#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:04:51 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179555 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/24/4502422.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_4502422
loop_
_publ_author_name
'Jiang, Hai-Long'
'Liu, Bo'
'Xu, Qiang'
_publ_section_title
;
 Rational Assembly of d10Metal−Organic Frameworks with Helical
 Nanochannels Based on Flexible V-Shaped Ligand
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              806
_journal_paper_doi               10.1021/cg901181x
_journal_volume                  10
_journal_year                    2010
_chemical_formula_sum            'C34 H16 F12 O9 Zn2'
_chemical_formula_weight         927.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           180
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 62 2 (0 0 4)'
_symmetry_space_group_name_H-M   'P 62 2 2'
_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            3
_cell_length_a                   21.250(3)
_cell_length_b                   21.250(3)
_cell_length_c                   7.7200(15)
_cell_measurement_temperature    293(2)
_cell_volume                     3019.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1082
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            28897
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    1.295
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7513
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1050P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                1635
_reflns_number_total             2294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg901181x_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P6222
_cod_database_code               4502422
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/3'
'-y, x-y, z+2/3'
'-x, -y, z'
'-x+y, -x, z+1/3'
'y, -x+y, z+2/3'
'-y, -x, -z+2/3'
'x-y, -y, -z'
'x, x-y, -z+1/3'
'y, x, -z+2/3'
'-x+y, y, -z'
'-x, -x+y, -z+1/3'
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
Zn1 Zn 0.40194(5) 0.70097(3) 0.1667 0.0476(3) Uani 1 2 d S
F1 F 0.2535(3) 0.1559(2) -0.1225(11) 0.146(3) Uani 1 1 d .
F2 F 0.3023(4) 0.2308(3) 0.0879(9) 0.121(2) Uani 1 1 d .
F3 F 0.1899(3) 0.1870(2) 0.0303(10) 0.148(3) Uani 1 1 d .
O1 O 0.3624(3) 0.6013(2) 0.0927(6) 0.0692(12) Uani 1 1 d .
O2 O 0.2934(2) 0.5356(2) 0.3143(6) 0.0720(12) Uani 1 1 d .
C1 C 0.3230(3) 0.5426(3) 0.1717(8) 0.0576(13) Uani 1 1 d .
C2 C 0.3107(3) 0.4735(3) 0.0846(7) 0.0532(13) Uani 1 1 d .
C3 C 0.2727(4) 0.4092(3) 0.1665(9) 0.0681(16) Uani 1 1 d .
H3A H 0.2536 0.4079 0.2756 0.082 Uiso 1 1 calc R
C4 C 0.2612(4) 0.3445(4) 0.0923(11) 0.077(2) Uani 1 1 d .
H4A H 0.2360 0.3010 0.1529 0.092 Uiso 1 1 calc R
C5 C 0.3371(3) 0.4754(3) -0.0813(9) 0.0612(15) Uani 1 1 d .
H5A H 0.3624 0.5192 -0.1408 0.073 Uiso 1 1 calc R
C6 C 0.3252(3) 0.4112(3) -0.1566(9) 0.0626(15) Uani 1 1 d .
H6A H 0.3431 0.4127 -0.2674 0.075 Uiso 1 1 calc R
C7 C 0.2880(3) 0.3453(3) -0.0738(9) 0.0595(15) Uani 1 1 d .
C8 C 0.2769(4) 0.2769(4) -0.1667 0.069(3) Uani 1 2 d S
C9 C 0.2553(5) 0.2125(4) -0.0411(16) 0.103(4) Uani 1 1 d .
O1W O 0.5000 0.5000 0.3333 0.162(6) Uiso 1 4 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'
F F 0.0171 0.0103 '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
O2 Zn1 O2 106.3(3) 7_665 3_664
O2 Zn1 O1 101.4(2) 7_665 .
O2 Zn1 O1 104.70(19) 3_664 .
O2 Zn1 O1 104.70(19) 7_665 9_565
O2 Zn1 O1 101.4(2) 3_664 9_565
O1 Zn1 O1 135.7(3) . 9_565
C1 O1 Zn1 130.7(4) . .
C1 O2 Zn1 136.8(4) . 5_565
O2 C1 O1 126.5(5) . .
O2 C1 C2 116.6(5) . .
O1 C1 C2 117.0(5) . .
C3 C2 C5 119.3(6) . .
C3 C2 C1 120.1(5) . .
C5 C2 C1 120.6(6) . .
C2 C3 C4 121.9(6) . .
C2 C3 H3A 119.0 . .
C4 C3 H3A 119.0 . .
C3 C4 C7 119.7(7) . .
C3 C4 H4A 120.2 . .
C7 C4 H4A 120.2 . .
C6 C5 C2 119.0(6) . .
C6 C5 H5A 120.5 . .
C2 C5 H5A 120.5 . .
C7 C6 C5 122.5(6) . .
C7 C6 H6A 118.8 . .
C5 C6 H6A 118.8 . .
C6 C7 C4 117.6(6) . .
C6 C7 C8 119.1(5) . .
C4 C7 C8 123.3(6) . .
C7 C8 C7 112.9(7) . 10_554
C7 C8 C9 105.6(4) . 10_554
C7 C8 C9 112.5(4) 10_554 10_554
C7 C8 C9 112.5(4) . .
C7 C8 C9 105.6(4) 10_554 .
C9 C8 C9 107.7(10) 10_554 .
F2 C9 F3 106.8(9) . .
F2 C9 F1 107.0(8) . .
F3 C9 F1 105.8(6) . .
F2 C9 C8 111.5(6) . .
F3 C9 C8 114.0(8) . .
F1 C9 C8 111.2(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 1.916(4) 7_665
Zn1 O2 1.916(4) 3_664
Zn1 O1 1.933(4) .
Zn1 O1 1.933(4) 9_565
F1 C9 1.342(8) .
F2 C9 1.325(12) .
F3 C9 1.332(9) .
O1 C1 1.259(7) .
O2 C1 1.240(7) .
O2 Zn1 1.916(4) 5_565
C1 C2 1.513(7) .
C2 C3 1.348(9) .
C2 C5 1.391(8) .
C3 C4 1.394(9) .
C3 H3A 0.9300 .
C4 C7 1.399(9) .
C4 H4A 0.9300 .
C5 C6 1.386(8) .
C5 H5A 0.9300 .
C6 C7 1.374(8) .
C6 H6A 0.9300 .
C7 C8 1.530(7) .
C8 C7 1.530(7) 10_554
C8 C9 1.546(11) 10_554
C8 C9 1.546(11) .
