#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/48/2224829.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_2224829
loop_
_publ_author_name
'Chen, Jin-Xi'
'Meng, Wei-Wei'
_publ_section_title
Poly[tetrakis(μ-cyclohexane-1,4-dicarboxylato)di-μ-hydroxido-pentazinc(II)]
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m16
_journal_page_last               m17
_journal_paper_doi               10.1107/S1600536809051666
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Zn5 (O H)2 (C8 H10 O4)4]'
_chemical_formula_moiety         'C32 H42 O18 Zn5'
_chemical_formula_sum            'C32 H42 O18 Zn5'
_chemical_formula_weight         1039.59
_chemical_name_common
Poly[di[(μ3-hydroxido)tetrakis(cyclohexane-1,4-dicarboxylato)-pentazinc(II)]
_chemical_name_systematic
;
Poly[tetrakis(μ-cyclohexane-1,4-dicarboxylato)di-μ-hydroxido-pentazinc(II)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                113.915(3)
_cell_angle_beta                 96.307(3)
_cell_angle_gamma                106.285(3)
_cell_formula_units_Z            1
_cell_length_a                   8.646(3)
_cell_length_b                   10.665(3)
_cell_length_c                   11.804(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     923.6(5)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       '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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3929
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.278
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.504
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0378
_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)+(0.0488P)²+2.2254P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                2789
_reflns_number_total             3202
_reflns_threshold_expression     'I>2σ(I) '
_cod_data_source_file            zs2020.cif
_cod_data_source_block           I
_cod_database_code               2224829
_cod_database_fobs_code          2224829
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_disorder_assembly
_atom_site_disorder_group
Zn Zn1 0.5000 0.5000 0.5000 0.01886(17) Uani d S 1 . .
Zn Zn2 0.23318(6) 0.53614(5) 0.33384(4) 0.02004(14) Uani d . 1 . .
Zn Zn3 0.22931(6) 0.63639(5) 0.63471(4) 0.02095(15) Uani d . 1 . .
O O1 0.2545(3) 0.4858(3) 0.4786(2) 0.0165(6) Uani d . 1 . .
O O2 0.4649(3) 0.5325(3) 0.3351(3) 0.0227(6) Uani d . 1 . .
O O3 -0.0494(4) 0.3940(3) 0.2794(3) 0.0260(7) Uani d . 1 . .
O O4 0.0760(4) 0.7048(3) 0.5332(3) 0.0292(7) Uani d . 1 . .
O O5 0.2146(4) 0.7268(3) 0.3889(3) 0.0329(8) Uani d . 1 . .
O O6 0.4102(4) 0.2695(3) 0.3800(3) 0.0333(8) Uani d . 1 . .
O O7 0.1035(4) 0.4072(4) 0.1489(3) 0.0354(8) Uani d . 1 . .
O O8 0.5888(4) 0.1755(3) 0.2861(3) 0.0367(8) Uani d . 1 . .
O O9 0.6515(4) 0.4466(4) 0.2502(3) 0.0391(9) Uani d . 1 . .
C C1 -0.0356(5) 0.3514(5) 0.1658(4) 0.0216(9) Uani d . 1 . .
C C2 0.4892(6) 0.5179(5) 0.1295(4) 0.0244(9) Uani d . 1 . .
H H2 0.4089 0.5681 0.1453 0.029 Uiso calc R 1 . .
C C3 0.5402(5) 0.4959(5) 0.2450(4) 0.0210(9) Uani d . 1 . .
C C4 -0.1756(5) 0.2307(5) 0.0558(4) 0.0239(9) Uani d . 1 . .
H H4 -0.2808 0.2294 0.0799 0.029 Uiso calc R 1 . .
C C5 0.4451(6) 0.1700(5) 0.2982(4) 0.0266(10) Uani d . 1 . .
C C6 0.3284(6) -0.1108(5) 0.1772(4) 0.0340(11) Uani d . 1 . .
H H6A 0.3326 -0.1206 0.2556 0.041 Uiso calc R 1 . .
H H6B 0.4337 -0.1087 0.1553 0.041 Uiso calc R 1 . .
C C7 0.4060(6) 0.3693(5) 0.0104(4) 0.0293(10) Uani d . 1 . .
H H7A 0.4817 0.3156 -0.0022 0.035 Uiso calc R 1 . .
H H7B 0.3068 0.3126 0.0236 0.035 Uiso calc R 1 . .
C C8 0.3027(5) 0.0317(5) 0.1984(4) 0.0274(10) Uani d . 1 . .
H H8 0.1995 0.0306 0.2258 0.033 Uiso calc R 1 . .
C C9 0.6414(6) 0.6136(5) 0.1087(4) 0.0330(11) Uani d . 1 . .
H H9A 0.6883 0.7096 0.1827 0.040 Uiso calc R 1 . .
H H9B 0.7258 0.5689 0.1000 0.040 Uiso calc R 1 . .
C C10 -0.1861(6) 0.2424(5) -0.0691(4) 0.0330(11) Uani d . 1 . .
H H10A -0.0815 0.2467 -0.0928 0.040 Uiso calc R 1 . .
H H10B -0.2041 0.3323 -0.0568 0.040 Uiso calc R 1 . .
C C11 0.1180(6) 0.7593(5) 0.4592(4) 0.0281(10) Uani d . 1 . .
C C12 0.0494(7) 0.8716(6) 0.4494(6) 0.0441(13) Uani d . 1 . .
H H12 0.0263 0.8499 0.3590 0.053 Uiso calc R 1 . .
C C13 -0.1518(7) 0.0883(5) 0.0363(5) 0.0425(13) Uani d . 1 . .
H H13A -0.1540 0.0779 0.1141 0.051 Uiso calc R 1 . .
H H13B -0.0434 0.0922 0.0200 0.051 Uiso calc R 1 . .
C C14 0.2867(7) 0.0456(5) 0.0755(5) 0.0396(12) Uani d . 1 . .
H H14A 0.3928 0.0582 0.0533 0.047 Uiso calc R 1 . .
H H14B 0.2606 0.1326 0.0894 0.047 Uiso calc R 1 . .
C C15 0.1774(7) 1.0209(7) 0.5214(7) 0.0554(16) Uani d . 1 . .
H H15A 0.2750 1.0237 0.4876 0.066 Uiso calc R 1 . .
H H15B 0.2105 1.0432 0.6107 0.066 Uiso calc R 1 . .
C C16 -0.1133(7) 0.8624(6) 0.4875(7) 0.0518(15) Uani d . 1 . .
H H16A -0.0976 0.8752 0.5746 0.062 Uiso calc R 1 . .
H H16B -0.1962 0.7657 0.4319 0.062 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'
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
_geom_angle_publ_flag
O1 Zn1 O2 . . 80.38(10) ?
O1 Zn1 O6 . . 87.49(11) ?
O2 Zn1 O6 . . 89.32(12) ?
O1 Zn1 O6 . 2_666 92.51(11) ?
O2 Zn1 O6 . 2_666 90.68(12) ?
O6 Zn1 O6 . 2_666 180.00(12) ?
O1 Zn1 Zn2 . 2_666 140.05(7) ?
O2 Zn1 Zn2 . 2_666 139.33(8) ?
O6 Zn1 Zn2 . 2_666 88.74(9) ?
O5 Zn2 O1 . . 111.19(13) ?
O5 Zn2 O2 . . 115.65(13) ?
O1 Zn2 O2 . . 84.68(11) ?
O5 Zn2 O7 . . 108.81(15) ?
O1 Zn2 O7 . . 129.58(13) ?
O2 Zn2 O7 . . 104.36(12) ?
O5 Zn2 O3 . . 98.81(13) ?
O1 Zn2 O3 . . 85.57(11) ?
O2 Zn2 O3 . . 145.41(12) ?
O7 Zn2 O3 . . 58.86(11) ?
O8 Zn3 O3 2_666 2_566 118.92(13) ?
O8 Zn3 O1 2_666 . 114.91(13) ?
O3 Zn3 O1 2_566 . 125.97(12) ?
O8 Zn3 O4 2_666 . 93.78(14) ?
O3 Zn3 O4 2_566 . 86.00(12) ?
O1 Zn3 O4 . . 94.98(11) ?
O8 Zn3 O9 2_666 2_666 92.49(15) ?
O3 Zn3 O9 2_566 2_666 84.37(13) ?
O1 Zn3 O9 . 2_666 89.19(12) ?
O4 Zn3 O9 . 2_666 170.20(13) ?
Zn3 O1 Zn2 . . 111.16(13) ?
Zn3 O1 Zn1 . . 110.07(12) ?
Zn2 O1 Zn1 . . 98.36(11) ?
C3 O2 Zn2 . . 132.3(3) ?
C3 O2 Zn1 . . 125.5(3) ?
Zn2 O2 Zn1 . . 96.09(11) ?
C1 O3 Zn3 . 2_566 137.0(3) ?
C1 O3 Zn2 . . 84.3(2) ?
Zn3 O3 Zn2 2_566 . 138.63(14) ?
C11 O4 Zn3 . . 125.9(3) ?
C11 O5 Zn2 . . 118.8(3) ?
C5 O6 Zn1 . . 142.7(3) ?
C1 O7 Zn2 . . 99.0(3) ?
C5 O8 Zn3 . 2_666 119.7(3) ?
C3 O9 Zn3 . 2_666 140.7(3) ?
O7 C1 O3 . . 117.8(4) ?
O7 C1 C4 . . 121.1(4) ?
O3 C1 C4 . . 121.0(4) ?
C3 C2 C7 . . 110.1(3) ?
C3 C2 C9 . . 110.3(4) ?
C7 C2 C9 . . 110.4(4) ?
C3 C2 H2 . . 108.6 ?
C7 C2 H2 . . 108.6 ?
C9 C2 H2 . . 108.6 ?
O9 C3 O2 . . 122.9(4) ?
O9 C3 C2 . . 119.3(4) ?
O2 C3 C2 . . 117.8(4) ?
C1 C4 C13 . . 106.4(4) ?
C1 C4 C10 . . 115.0(4) ?
C13 C4 C10 . . 109.7(4) ?
C1 C4 H4 . . 108.5 ?
C13 C4 H4 . . 108.5 ?
C10 C4 H4 . . 108.5 ?
O6 C5 O8 . . 125.7(4) ?
O6 C5 C8 . . 118.6(4) ?
O8 C5 C8 . . 115.7(4) ?
C8 C6 C10 . 2 110.4(4) ?
C8 C6 H6A . . 109.6 ?
C10 C6 H6A 2 . 109.6 ?
C8 C6 H6B . . 109.6 ?
C10 C6 H6B 2 . 109.6 ?
H6A C6 H6B . . 108.1 ?
C9 C7 C2 2_665 . 111.9(4) ?
C9 C7 H7A 2_665 . 109.2 ?
C2 C7 H7A . . 109.2 ?
C9 C7 H7B 2_665 . 109.2 ?
C2 C7 H7B . . 109.2 ?
H7A C7 H7B . . 107.9 ?
C14 C8 C6 . . 110.5(4) ?
C14 C8 C5 . . 106.2(4) ?
C6 C8 C5 . . 114.1(4) ?
C14 C8 H8 . . 108.6 ?
C6 C8 H8 . . 108.6 ?
C5 C8 H8 . . 108.6 ?
C7 C9 C2 2_665 . 111.0(4) ?
C7 C9 H9A 2_665 . 109.4 ?
C2 C9 H9A . . 109.4 ?
C7 C9 H9B 2_665 . 109.4 ?
C2 C9 H9B . . 109.4 ?
H9A C9 H9B . . 108.0 ?
C4 C10 C6 . 2 111.1(4) ?
C4 C10 H10A . . 109.4 ?
C6 C10 H10A 2 . 109.4 ?
C4 C10 H10B . . 109.4 ?
C6 C10 H10B 2 . 109.4 ?
H10A C10 H10B . . 108.0 ?
O5 C11 O4 . . 124.9(4) ?
O5 C11 C12 . . 115.1(4) ?
O4 C11 C12 . . 120.0(4) ?
C15 C12 C16 . . 112.4(5) ?
C15 C12 C11 . . 110.3(5) ?
C16 C12 C11 . . 113.4(4) ?
C15 C12 H12 . . 106.8 ?
C16 C12 H12 . . 106.8 ?
C11 C12 H12 . . 106.8 ?
C4 C13 C14 . 2 112.1(4) ?
C4 C13 H13A . . 109.2 ?
C14 C13 H13A 2 . 109.2 ?
C4 C13 H13B . . 109.2 ?
C14 C13 H13B 2 . 109.2 ?
H13A C13 H13B . . 107.9 ?
C8 C14 C13 . 2 112.6(4) ?
C8 C14 H14A . . 109.1 ?
C13 C14 H14A 2 . 109.1 ?
C8 C14 H14B . . 109.1 ?
C13 C14 H14B 2 . 109.1 ?
H14A C14 H14B . . 107.8 ?
C12 C15 C16 . 2_576 111.8(5) ?
C12 C15 H15A . . 109.2 ?
C16 C15 H15A 2_576 . 109.2 ?
C12 C15 H15B . . 109.2 ?
C16 C15 H15B 2_576 . 109.2 ?
H15A C15 H15B . . 107.9 ?
C12 C16 C15 . 2_576 112.0(5) ?
C12 C16 H16A . . 109.2 ?
C15 C16 H16A 2_576 . 109.2 ?
C12 C16 H16B . . 109.2 ?
C15 C16 H16B 2_576 . 109.2 ?
H16A C16 H16B . . 107.9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 O1 . 2.065(3) ?
Zn1 O1 2_666 2.065(3) ?
Zn1 O2 2_666 2.116(3) ?
Zn1 O2 . 2.116(3) ?
Zn1 O6 . 2.125(3) ?
Zn1 O6 2_666 2.125(3) ?
Zn2 O5 . 1.928(3) ?
Zn2 O1 . 1.993(3) ?
Zn2 O2 . 2.013(3) ?
Zn2 O7 . 2.019(3) ?
Zn2 O3 . 2.338(3) ?
Zn3 O8 2_666 1.939(3) ?
Zn3 O3 2_566 1.971(3) ?
Zn3 O1 . 1.977(3) ?
Zn3 O4 . 2.151(3) ?
Zn3 O9 2_666 2.207(3) ?
O2 C3 . 1.290(5) ?
O3 C1 . 1.261(5) ?
O4 C11 . 1.263(5) ?
O5 C11 . 1.260(5) ?
O6 C5 . 1.250(5) ?
O7 C1 . 1.261(5) ?
O8 C5 . 1.254(5) ?
O9 C3 . 1.226(5) ?
C1 C4 . 1.495(6) ?
C2 C3 . 1.514(5) ?
C2 C7 . 1.529(6) ?
C2 C9 . 1.535(6) ?
C2 H2 . 0.9800 ?
C4 C13 . 1.518(6) ?
C4 C10 . 1.524(6) ?
C4 H4 . 0.9800 ?
C5 C8 . 1.528(6) ?
C6 C8 . 1.521(6) ?
C6 C10 2 1.532(6) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 C9 2_665 1.517(6) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 C14 . 1.513(7) ?
C8 H8 . 0.9800 ?
C9 C7 2_665 1.517(6) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C10 C6 2 1.532(6) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 C12 . 1.516(6) ?
C12 C15 . 1.480(8) ?
C12 C16 . 1.513(8) ?
C12 H12 . 0.9800 ?
C13 C14 2 1.530(6) ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C14 C13 2 1.530(6) ?
C14 H14A . 0.9700 ?
C14 H14B . 0.9700 ?
C15 C16 2_576 1.532(7) ?
C15 H15A . 0.9700 ?
C15 H15B . 0.9700 ?
C16 C15 2_576 1.532(7) ?
C16 H16A . 0.9700 ?
C16 H16B . 0.9700 ?
