 0.3184 0.2607 0.047 Uiso 1 1 calc R
C4 C 0.2559(2) 0.2162(3) 0.33139(15) 0.0395(7) Uani 1 1 d .
H4A H 0.3181 0.2109 0.3718 0.047 Uiso 1 1 calc R
C5 C 0.1620(2) 0.1595(3) 0.33790(14) 0.0316(6) Uani 1 1 d .
C6 C 0.0696(2) 0.1666(3) 0.27710(16) 0.0449(8) Uani 1 1 d .
H6A H 0.0062 0.1278 0.2810 0.054 Uiso 1 1 calc R
C7 C 0.0718(2) 0.2313(4) 0.21072(16) 0.0431(7) Uani 1 1 d .
H7B H 0.0100 0.2353 0.1700 0.052 Uiso 1 1 calc R
C8 C 0.1582(2) 0.0886(3) 0.40959(14) 0.0319(6) Uani 1 1 d .
C9 C 0.1435(2) 0.7696(3) 0.00780(15) 0.0347(6) Uani 1 1 d .
C10 C 0.0678(2) 0.8878(3) 0.00336(15) 0.0310(6) Uani 1 1 d .
C11 C -0.0036(2) 0.8875(3) 0.04584(16) 0.0369(6) Uani 1 1 d .
H11A H -0.0058 0.8125 0.0770 0.044 Uiso 1 1 calc R
C12 C 0.0723(2) 1.0010(3) -0.04218(17) 0.0383(6) Uani 1 1 d .
H12A H 0.1211 1.0021 -0.0702 0.046 Uiso 1 1 calc R
N1 N 0.7024(2) 0.3482(4) 0.22096(17) 0.0687(9) Uani 1 1 d .
O8 O 0.5462(2) 0.4629(4) 0.18930(18) 0.0845(10) Uani 1 1 d .
C13 C 0.6227(3) 0.4144(4) 0.1739(2) 0.0608(9) Uani 1 1 d .
H13 H 0.629(3) 0.420(4) 0.124(2) 0.077(13) Uiso 1 1 d .
C14 C 0.7064(5) 0.3357(10) 0.2997(3) 0.183(4) Uani 1 1 d .
H14A H 0.6422 0.3738 0.3071 0.274 Uiso 1 1 calc R
H14B H 0.7674 0.3852 0.3304 0.274 Uiso 1 1 calc R
H14C H 0.7122 0.2397 0.3140 0.274 Uiso 1 1 calc R
C15 C 0.7923(4) 0.2952(6) 0.1995(3) 0.0952(16) Uani 1 1 d .
H15A H 0.7811 0.3101 0.1464 0.143 Uiso 1 1 calc R
H15B H 0.7997 0.1978 0.2102 0.143 Uiso 1 1 calc R
H15C H 0.8563 0.3422 0.2277 0.143 Uiso 1 1 calc R
N2 N 0.4803(3) 0.1145(4) 0.0816(2) 0.0818(11) Uani 1 1 d .
O9 O 0.4957(3) 0.2348(4) -0.0188(2) 0.1083(13) Uani 1 1 d .
C16 C 0.5344(4) 0.1672(5) 0.0361(3) 0.0810(13) Uani 1 1 d .
H16 H 0.623(5) 0.135(7) 0.060(3) 0.15(2) Uiso 1 1 d .
C17 C 0.3717(5) 0.1416(7) 0.0687(4) 0.137(3) Uani 1 1 d .
H17A H 0.3464 0.1983 0.0243 0.205 Uiso 1 1 calc R
H17B H 0.3610 0.1893 0.1115 0.205 Uiso 1 1 calc R
H17C H 0.3327 0.0559 0.0613 0.205 Uiso 1 1 calc R
C18 C 0.5356(6) 0.0313(7) 0.1449(4) 0.128(2) Uani 1 1 d .
H18A H 0.6094 0.0224 0.1461 0.192 Uiso 1 1 calc R
H18B H 0.5033 -0.0588 0.1404 0.192 Uiso 1 1 calc R
H18C H 0.5314 0.0744 0.1908 0.192 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
Zn Zn 0.2839 1.4301 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
O4 Zn1 O7 110.24(10) 4_565 .
O4 Zn1 O2 113.66(9) 4_565 .
O7 Zn1 O2 96.89(10) . .
O4 Zn1 O5 112.63(8) 4_565 .
O7 Zn1 O5 123.68(10) . .
O2 Zn1 O5 97.67(8) . .
O1 Zn2 O1 180.00(8) . 3_565
O1 Zn2 O3 94.94(8) . 4_565
O1 Zn2 O3 85.06(8) 3_565 4_565
O1 Zn2 O3 85.06(8) . 2
O1 Zn2 O3 94.94(8) 3_565 2
O3 Zn2 O3 180.00(8) 4_565 2
O1 Zn2 O5 89.65(7) . 3_565
O1 Zn2 O5 90.35(7) 3_565 3_565
O3 Zn2 O5 89.40(8) 4_565 3_565
O3 Zn2 O5 90.60(8) 2 3_565
O1 Zn2 O5 90.35(7) . .
O1 Zn2 O5 89.65(7) 3_565 .
O3 Zn2 O5 90.60(8) 4_565 .
O3 Zn2 O5 89.40(8) 2 .
O5 Zn2 O5 180.00(9) 3_565 .
C1 O1 Zn2 136.73(18) . .
C1 O2 Zn1 119.75(16) . .
C8 O3 Zn2 140.21(18) . 2_545
C8 O4 Zn1 121.62(17) . 4_566
C9 O5 Zn1 102.93(16) . .
C9 O5 Zn2 128.92(16) . .
Zn1 O5 Zn2 100.84(8) . .
O1 C1 O2 125.4(2) . .
O1 C1 C2 118.2(2) . .
O2 C1 C2 116.4(2) . .
C3 C2 C7 119.4(2) . .
C3 C2 C1 120.6(2) . .
C7 C2 C1 119.9(2) . .
C2 C3 C4 120.4(3) . .
C5 C4 C3 120.2(3) . .
C4 C5 C6 119.6(2) . .
C4 C5 C8 121.0(2) . .
C6 C5 C8 119.4(2) . .
C7 C6 C5 120.1(3) . .
C6 C7 C2 120.2(3) . .
O3 C8 O4 125.8(2) . .
O3 C8 C5 118.0(2) . .
O4 C8 C5 116.2(2) . .
O6 C9 O5 120.7(2) . .
O6 C9 C10 121.8(3) . .
O5 C9 C10 117.5(2) . .
C11 C10 C12 119.9(2) . .
C11 C10 C9 120.7(2) . .
C12 C10 C9 119.4(2) . .
C10 C11 C12 120.2(3) . 3_575
C11 C12 C10 119.9(3) 3_575 .
C13 N1 C15 123.0(4) . .
C13 N1 C14 119.8(4) . .
C15 N1 C14 117.0(4) . .
O8 C13 N1 125.7(4) . .
C16 N2 C17 121.0(4) . .
C16 N2 C18 119.5(5) . .
C17 N2 C18 119.5(5) . .
O9 C16 N2 124.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.9392(18) 4_565
Zn1 O7 1.940(2) .
Zn1 O2 1.9654(18) .
Zn1 O5 2.0080(18) .
Zn2 O1 2.0325(18) .
Zn2 O1 2.0325(18) 3_565
Zn2 O3 2.0698(18) 4_565
Zn2 O3 2.0698(18) 2
Zn2 O5 2.2013(18) 3_565
Zn2 O5 2.2013(19) .
O1 C1 1.244(3) .
O2 C1 1.263(3) .
O3 C8 1.243(3) .
O3 Zn2 2.0698(18) 2_545
O4 C8 1.267(3) .
O4 Zn1 1.9392(18) 4_566
O5 C9 1.302(3) .
O6 C9 1.230(3) .
C1 C2 1.504(3) .
C2 C3 1.382(4) .
C2 C7 1.388(4) .
C3 C4 1.386(4) .
C4 C5 1.379(4) .
C5 C6 1.390(4) .
C5 C8 1.504(3) .
C6 C7 1.383(4) .
C9 C10 1.495(4) .
C10 C11 1.382(4) .
C10 C12 1.391(4) .
C11 C12 1.389(4) 3_575
C12 C11 1.389(4) 3_575
N1 C13 1.311(5) .
N1 C15 1.437(5) .
N1 C14 1.445(6) .
O8 C13 1.209(5) .
N2 C16 1.344(6) .
N2 C17 1.392(6) .
N2 C18 1.430(6) .
O9 C16 1.187(5) .
