#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:07:42 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180491 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/60/7216012.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_7216012
loop_
_publ_author_name
'Hawxwell, Samuel M.'
'Brammer, Lee'
_publ_section_title
;
 Solvent hydrolysis leads to an unusual Cu(ii) metal--organic framework
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              473
_journal_paper_doi               10.1039/b603274e
_journal_volume                  8
_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                 108.577(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8991(12)
_cell_length_b                   9.7403(9)
_cell_length_c                   18.2827(18)
_cell_measurement_reflns_used    1451
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.732
_cell_measurement_theta_min      7.492
_cell_volume                     2177.4(4)
_computing_cell_refinement       'Bruker APEX 2'
_computing_data_collection       'Bruker APEX 2'
_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 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.84600
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2121
_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       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8751
_diffrn_reflns_theta_full        32.98
_diffrn_reflns_theta_max         32.98
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    1.716
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_correction_T_min  0.8471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.551
_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         1.617
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         8751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.830
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.0668
_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)+(0.0494P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                4181
_reflns_number_total             8751
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7203372
_cod_data_source_file            b603274e.txt
_cod_data_source_block           hkl5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7216012
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 0.26552(5) 0.44779(6) -0.93549(4) 0.01933(17) Uani 1 1 d .
Zn2 Zn 0.0000 0.5000 -1.0000 0.0184(2) Uani 1 2 d S
O1 O 0.2528(3) 0.5456(4) -0.84549(19) 0.0238(9) Uani 1 1 d .
O2 O 0.0685(3) 0.5444(4) -0.8830(2) 0.0294(10) Uani 1 1 d .
O3 O 0.0896(3) 0.8593(3) -0.5356(2) 0.0253(9) Uani 1 1 d .
O4 O 0.2620(3) 0.9260(3) -0.52133(19) 0.0226(9) Uani 1 1 d .
C1 C 0.1622(5) 0.5708(5) -0.8365(3) 0.0228(13) Uani 1 1 d .
C2 C 0.1646(5) 0.6418(5) -0.7617(3) 0.0233(14) Uani 1 1 d .
C3 C 0.2640(5) 0.6822(5) -0.7102(3) 0.0239(13) Uani 1 1 d .
H3 H 0.3300 0.6609 -0.7203 0.029 Uiso 1 1 calc R
C4 C 0.2674(4) 0.7538(5) -0.6437(3) 0.0227(13) Uani 1 1 d .
H4 H 0.3355 0.7840 -0.6092 0.027 Uiso 1 1 calc R
C5 C 0.1723(5) 0.7806(5) -0.6279(3) 0.0216(13) Uani 1 1 d .
C6 C 0.0728(5) 0.7362(6) -0.6776(3) 0.0284(14) Uani 1 1 d .
H6 H 0.0073 0.7528 -0.6657 0.034 Uiso 1 1 calc R
C7 C 0.0692(5) 0.6669(6) -0.7452(3) 0.0299(15) Uani 1 1 d .
H7 H 0.0011 0.6371 -0.7799 0.036 Uiso 1 1 calc R
C8 C 0.1730(5) 0.8625(5) -0.5558(3) 0.0252(14) Uani 1 1 d .
O10 O 0.1226(3) 0.3462(3) -0.9948(2) 0.0259(10) Uani 1 1 d .
O11 O 0.2327(3) 0.2226(4) -0.9006(2) 0.0344(10) Uani 1 1 d .
C10 C 0.1448(5) 0.2311(6) -0.9552(3) 0.0245(14) Uani 1 1 d .
C11 C 0.0692(4) 0.1120(5) -0.9795(3) 0.0215(13) Uani 1 1 d .
C12 C 0.0824(5) 0.0003(6) -0.9296(3) 0.0336(15) Uani 1 1 d .
H12 H 0.1390 0.0010 -0.8813 0.040 Uiso 1 1 calc R
C13 C -0.0131(4) 0.1117(5) -1.0495(3) 0.0227(13) Uani 1 1 d .
H13 H -0.0222 0.1880 -1.0833 0.027 Uiso 1 1 calc R
O1W O 0.4203(3) 0.3978(3) -0.9149(2) 0.0327(10) Uani 1 1 d .
H1WA H 0.4637 0.4252 -0.8639 0.039 Uiso 1 1 d R
H1WB H 0.4306 0.3029 -0.9002 0.039 Uiso 1 1 d R
O1S O 0.4280(3) 0.4295(4) -1.1569(2) 0.0458(12) Uani 1 1 d .
N1S N 0.3125(4) 0.2607(5) -1.1466(3) 0.0381(14) Uani 1 1 d .
C1S C 0.3874(5) 0.3571(6) -1.1160(4) 0.0376(17) Uani 1 1 d .
H1S H 0.4106 0.3714 -1.0617 0.045 Uiso 1 1 calc R
C2S C 0.2704(6) 0.1752(7) -1.0968(4) 0.057(2) Uani 1 1 d .
H2S1 H 0.2829 0.0783 -1.1057 0.085 Uiso 1 1 calc R
H2S2 H 0.1918 0.1917 -1.1086 0.085 Uiso 1 1 calc R
H2S3 H 0.3083 0.1983 -1.0427 0.085 Uiso 1 1 calc R
C3S C 0.2748(6) 0.2340(8) -1.2278(4) 0.074(3) Uani 1 1 d .
H3S1 H 0.2845 0.3164 -1.2556 0.110 Uiso 1 1 calc R
H3S2 H 0.1971 0.2093 -1.2438 0.110 Uiso 1 1 calc R
H3S3 H 0.3169 0.1581 -1.2394 0.110 Uiso 1 1 calc R
O2S O 0.4736(3) 0.1361(4) -0.9066(3) 0.0417(12) Uani 1 1 d .
N2S N 0.4142(4) -0.0691(5) -0.8757(3) 0.0371(13) Uani 1 1 d .
C4S C 0.4489(5) 0.0583(7) -0.8598(4) 0.0440(17) Uani 1 1 d .
H4S H 0.4557 0.0933 -0.8100 0.053 Uiso 1 1 calc R
C5S C 0.3889(6) -0.1239(7) -0.9534(4) 0.060(2) Uani 1 1 d .
H5S1 H 0.3129 -0.1022 -0.9829 0.089 Uiso 1 1 calc R
H5S2 H 0.3989 -0.2237 -0.9509 0.089 Uiso 1 1 calc R
H5S3 H 0.4378 -0.0826 -0.9787 0.089 Uiso 1 1 calc R
C6S C 0.3845(6) -0.1537(7) -0.8190(4) 0.059(2) Uani 1 1 d .
H6S1 H 0.4260 -0.2397 -0.8109 0.088 Uiso 1 1 calc R
H6S2 H 0.3061 -0.1740 -0.8382 0.088 Uiso 1 1 calc R
H6S3 H 0.4016 -0.1038 -0.7700 0.088 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'
N N 0.0061 0.0033 '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
O1 Zn1 O1W 108.16(16) . .
O1 Zn1 O4 112.16(14) . 4_575
O1W Zn1 O4 94.06(15) . 4_575
O1 Zn1 O10 112.00(14) . .
O1W Zn1 O10 131.39(14) . .
O4 Zn1 O10 95.17(14) 4_575 .
O1 Zn1 O11 98.92(14) . .
O1W Zn1 O11 88.69(14) . .
O4 Zn1 O11 146.05(14) 4_575 .
O10 Zn1 O11 59.35(13) . .
O3 Zn2 O3 180.00(17) 4_575 2_543
O3 Zn2 O2 95.17(15) 4_575 .
O3 Zn2 O2 84.83(14) 2_543 .
O3 Zn2 O2 84.83(14) 4_575 3_563
O3 Zn2 O2 95.17(15) 2_543 3_563
O2 Zn2 O2 180.000(1) . 3_563
O3 Zn2 O10 90.06(14) 4_575 3_563
O3 Zn2 O10 89.94(14) 2_543 3_563
O2 Zn2 O10 88.08(14) . 3_563
O2 Zn2 O10 91.92(14) 3_563 3_563
O3 Zn2 O10 89.94(14) 4_575 .
O3 Zn2 O10 90.06(14) 2_543 .
O2 Zn2 O10 91.92(14) . .
O2 Zn2 O10 88.08(14) 3_563 .
O10 Zn2 O10 180.00(19) 3_563 .
C1 O1 Zn1 122.5(3) . .
C1 O2 Zn2 137.4(4) . .
C8 O3 Zn2 135.5(3) . 2_553
C8 O4 Zn1 118.8(3) . 4_576
O1 C1 O2 127.1(5) . .
O1 C1 C2 116.9(5) . .
O2 C1 C2 116.0(5) . .
C7 C2 C3 120.0(5) . .
C7 C2 C1 120.8(5) . .
C3 C2 C1 119.3(5) . .
C2 C3 C4 120.1(5) . .
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 . .
C5 C4 C3 119.9(5) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 C6 120.4(5) . .
C4 C5 C8 121.2(5) . .
C6 C5 C8 118.4(5) . .
C5 C6 C7 119.6(5) . .
C5 C6 H6 120.2 . .
C7 C6 H6 120.2 . .
C2 C7 C6 119.9(5) . .
C2 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
O3 C8 O4 126.1(5) . .
O3 C8 C5 118.2(5) . .
O4 C8 C5 115.7(5) . .
C10 O10 Zn1 96.8(3) . .
C10 O10 Zn2 130.1(3) . .
Zn1 O10 Zn2 102.07(14) . .
C10 O11 Zn1 85.3(3) . .
O11 C10 O10 118.6(5) . .
O11 C10 C11 121.8(5) . .
O10 C10 C11 119.5(5) . .
C13 C11 C12 120.2(5) . .
C13 C11 C10 121.1(5) . .
C12 C11 C10 118.7(5) . .
C13 C12 C11 120.0(5) 3_553 .
C13 C12 H12 120.0 3_553 .
C11 C12 H12 120.0 . .
C11 C13 C12 119.8(5) . 3_553
C11 C13 H13 120.1 . .
C12 C13 H13 120.1 3_553 .
Zn1 O1W H1WA 110.9 . .
Zn1 O1W H1WB 109.4 . .
H1WA O1W H1WB 90.5 . .
C1S N1S C3S 121.6(5) . .
C1S N1S C2S 120.1(5) . .
C3S N1S C2S 118.2(5) . .
O1S C1S N1S 121.8(6) . .
O1S C1S H1S 119.1 . .
N1S C1S H1S 119.1 . .
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 121.0(6) . .
C4S N2S C6S 121.3(6) . .
C5S N2S C6S 117.2(5) . .
O2S C4S N2S 124.0(7) . .
O2S C4S H4S 118.0 . .
N2S C4S H4S 118.0 . .
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_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.953(3) .
Zn1 O1W 1.972(3) .
Zn1 O4 1.983(3) 4_575
Zn1 O10 2.069(4) .
Zn1 O11 2.361(4) .
Zn2 O3 2.029(3) 4_575
Zn2 O3 2.029(3) 2_543
Zn2 O2 2.082(3) .
Zn2 O2 2.082(3) 3_563
Zn2 O10 2.158(3) 3_563
Zn2 O10 2.158(3) .
O1 C1 1.255(6) .
O2 C1 1.262(6) .
O3 C8 1.245(6) .
O3 Zn2 2.029(3) 2_553
O4 C8 1.278(6) .
O4 Zn1 1.983(3) 4_576
C1 C2 1.525(7) .
C2 C7 1.379(7) .
C2 C3 1.383(7) .
C3 C4 1.391(6) .
C3 H3 0.9500 .
C4 C5 1.372(7) .
C4 H4 0.9500 .
C5 C6 1.385(7) .
C5 C8 1.537(7) .
C6 C7 1.397(7) .
C6 H6 0.9500 .
C7 H7 0.9500 .
O10 C10 1.315(6) .
O11 C10 1.253(6) .
C10 C11 1.489(7) .
C11 C13 1.377(7) .
C11 C12 1.395(7) .
C12 C13 1.385(7) 3_553
C12 H12 0.9500 .
C13 C12 1.385(7) 3_553
C13 H13 0.9500 .
O1W H1WA 0.9600 .
O1W H1WB 0.9600 .
O1S C1S 1.258(7) .
N1S C1S 1.335(7) .
N1S C3S 1.430(7) .
N1S C2S 1.460(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 1.257(7) .
N2S C4S 1.320(7) .
N2S C5S 1.453(7) .
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_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O1S 0.96 1.94 2.597(5) 123.6 3_663
O1W H1WB O2S 0.96 1.73 2.632(5) 154.5 .
