#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:10:15 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180171 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/67/7106744.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_7106744
loop_
_publ_author_name
'Jiangtao Jia'
'Fuxing Sun'
'Qianrong Fang'
'Xiaoqiang Liang'
'Kun Cai'
'Zheng Bian'
'Huijun Zhao'
'Lianxun Gao'
'Guangshan Zhu'
_publ_section_title
;
 A novel low density metal-organic framework with pcu topology by
 dendritic ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              9167
_journal_paper_doi               10.1039/c1cc12891d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C66 H36 O13 Zn4'
_chemical_formula_sum            'C66 H36 O13 Zn4'
_chemical_formula_weight         1298.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :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            12
_cell_length_a                   20.4586(8)
_cell_length_b                   20.4586(8)
_cell_length_c                   80.370(3)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.51
_cell_volume                     29132.4(19)
_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      296(2)
_diffrn_detector_area_resol_mean 6.00cm
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -99
_diffrn_reflns_number            51924
_diffrn_reflns_theta_full        26.08
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7872
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.731
_refine_diff_density_min         -2.137
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6430
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0743
_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)+(0.1794P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2375
_reflns_number_gt                4997
_reflns_number_total             6430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12891d.txt
_cod_data_source_block           s1
_cod_original_cell_volume        29132(2)
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7106744
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
C1 C 0.3787(2) 0.5541(2) 0.05028(5) 0.0371(8) Uani 1 1 d . . .
C2 C 0.3964(2) 0.5053(2) 0.03923(5) 0.0409(9) Uani 1 1 d . . .
C3 C 0.3375(2) 0.4341(3) 0.03397(5) 0.0506(10) Uani 1 1 d . . .
H1 H 0.2887 0.4156 0.0379 0.061 Uiso 1 1 calc R . .
C4 C 0.3531(2) 0.3928(3) 0.02300(6) 0.0517(11) Uani 1 1 d . . .
H2 H 0.3138 0.3469 0.0192 0.062 Uiso 1 1 calc R . .
C5 C 0.4266(2) 0.4172(2) 0.01719(5) 0.0442(9) Uani 1 1 d . . .
C6 C 0.4833(2) 0.4856(2) 0.02321(6) 0.0489(10) Uani 1 1 d . . .
H4 H 0.5329 0.5028 0.0199 0.059 Uiso 1 1 calc R . .
C7 C 0.4681(3) 0.5288(2) 0.03391(6) 0.0504(10) Uani 1 1 d . . .
H3 H 0.5074 0.5749 0.0376 0.060 Uiso 1 1 calc R . .
C8 C 0.4410(2) 0.3707(2) 0.00525(5) 0.0413(9) Uani 1 1 d . . .
C9 C 0.5108(2) 0.3738(2) 0.00479(5) 0.0406(9) Uani 1 1 d . . .
H5 H 0.5484 0.4046 0.0123 0.049 Uiso 1 1 calc R . .
C10 C 0.5250(2) 0.3306(2) -0.00690(5) 0.0351(8) Uani 1 1 d . . .
C11 C 0.4690(2) 0.2867(2) -0.01832(5) 0.0412(9) Uani 1 1 d . . .
H7 H 0.4780 0.2585 -0.0261 0.049 Uiso 1 1 calc R . .
C12 C 0.3995(2) 0.2841(2) -0.01838(5) 0.0442(10) Uani 1 1 d . . .
C13 C 0.3869(2) 0.3269(3) -0.00643(5) 0.0478(10) Uani 1 1 d . . .
H6 H 0.3408 0.3257 -0.0064 0.057 Uiso 1 1 calc R . .
C14 C 0.3404(2) 0.2397(3) -0.03066(6) 0.0540(12) Uani 1 1 d . . .
C15 C 0.2656(3) 0.2031(4) -0.02667(7) 0.095(2) Uani 1 1 d U . .
H10 H 0.2520 0.2064 -0.0158 0.114 Uiso 1 1 calc R . .
C16 C 0.2090(4) 0.1613(4) -0.03801(8) 0.097(2) Uani 1 1 d U . .
H11 H 0.1587 0.1351 -0.0347 0.116 Uiso 1 1 calc R . .
C17 C 0.2297(3) 0.1596(4) -0.05469(7) 0.0747(16) Uani 1 1 d . . .
C18 C 0.3048(3) 0.1972(3) -0.05889(6) 0.0623(13) Uani 1 1 d . . .
H9 H 0.3188 0.1967 -0.0699 0.075 Uiso 1 1 calc R . .
C19 C 0.3595(3) 0.2352(3) -0.04720(6) 0.0573(12) Uani 1 1 d . . .
H8 H 0.4101 0.2583 -0.0503 0.069 Uiso 1 1 calc R . .
C20 C 0.5979(2) 0.3321(2) -0.00695(5) 0.0323(8) Uani 1 1 d . . .
C21 C 0.5995(2) 0.2646(2) -0.00682(5) 0.0333(8) Uani 1 1 d . . .
H12 H 0.5545 0.2186 -0.0067 0.040 Uiso 1 1 calc R . .
C22 C 0.2166(5) 0.4994(3) 0.09964(9) 0.096(2) Uani 1 1 d . . .
O1 O 0.31116(17) 0.53057(17) 0.05368(4) 0.0506(7) Uani 1 1 d . . .
O2 O 0.2096(2) 0.4822(2) 0.08433(5) 0.0696(10) Uani 1 1 d . . .
O3 O 0.3333 0.6667 0.07665(5) 0.0289(9) Uani 1 3 d S . .
O4 O 0.18151(17) 0.56685(17) 0.05526(4) 0.0512(8) Uani 1 1 d . . .
O5 O 0.2698(5) 0.5663(4) 0.10626(9) 0.167(3) Uani 1 1 d U . .
Zn1 Zn 0.26087(2) 0.56571(2) 0.069132(5) 0.0357(2) Uani 1 1 d . . .
Zn2 Zn 0.3333 0.6667 0.101809(14) 0.0813(4) Uani 1 3 d S . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O4 125.5(4) . 2_665 ?
O1 C1 C2 117.5(3) . . ?
O4 C1 C2 117.1(3) 2_665 . ?
C7 C2 C3 118.9(4) . . ?
C7 C2 C1 121.5(4) . . ?
C3 C2 C1 119.6(4) . . ?
C4 C3 C2 119.2(4) . . ?
C4 C3 H1 120.4 . . ?
C2 C3 H1 120.4 . . ?
C3 C4 C5 122.3(4) . . ?
C3 C4 H2 118.9 . . ?
C5 C4 H2 118.9 . . ?
C6 C5 C4 116.7(4) . . ?
C6 C5 C8 122.8(4) . . ?
C4 C5 C8 120.5(4) . . ?
C7 C6 C5 121.6(4) . . ?
C7 C6 H4 119.2 . . ?
C5 C6 H4 119.2 . . ?
C2 C7 C6 121.2(4) . . ?
C2 C7 H3 119.4 . . ?
C6 C7 H3 119.4 . . ?
C13 C8 C9 118.7(3) . . ?
C13 C8 C5 120.3(4) . . ?
C9 C8 C5 120.9(3) . . ?
C8 C9 C10 120.8(3) . . ?
C8 C9 H5 119.6 . . ?
C10 C9 H5 119.6 . . ?
C11 C10 C9 118.7(3) . . ?
C11 C10 C20 120.6(3) . . ?
C9 C10 C20 120.6(3) . . ?
C10 C11 C12 121.5(3) . . ?
C10 C11 H7 119.2 . . ?
C12 C11 H7 119.2 . . ?
C11 C12 C13 118.3(3) . . ?
C11 C12 C14 122.2(4) . . ?
C13 C12 C14 119.6(4) . . ?
C8 C13 C12 122.0(4) . . ?
C8 C13 H6 119.0 . . ?
C12 C13 H6 119.0 . . ?
C15 C14 C19 117.4(4) . . ?
C15 C14 C12 122.1(4) . . ?
C19 C14 C12 120.5(4) . . ?
C14 C15 C16 123.2(5) . . ?
C14 C15 H10 118.4 . . ?
C16 C15 H10 118.4 . . ?
C15 C16 C17 118.3(6) . . ?
C15 C16 H11 120.9 . . ?
C17 C16 H11 120.9 . . ?
C18 C17 C16 119.0(5) . . ?
C18 C17 C22 123.4(5) . 28 ?
C16 C17 C22 117.6(5) . 28 ?
C19 C18 C17 121.2(5) . . ?
C19 C18 H9 119.4 . . ?
C17 C18 H9 119.4 . . ?
C18 C19 C14 120.9(4) . . ?
C18 C19 H8 119.5 . . ?
C14 C19 H8 119.5 . . ?
C21 C20 C21 119.8(4) 3_665 . ?
C21 C20 C10 120.1(3) 3_665 . ?
C21 C20 C10 120.1(3) . . ?
C20 C21 C20 120.2(4) 2_655 . ?
C20 C21 H12 119.9 2_655 . ?
C20 C21 H12 119.9 . . ?
O2 C22 O5 125.5(5) . . ?
O2 C22 C17 117.9(6) . 34 ?
O5 C22 C17 115.5(6) . 34 ?
C1 O1 Zn1 132.9(3) . . ?
C22 O2 Zn1 115.7(4) . . ?
Zn1 O3 Zn1 110.78(11) 3_565 2_665 ?
Zn1 O3 Zn1 110.78(11) 3_565 . ?
Zn1 O3 Zn1 110.78(11) 2_665 . ?
Zn1 O3 Zn2 108.13(12) 3_565 . ?
Zn1 O3 Zn2 108.13(12) 2_665 . ?
Zn1 O3 Zn2 108.13(12) . . ?
C1 O4 Zn1 129.8(3) 3_565 . ?
C22 O5 Zn2 144.3(6) . . ?
O2 Zn1 O3 122.22(17) . . ?
O2 Zn1 O1 103.22(16) . . ?
O3 Zn1 O1 108.97(11) . . ?
O2 Zn1 O4 106.35(15) . . ?
O3 Zn1 O4 110.94(10) . . ?
O1 Zn1 O4 103.36(14) . . ?
O5 Zn2 O5 116.30(16) 2_665 . ?
O5 Zn2 O5 116.29(16) 2_665 3_565 ?
O5 Zn2 O5 116.29(16) . 3_565 ?
O5 Zn2 O3 101.2(2) 2_665 . ?
O5 Zn2 O3 101.2(2) . . ?
O5 Zn2 O3 101.2(2) 3_565 . ?
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
C1 O1 1.245(5) . ?
C1 O4 1.248(5) 2_665 ?
C1 C2 1.510(5) . ?
C2 C7 1.363(6) . ?
C2 C3 1.413(6) . ?
C3 C4 1.366(6) . ?
C3 H1 0.9300 . ?
C4 C5 1.406(6) . ?
C4 H2 0.9300 . ?
C5 C6 1.384(6) . ?
C5 C8 1.480(5) . ?
C6 C7 1.376(6) . ?
C6 H4 0.9300 . ?
C7 H3 0.9300 . ?
C8 C13 1.384(5) . ?
C8 C9 1.399(5) . ?
C9 C10 1.415(5) . ?
C9 H5 0.9300 . ?
C10 C11 1.391(5) . ?
C10 C20 1.476(5) . ?
C11 C12 1.396(5) . ?
C11 H7 0.9300 . ?
C12 C13 1.407(6) . ?
C12 C14 1.470(5) . ?
C13 H6 0.9300 . ?
C14 C15 1.364(7) . ?
C14 C19 1.401(6) . ?
C15 C16 1.383(8) . ?
C15 H10 0.9300 . ?
C16 C17 1.411(8) . ?
C16 H11 0.9300 . ?
C17 C18 1.374(8) . ?
C17 C22 1.504(7) 28 ?
C18 C19 1.367(6) . ?
C18 H9 0.9300 . ?
C19 H8 0.9300 . ?
C20 C21 1.387(5) 3_665 ?
C20 C21 1.398(5) . ?
C21 C20 1.387(5) 2_655 ?
C21 H12 0.9300 . ?
C22 O2 1.268(8) . ?
C22 O5 1.361(10) . ?
C22 C17 1.504(7) 34 ?
O1 Zn1 1.964(3) . ?
O2 Zn1 1.928(3) . ?
O3 Zn1 1.9407(14) 3_565 ?
O3 Zn1 1.9408(14) 2_665 ?
O3 Zn1 1.9408(14) . ?
O3 Zn2 2.022(4) . ?
O4 C1 1.248(5) 3_565 ?
O4 Zn1 1.979(3) . ?
O5 Zn2 1.834(6) . ?
Zn2 O5 1.834(6) 2_665 ?
Zn2 O5 1.834(6) 3_565 ?
