#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:14:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180383 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/52/7205222.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_7205222
loop_
_publ_author_name
'Karmakar, Anirban'
'Goldberg, Israel'
_publ_section_title
;
 Coordination polymers of flexible tetracarboxylic acids with metal
 ions. II. Supramolecular assemblies of 5,5′-methylene- and
 5,5′-(ethane-1,2-diyl)-bis(oxy)diisophthalic acid ligands with
 d-transition metals
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              350
_journal_paper_doi               10.1039/c0ce00268b
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C17 H14 O13 Zn, 3(H2 O)'
_chemical_formula_sum            'C17 H20 O16 Zn'
_chemical_formula_weight         545.70
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.7486(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.7034(4)
_cell_length_b                   7.5718(2)
_cell_length_c                   30.7679(9)
_cell_measurement_reflns_used    4655
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.32
_cell_volume                     4817.7(2)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. φ and ω 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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            16675
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.8109
_exptl_absorpt_correction_T_min  0.7007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0547
_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)+(0.0954P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                3499
_reflns_number_total             5583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00268B.TXT
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7205222
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.030140(16) 0.24782(5) 0.428744(12) 0.01617(14) Uani 1 1 d . . .
O1 O 0.04893(10) 0.2030(3) 0.10817(8) 0.0208(5) Uani 1 1 d . . .
O2 O 0.10483(10) 0.3602(4) 0.06228(9) 0.0301(6) Uani 1 1 d . . .
C3 C 0.10166(15) 0.2673(4) 0.09489(12) 0.0167(7) Uani 1 1 d . . .
C4 C 0.16214(14) 0.2221(4) 0.12220(11) 0.0169(7) Uani 1 1 d . . .
C5 C 0.15693(14) 0.1520(4) 0.16329(11) 0.0181(7) Uani 1 1 d . . .
H5 H 0.1154 0.1332 0.1743 0.022 Uiso 1 1 calc R . .
C6 C 0.21188(14) 0.1089(4) 0.18858(11) 0.0168(7) Uani 1 1 d . . .
C7 C 0.27277(14) 0.1349(4) 0.17274(11) 0.0160(7) Uani 1 1 d . . .
H7 H 0.3104 0.1029 0.1898 0.019 Uiso 1 1 calc R . .
C8 C 0.27822(14) 0.2083(4) 0.13156(11) 0.0153(7) Uani 1 1 d . . .
C9 C 0.22325(14) 0.2533(4) 0.10593(11) 0.0164(7) Uani 1 1 d . . .
H9 H 0.2271 0.3041 0.0779 0.020 Uiso 1 1 calc R . .
C10 C 0.34515(15) 0.2400(4) 0.11579(11) 0.0165(7) Uani 1 1 d . . .
O11 O 0.39216(10) 0.1862(3) 0.13971(8) 0.0245(6) Uani 1 1 d . . .
O12 O 0.35061(10) 0.3171(3) 0.07987(8) 0.0215(5) Uani 1 1 d . . .
O13 O 0.20150(9) 0.0446(3) 0.22986(7) 0.0210(5) Uani 1 1 d . . .
C14 C 0.25422(14) -0.0322(5) 0.25379(11) 0.0215(8) Uani 1 1 d . . .
H14A H 0.2374 -0.1133 0.2758 0.026 Uiso 1 1 calc R . .
H14B H 0.2799 -0.1032 0.2338 0.026 Uiso 1 1 calc R . .
O15 O 0.29504(9) 0.0934(3) 0.27492(8) 0.0206(5) Uani 1 1 d . . .
C16 C 0.28040(14) 0.1401(4) 0.31727(11) 0.0168(7) Uani 1 1 d . . .
C17 C 0.21722(14) 0.1509(4) 0.33061(11) 0.0168(7) Uani 1 1 d . . .
H17 H 0.1819 0.1245 0.3109 0.020 Uiso 1 1 calc R . .
C18 C 0.20639(15) 0.2011(4) 0.37338(12) 0.0174(7) Uani 1 1 d . . .
C19 C 0.25908(14) 0.2379(4) 0.40253(11) 0.0138(7) Uani 1 1 d . . .
H19 H 0.2520 0.2697 0.4318 0.017 Uiso 1 1 calc R . .
C20 C 0.32128(15) 0.2274(4) 0.38821(12) 0.0170(7) Uani 1 1 d . . .
C21 C 0.33196(14) 0.1782(5) 0.34558(11) 0.0181(7) Uani 1 1 d . . .
H21 H 0.3748 0.1710 0.3360 0.022 Uiso 1 1 calc R . .
C22 C 0.37883(15) 0.2623(4) 0.41928(12) 0.0184(7) Uani 1 1 d . . .
O23 O 0.36940(11) 0.2817(3) 0.45875(8) 0.0243(6) Uani 1 1 d . . .
O24 O 0.43433(10) 0.2683(3) 0.40310(8) 0.0212(6) Uani 1 1 d . . .
C25 C 0.13829(15) 0.2149(4) 0.38741(13) 0.0188(8) Uani 1 1 d . . .
O26 O 0.09287(10) 0.1866(3) 0.36044(8) 0.0244(6) Uani 1 1 d . . .
O27 O 0.12929(11) 0.2548(3) 0.42691(8) 0.0189(5) Uani 1 1 d . . .
O28 O 0.02071(12) 0.2943(4) 0.49338(8) 0.0302(6) Uani 1 1 d . . .
H28A H 0.0524 0.2309 0.5094 0.045 Uiso 1 1 d R . .
H28B H -0.0190 0.2339 0.4991 0.045 Uiso 1 1 d R . .
O29 O 0.03039(10) 0.5198(3) 0.41645(9) 0.0274(6) Uani 1 1 d . . .
H29A H 0.0596 0.5554 0.3949 0.041 Uiso 1 1 d R . .
H29B H -0.0038 0.5833 0.4146 0.041 Uiso 1 1 d R . .
O30 O 0.03583(10) -0.0313(3) 0.44135(8) 0.0232(6) Uani 1 1 d . . .
H30A H 0.0707 -0.0862 0.4285 0.035 Uiso 1 1 d R . .
H30B H 0.0014 -0.1004 0.4294 0.035 Uiso 1 1 d R . .
O31 O 0.29845(11) 0.4701(4) 0.00301(8) 0.0315(6) Uani 1 1 d . . .
H31A H 0.3221 0.5540 -0.0149 0.047 Uiso 1 1 d R . .
H31B H 0.3148 0.4791 0.0349 0.047 Uiso 1 1 d R . .
O32 O 0.33332(13) 0.0456(4) 0.01300(10) 0.0435(7) Uani 1 1 d . . .
H32A H 0.3434 -0.0756 0.0228 0.065 Uiso 1 1 d R . .
H32B H 0.3481 0.1500 0.0302 0.065 Uiso 1 1 d R . .
O33 O 0.49531(12) 0.4120(4) 0.16395(10) 0.0428(7) Uani 1 1 d . . .
H33A H 0.4613 0.3253 0.1617 0.064 Uiso 1 1 d R . .
H33B H 0.4750 0.5351 0.1608 0.064 Uiso 1 1 d 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'
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
_geom_angle_publ_flag
O1 Zn O28 118.36(10) 2 . ?
O1 Zn O27 142.07(10) 2 . ?
O28 Zn O27 99.48(10) . . ?
O1 Zn O29 94.27(10) 2 . ?
O28 Zn O29 90.43(10) . . ?
O27 Zn O29 87.62(8) . . ?
O1 Zn O30 88.37(9) 2 . ?
O28 Zn O30 90.05(10) . . ?
O27 Zn O30 89.09(8) . . ?
O29 Zn O30 176.72(8) . . ?
C3 O1 Zn 116.5(2) . 2 ?
O2 C3 O1 123.9(3) . . ?
O2 C3 C4 120.5(3) . . ?
O1 C3 C4 115.6(3) . . ?
C5 C4 C9 120.2(3) . . ?
C5 C4 C3 119.8(3) . . ?
C9 C4 C3 120.0(3) . . ?
C6 C5 C4 120.5(3) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 O13 116.0(3) . . ?
C5 C6 C7 120.3(3) . . ?
O13 C6 C7 123.7(3) . . ?
C6 C7 C8 119.4(3) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C9 C8 C7 120.8(3) . . ?
C9 C8 C10 121.1(3) . . ?
C7 C8 C10 118.1(3) . . ?
C8 C9 C4 118.8(3) . . ?
C8 C9 H9 120.6 . . ?
C4 C9 H9 120.6 . . ?
O11 C10 O12 124.3(3) . . ?
O11 C10 C8 117.1(3) . . ?
O12 C10 C8 118.6(3) . . ?
C6 O13 C14 118.2(2) . . ?
O15 C14 O13 113.2(3) . . ?
O15 C14 H14A 108.9 . . ?
O13 C14 H14A 108.9 . . ?
O15 C14 H14B 108.9 . . ?
O13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.8 . . ?
C16 O15 C14 116.7(2) . . ?
C21 C16 C17 120.9(3) . . ?
C21 C16 O15 116.5(3) . . ?
C17 C16 O15 122.6(3) . . ?
C16 C17 C18 119.3(3) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C17 C18 C19 120.0(3) . . ?
C17 C18 C25 119.1(3) . . ?
C19 C18 C25 121.0(3) . . ?
C20 C19 C18 119.4(3) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 120.5(3) . . ?
C19 C20 C22 120.3(3) . . ?
C21 C20 C22 119.1(3) . . ?
C16 C21 C20 120.0(3) . . ?
C16 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
O23 C22 O24 124.2(3) . . ?
O23 C22 C20 118.7(3) . . ?
O24 C22 C20 117.2(3) . . ?
O26 C25 O27 122.5(3) . . ?
O26 C25 C18 119.2(3) . . ?
O27 C25 C18 118.3(3) . . ?
C25 O27 Zn 102.22(19) . . ?
Zn O28 H28A 109.2 . . ?
Zn O28 H28B 102.6 . . ?
H28A O28 H28B 104.0 . . ?
Zn O29 H29A 114.1 . . ?
Zn O29 H29B 123.7 . . ?
H29A O29 H29B 110.1 . . ?
Zn O30 H30A 113.4 . . ?
Zn O30 H30B 116.1 . . ?
H30A O30 H30B 100.0 . . ?
H31A O31 H31B 110.0 . . ?
H32A O32 H32B 121.5 . . ?
H33A O33 H33B 108.6 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn O1 1.976(2) 2 ?
Zn O28 2.038(3) . ?
Zn O27 2.057(2) . ?
Zn O29 2.094(2) . ?
Zn O30 2.151(2) . ?
O1 C3 1.280(4) . ?
O1 Zn 1.976(2) 2 ?
O2 C3 1.230(4) . ?
C3 C4 1.513(5) . ?
C4 C5 1.380(5) . ?
C4 C9 1.403(4) . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 O13 1.386(4) . ?
C6 C7 1.387(4) . ?
C7 C8 1.393(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.395(4) . ?
C8 C10 1.509(4) . ?
C9 H9 0.9500 . ?
C10 O11 1.259(4) . ?
C10 O12 1.260(4) . ?
O13 C14 1.412(4) . ?
C14 O15 1.410(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
O15 C16 1.398(4) . ?
C16 C21 1.375(4) . ?
C16 C17 1.392(4) . ?
C17 C18 1.398(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.407(5) . ?
C18 C25 1.498(4) . ?
C19 C20 1.383(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.391(5) . ?
C20 C22 1.515(5) . ?
C21 H21 0.9500 . ?
C22 O23 1.248(4) . ?
C22 O24 1.275(4) . ?
C25 O26 1.242(4) . ?
C25 O27 1.275(4) . ?
O28 H28A 0.9341 . ?
O28 H28B 0.9633 . ?
O29 H29A 0.9583 . ?
O29 H29B 0.8554 . ?
O30 H30A 0.9364 . ?
O30 H30B 0.9445 . ?
O31 H31A 0.9861 . ?
O31 H31B 1.0253 . ?
O32 H32A 0.9862 . ?
O32 H32B 0.9915 . ?
O33 H33A 0.9621 . ?
O33 H33B 1.0255 . ?
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
O28 H28A O23 0.93 1.85 2.712(3) 151 7_556
O28 H28B O30 0.96 2.43 3.098(4) 126 5_556
O29 H29A O11 0.96 1.79 2.722(3) 163 4
O29 H29B O24 0.86 1.92 2.754(3) 165 3_455
O30 H30A O12 0.94 1.82 2.724(3) 162 4_545
O30 H30B O24 0.94 1.86 2.805(3) 177 3_445
O31 H31A O23 0.99 1.80 2.781(3) 173 6_565
O31 H31B O12 1.03 1.97 2.803(3) 137 .
O32 H32A O27 0.99 2.07 2.954(4) 149 4_545
O32 H32B O12 0.99 1.98 2.918(4) 156 .
O33 H33A O11 0.96 1.88 2.808(4) 162 .
O33 H33B O26 1.03 1.90 2.844(4) 151 4
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 -0.030 0.250 191 54 ' '
2 1.000 0.009 0.250 191 54 ' '
3 0.500 0.000 0.750 191 54 ' '
4 1.000 -0.101 0.750 191 54 ' '
