#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:29:14 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179581 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/46/4504639.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_4504639
loop_
_publ_author_name
'Wang, Jing'
'Zheng, Ling-Ling'
'Li, Cui-Jin'
'Zheng, Yan-Zhen'
'Tong, Ming-Liang'
_publ_section_title
;
 Coexistence of Planar and Chair-Shaped Cyclic Water Hexamers in a Unique
 Cyclohexanehexacarboxylate-Bridged Metal−Organic Framework
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              357
_journal_paper_doi               10.1021/cg050388f
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C12 H18 Co3 O18'
_chemical_formula_weight         627.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.3139(10)
_cell_length_b                   14.3139(10)
_cell_length_c                   14.6728(16)
_cell_measurement_temperature    123(2)
_cell_volume                     2603.5(4)
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_collection       'SMART, 1998.'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3966
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.942
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1890
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00036(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1254
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0309
_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)+(0.0370P)²+13.1497P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                1214
_reflns_number_total             1254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050388fsi20050807_063751.cif
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4504639
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Co1 Co 0.32029(2) 0.05280(2) 0.89186(2) 0.00758(16) Uani 1 1 d .
O1W O 0.20433(15) 0.01359(15) 0.99735(13) 0.0138(4) Uani 1 1 d D
H1WA H 0.244(2) 0.027(3) 1.0440(16) 0.034(10) Uiso 1 1 d D
H1WB H 0.1481(19) -0.0478(17) 1.002(3) 0.046(12) Uiso 1 1 d D
O2W O 0.45084(14) 0.13826(14) 0.80098(12) 0.0126(4) Uani 1 1 d D
H2WA H 0.434(3) 0.118(3) 0.7464(11) 0.032(10) Uiso 1 1 d D
H2WB H 0.501(2) 0.128(3) 0.818(2) 0.038(11) Uiso 1 1 d D
O1 O 0.35700(14) -0.05844(13) 0.94657(12) 0.0109(4) Uani 1 1 d .
O2 O 0.44493(14) -0.06924(14) 0.82591(13) 0.0113(4) Uani 1 1 d .
O3 O 0.57193(14) -0.16963(14) 1.01858(12) 0.0118(4) Uani 1 1 d .
O4 O 0.62644(13) -0.09387(14) 0.88194(13) 0.0125(4) Uani 1 1 d .
C1 C 0.36512(18) -0.21958(18) 0.93006(17) 0.0079(5) Uani 1 1 d .
H1 H 0.3649 -0.2204 0.9969 0.010 Uiso 1 1 calc R
C2 C 0.44837(18) -0.25020(18) 0.89632(17) 0.0092(5) Uani 1 1 d .
H2 H 0.4509 -0.2483 0.8296 0.011 Uiso 1 1 calc R
C3 C 0.39324(18) -0.10648(18) 0.89819(17) 0.0079(5) Uani 1 1 d .
C4 C 0.55803(19) -0.16533(18) 0.93481(17) 0.0095(5) Uani 1 1 d .
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'
Co Co 0.3494 0.9721 '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 Co1 O3 90.11(7) . 10_657
O1 Co1 O4 89.53(7) . 17_556
O3 Co1 O4 168.32(7) 10_657 17_556
O1 Co1 O2 173.19(7) . 17_556
O3 Co1 O2 93.53(7) 10_657 17_556
O4 Co1 O2 88.07(7) 17_556 17_556
O1 Co1 O2W 101.44(7) . .
O3 Co1 O2W 81.24(7) 10_657 .
O4 Co1 O2W 87.39(7) 17_556 .
O2 Co1 O2W 84.81(7) 17_556 .
O1 Co1 O1W 88.83(7) . .
O3 Co1 O1W 85.39(7) 10_657 .
O4 Co1 O1W 106.27(7) 17_556 .
O2 Co1 O1W 85.74(7) 17_556 .
O2W Co1 O1W 163.10(7) . .
Co1 O1W H1WA 100(3) . .
Co1 O1W H1WB 123(3) . .
H1WA O1W H1WB 110.2(17) . .
Co1 O2W H2WA 112(3) . .
Co1 O2W H2WB 107(3) . .
H2WA O2W H2WB 110.0(17) . .
C3 O1 Co1 122.04(15) . .
C3 O2 Co1 139.19(16) . 18_546
C4 O3 Co1 130.80(16) . 10_657
C4 O4 Co1 128.96(15) . 18_546
C3 C1 C2 111.71(19) . .
C3 C1 C2 108.68(19) . 2_545
C2 C1 C2 111.2(2) . 2_545
C3 C1 H1 108.4 . .
C2 C1 H1 108.4 . .
C2 C1 H1 108.4 2_545 .
C4 C2 C1 106.67(19) . .
C4 C2 C1 111.83(19) . 3_655
C1 C2 C1 109.3(2) . 3_655
C4 C2 H2 109.7 . .
C1 C2 H2 109.7 . .
C1 C2 H2 109.7 3_655 .
O2 C3 O1 124.1(2) . .
O2 C3 C1 119.8(2) . .
O1 C3 C1 116.1(2) . .
O3 C4 O4 124.3(2) . .
O3 C4 C2 116.6(2) . .
O4 C4 C2 119.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.0718(17) .
Co1 O3 2.0793(18) 10_657
Co1 O4 2.0900(18) 17_556
Co1 O2 2.0960(17) 17_556
Co1 O2W 2.1167(18) .
Co1 O1W 2.1294(19) .
O1W H1WA 0.851(10) .
O1W H1WB 0.847(10) .
O2W H2WA 0.846(10) .
O2W H2WB 0.844(10) .
O1 C3 1.266(3) .
O2 C3 1.250(3) .
O2 Co1 2.0961(17) 18_546
O3 C4 1.252(3) .
O3 Co1 2.0793(18) 10_657
O4 C4 1.267(3) .
O4 Co1 2.0899(18) 18_546
C1 C3 1.533(3) .
C1 C2 1.543(3) .
C1 C2 1.548(3) 2_545
C1 H1 0.9800 .
C2 C4 1.534(3) .
C2 C1 1.548(3) 3_655
C2 H2 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 O4 0.851(10) 1.936(15) 2.746(3) 159(3) 10_657
O1W H1WB O1W 0.847(10) 1.989(10) 2.8335(18) 175(3) 11_557
O2W H2WA O1 0.846(10) 2.033(11) 2.876(3) 174(3) 8_544
O2W H2WB O2W 0.844(10) 2.259(10) 3.101(2) 174(4) 18_546
