#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/05/2100590.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_2100590
loop_
_publ_author_name
'S. M. Hawxwell'
'H. Adams'
'L. Brammer'
_publ_section_title
;
 Two-dimensional metal-organic frameworks containing linear
 dicarboxylates
;
_journal_coeditor_code           BM5038
_journal_date_accepted           2006-08-18
_journal_date_recd_electronic    2006-06-14
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              808
_journal_page_last               814
_journal_paper_category          FA
_journal_paper_doi               10.1107/S0108768106033283
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C24 H16 O14 Zn3, 4(C3 H7 N O)'
_chemical_formula_sum            'C36 H44 N4 O18 Zn3'
_chemical_formula_weight         1016.86
_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                 108.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.968(2)
_cell_length_b                   9.761(3)
_cell_length_c                   18.336(2)
_cell_measurement_reflns_used    1451
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.732
_cell_measurement_theta_min      7.492
_cell_volume                     2198.6(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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           synchrotron
_diffrn_radiation_wavelength     0.84600
_diffrn_reflns_av_R_equivalents  0.117
_diffrn_reflns_av_sigmaI/netI    0.2043
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26356
_diffrn_reflns_theta_full        32.21
_diffrn_reflns_theta_max         32.21
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    1.700
_exptl_absorpt_correction_T_max  0.9508
_exptl_absorpt_correction_T_min  0.8484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.605
_refine_diff_density_min         -1.008
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         8551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_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          0.1175
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                4219
_reflns_number_total             8551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm5038.cif
_cod_data_source_block           3
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2198.7(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               2100590
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_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
Zn Zn1 0.76557(5) 0.05221(5) 0.06460(3) 0.01967(16) Uani d . 1
Zn Zn2 0.5000 0.0000 0.0000 0.0188(2) Uani d S 1
O O1 0.5684(3) -0.0444(3) 0.11715(19) 0.0299(9) Uani d . 1
O O2 0.7527(3) -0.0459(3) 0.15464(18) 0.0245(9) Uani d . 1
O O3 0.5898(3) -0.3593(3) 0.4645(2) 0.0256(9) Uani d . 1
O O4 0.7620(3) -0.4258(3) 0.47858(18) 0.0228(9) Uani d . 1
C C1 0.6617(5) -0.0709(5) 0.1636(3) 0.0230(13) Uani d . 1
C C2 0.6644(4) -0.1422(5) 0.2386(3) 0.0217(13) Uani d . 1
C C3 0.5693(4) -0.1675(5) 0.2548(3) 0.0299(14) Uani d . 1
H H3 0.5015 -0.1382 0.2200 0.036 Uiso calc R 1
C C4 0.5729(4) -0.2364(5) 0.3223(3) 0.0285(14) Uani d . 1
H H4 0.5079 -0.2529 0.3341 0.034 Uiso calc R 1
C C5 0.6725(4) -0.2805(5) 0.3721(3) 0.0223(13) Uani d . 1
C C6 0.7678(4) -0.2539(5) 0.3566(3) 0.0239(13) Uani d . 1
H H6 0.8355 -0.2844 0.3910 0.029 Uiso calc R 1
C C7 0.7641(4) -0.1820(5) 0.2902(3) 0.0236(13) Uani d . 1
H H7 0.8296 -0.1603 0.2801 0.028 Uiso calc R 1
C C8 0.6737(5) -0.3630(5) 0.4443(3) 0.0254(14) Uani d . 1
O O10 0.6226(3) 0.1538(3) 0.00540(19) 0.0261(9) Uani d . 1
O O11 0.7326(3) 0.2773(3) 0.0994(2) 0.0350(10) Uani d . 1
C C10 0.6448(4) 0.2689(5) 0.0447(3) 0.0240(13) Uani d . 1
C C11 0.5691(4) 0.3882(5) 0.0206(3) 0.0216(12) Uani d . 1
C C12 0.5824(5) 0.4994(5) 0.0707(3) 0.0333(14) Uani d . 1
H H12 0.6384 0.4984 0.1192 0.040 Uiso calc R 1
C C13 0.4867(4) 0.3887(5) -0.0492(3) 0.0230(13) Uani d . 1
H H13 0.4773 0.3121 -0.0827 0.028 Uiso calc R 1
O O1W 0.9194(3) 0.1030(3) 0.0860(2) 0.0347(10) Uani d . 1
H H1WA 0.9830 0.0460 0.0985 0.042 Uiso d R 1
H H1WB 0.9589 0.1834 0.1092 0.042 Uiso d R 1
O O1S 0.9733(3) 0.3638(4) 0.0933(2) 0.0431(11) Uani d . 1
N N1S 0.9143(4) 0.5693(5) 0.1243(3) 0.0390(13) Uani d . 1
C C1S 0.9490(5) 0.4420(7) 0.1399(4) 0.0456(17) Uani d . 1
H H1S 0.9560 0.4071 0.1896 0.055 Uiso calc R 1
C C2S 0.8851(6) 0.6538(6) 0.1809(4) 0.060(2) Uani d . 1
H H2S1 0.8071 0.6742 0.1618 0.091 Uiso calc R 1
H H2S2 0.9265 0.7396 0.1889 0.091 Uiso calc R 1
H H2S3 0.9023 0.6040 0.2297 0.091 Uiso calc R 1
C C3S 0.8886(6) 0.6236(6) 0.0465(4) 0.062(2) Uani d . 1
H H3S1 0.9371 0.5822 0.0212 0.093 Uiso calc R 1
H H3S2 0.8986 0.7232 0.0488 0.093 Uiso calc R 1
H H3S3 0.8129 0.6019 0.0172 0.093 Uiso calc R 1
O O2S 0.0720(3) 0.9293(4) 0.1568(2) 0.0460(12) Uani d . 1
N N2S 0.1872(4) 0.7607(5) 0.1466(3) 0.0384(13) Uani d . 1
C C4S 0.1128(5) 0.8567(6) 0.1162(4) 0.0388(17) Uani d . 1
H H4S 0.0897 0.8709 0.0621 0.047 Uiso calc R 1
C C5S 0.2249(6) 0.7342(7) 0.2277(3) 0.076(3) Uani d . 1
H H5S1 0.2160 0.8167 0.2555 0.113 Uiso calc R 1
H H5S2 0.3020 0.7086 0.2437 0.113 Uiso calc R 1
H H5S3 0.1826 0.6590 0.2394 0.113 Uiso calc R 1
C C6S 0.2296(6) 0.6747(6) 0.0970(4) 0.058(2) Uani d . 1
H H6S1 0.1924 0.6982 0.0429 0.087 Uiso calc R 1
H H6S2 0.2166 0.5781 0.1055 0.087 Uiso calc R 1
H H6S3 0.3079 0.6906 0.1093 0.087 Uiso calc R 1
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'
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'
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
O2 Zn1 O1W . . 108.00(15)
O2 Zn1 O4 . 4 112.18(13)
O1W Zn1 O4 . 4 94.50(15)
O2 Zn1 O10 . . 111.77(14)
O1W Zn1 O10 . . 131.45(13)
O4 Zn1 O10 4 . 95.27(14)
O2 Zn1 O11 . . 98.94(14)
O1W Zn1 O11 . . 88.38(13)
O4 Zn1 O11 4 . 145.99(13)
O10 Zn1 O11 . . 59.25(13)
O3 Zn2 O3 4 2_655 180.0(2)
O3 Zn2 O1 4 . 95.18(14)
O3 Zn2 O1 2_655 . 84.82(14)
O3 Zn2 O1 4 3_655 84.82(14)
O3 Zn2 O1 2_655 3_655 95.18(14)
O1 Zn2 O1 . 3_655 180.00(9)
O3 Zn2 O10 4 3_655 90.26(13)
O3 Zn2 O10 2_655 3_655 89.74(13)
O1 Zn2 O10 . 3_655 88.10(13)
O1 Zn2 O10 3_655 3_655 91.90(13)
O3 Zn2 O10 4 . 89.74(13)
O3 Zn2 O10 2_655 . 90.26(13)
O1 Zn2 O10 . . 91.90(13)
O1 Zn2 O10 3_655 . 88.10(13)
O10 Zn2 O10 3_655 . 180.0(2)
C1 O1 Zn2 . . 137.3(3)
C1 O2 Zn1 . . 122.5(3)
C8 O3 Zn2 . 2_645 135.4(3)
C8 O4 Zn1 . 4_556 118.5(3)
O1 C1 O2 . . 127.1(5)
O1 C1 C2 . . 116.1(5)
O2 C1 C2 . . 116.7(5)
C3 C2 C7 . . 120.2(5)
C3 C2 C1 . . 120.6(5)
C7 C2 C1 . . 119.1(5)
C2 C3 C4 . . 119.9(5)
C2 C3 H3 . . 120.1
C4 C3 H3 . . 120.1
C5 C4 C3 . . 119.5(5)
C5 C4 H4 . . 120.2
C3 C4 H4 . . 120.2
C6 C5 C4 . . 120.8(5)
C6 C5 C8 . . 120.7(5)
C4 C5 C8 . . 118.5(5)
C5 C6 C7 . . 119.5(5)
C5 C6 H6 . . 120.2
C7 C6 H6 . . 120.2
C2 C7 C6 . . 120.0(5)
C2 C7 H7 . . 120.0
C6 C7 H7 . . 120.0
O3 C8 O4 . . 126.5(5)
O3 C8 C5 . . 117.7(5)
O4 C8 C5 . . 115.7(5)
C10 O10 Zn1 . . 96.9(3)
C10 O10 Zn2 . . 130.2(3)
Zn1 O10 Zn2 . . 102.26(13)
C10 O11 Zn1 . . 85.4(3)
O11 C10 O10 . . 118.4(5)
O11 C10 C11 . . 121.7(5)
O10 C10 C11 . . 119.7(5)
C13 C11 C12 . . 120.3(5)
C13 C11 C10 . . 121.1(5)
C12 C11 C10 . . 118.6(5)
C13 C12 C11 3_665 . 119.5(5)
C13 C12 H12 3_665 . 120.3
C11 C12 H12 . . 120.3
C11 C13 C12 . 3_665 120.3(5)
C11 C13 H13 . . 119.9
C12 C13 H13 3_665 . 119.9
Zn1 O1W H1WA . . 129.8
Zn1 O1W H1WB . . 131.1
H1WA O1W H1WB . . 94.1
C1S N1S C3S . . 120.6(5)
C1S N1S C2S . . 121.5(5)
C3S N1S C2S . . 117.3(5)
O1S C1S N1S . . 124.4(6)
O1S C1S H1S . . 117.8
N1S C1S H1S . . 117.8
N1S C2S H2S1 . . 109.5
N1S C2S H2S2 . . 109.5
H2S1 C2S H2S2 . . 109.5
N1S C2S H2S3 . . 109.5
H2S1 C2S H2S3 . . 109.5
H2S2 C2S H2S3 . . 109.5
N1S C3S H3S1 . . 109.5
N1S C3S H3S2 . . 109.5
H3S1 C3S H3S2 . . 109.5
N1S C3S H3S3 . . 109.5
H3S1 C3S H3S3 . . 109.5
H3S2 C3S H3S3 . . 109.5
C4S N2S C5S . . 121.5(5)
C4S N2S C6S . . 120.5(5)
C5S N2S C6S . . 117.9(5)
O2S C4S N2S . . 122.2(6)
O2S C4S H4S . . 118.9
N2S C4S H4S . . 118.9
N2S C5S H5S1 . . 109.5
N2S C5S H5S2 . . 109.5
H5S1 C5S H5S2 . . 109.5
N2S C5S H5S3 . . 109.5
H5S1 C5S H5S3 . . 109.5
H5S2 C5S H5S3 . . 109.5
N2S C6S H6S1 . . 109.5
N2S C6S H6S2 . . 109.5
H6S1 C6S H6S2 . . 109.5
N2S C6S H6S3 . . 109.5
H6S1 C6S H6S3 . . 109.5
H6S2 C6S H6S3 . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Zn1 O2 . 1.962(3)
Zn1 O1W . 1.969(3)
Zn1 O4 4 1.992(3)
Zn1 O10 . 2.076(3)
Zn1 O11 . 2.365(3)
Zn2 O3 4 2.038(3)
Zn2 O3 2_655 2.038(3)
Zn2 O1 . 2.090(3)
Zn2 O1 3_655 2.090(3)
Zn2 O10 3_655 2.166(3)
Zn2 O10 . 2.166(3)
O1 C1 . 1.263(6)
O2 C1 . 1.267(6)
O3 C8 . 1.257(6)
O3 Zn2 2_645 2.038(3)
O4 C8 . 1.274(6)
O4 Zn1 4_556 1.992(3)
C1 C2 . 1.531(6)
C2 C3 . 1.380(7)
C2 C7 . 1.390(7)
C3 C4 . 1.397(6)
C3 H3 . 0.9500
C4 C5 . 1.389(7)
C4 H4 . 0.9500
C5 C6 . 1.379(7)
C5 C8 . 1.546(7)
C6 C7 . 1.393(6)
C6 H6 . 0.9500
C7 H7 . 0.9500
O10 C10 . 1.315(6)
O11 C10 . 1.256(5)
C10 C11 . 1.496(6)
C11 C13 . 1.379(6)
C11 C12 . 1.397(6)
C12 C13 3_665 1.388(6)
C12 H12 . 0.9500
C13 C12 3_665 1.388(6)
C13 H13 . 0.9500
O1W H1WA . 0.9599
O1W H1WB . 0.9600
O1S C1S . 1.259(7)
N1S C1S . 1.322(7)
N1S C3S . 1.456(7)
N1S C2S . 1.467(7)
C1S H1S . 0.9500
C2S H2S1 . 0.9800
C2S H2S2 . 0.9800
C2S H2S3 . 0.9800
C3S H3S1 . 0.9800
C3S H3S2 . 0.9800
C3S H3S3 . 0.9800
O2S C4S . 1.261(6)
N2S C4S . 1.332(7)
N2S C5S . 1.432(6)
N2S C6S . 1.468(7)
C4S H4S . 0.9500
C5S H5S1 . 0.9800
C5S H5S2 . 0.9800
C5S H5S3 . 0.9800
C6S H6S1 . 0.9800
C6S H6S2 . 0.9800
C6S H6S3 . 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H1WA O2S 1_645 0.96 1.73 2.614(5) 152.0
O1W H1WB O1S . 0.96 1.80 2.632(5) 142.6
