#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:04:51 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179555 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/24/4502424.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_4502424
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            'C30 H24 F6 N3 O5 Zn'
_chemical_formula_weight         685.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.080(3)
_cell_length_b                   9.7100(19)
_cell_length_c                   25.530(8)
_cell_measurement_temperature    293(2)
_cell_volume                     3128.2(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            29253
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7347
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7105
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0971P)²+1.2742P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1516
_reflns_number_gt                5602
_reflns_number_total             7105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg901181x_si_004.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4502424
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Zn1 Zn 0.55224(2) -0.13658(3) -0.498908(11) 0.03260(12) Uani 1 1 d .
F1 F 0.0109(2) -0.4207(3) -0.39595(8) 0.0866(8) Uani 1 1 d .
F2 F -0.01563(18) -0.5033(3) -0.32287(9) 0.0818(7) Uani 1 1 d .
F3 F 0.1249(2) -0.5571(2) -0.34600(9) 0.0721(6) Uani 1 1 d .
F4 F -0.0099(2) -0.2767(3) -0.26472(10) 0.0887(8) Uani 1 1 d .
F5 F 0.0757(2) -0.1065(3) -0.28461(10) 0.0786(7) Uani 1 1 d .
F6 F -0.04503(18) -0.2027(3) -0.34687(10) 0.0890(8) Uani 1 1 d .
O1 O 0.43571(18) -0.1907(2) -0.46399(9) 0.0526(5) Uani 1 1 d .
O2 O 0.35870(19) 0.0150(2) -0.46534(9) 0.0536(5) Uani 1 1 d .
O3 O 0.3749(2) -0.5481(2) -0.07413(9) 0.0594(6) Uani 1 1 d .
O4 O 0.4496(2) -0.3411(2) -0.07399(8) 0.0553(6) Uani 1 1 d .
N1 N 0.9876(4) -0.8843(4) -0.4350(2) 0.1159(19) Uani 1 1 d .
H1A H 1.0292 -0.9544 -0.4282 0.139 Uiso 1 1 calc R
N2 N 0.64045(19) -0.3127(2) -0.48987(9) 0.0391(5) Uani 1 1 d .
C1 C 0.3716(2) -0.1094(3) -0.45178(11) 0.0399(6) Uani 1 1 d .
C2 C 0.3054(2) -0.1641(3) -0.41663(11) 0.0373(6) Uani 1 1 d .
C3 C 0.3331(2) -0.2850(3) -0.38763(12) 0.0454(7) Uani 1 1 d .
H3A H 0.3924 -0.3340 -0.3907 0.054 Uiso 1 1 calc R
C4 C 0.2735(2) -0.3336(3) -0.35414(12) 0.0441(6) Uani 1 1 d .
H4A H 0.2942 -0.4135 -0.3341 0.053 Uiso 1 1 calc R
C5 C 0.2161(2) -0.0943(3) -0.41203(12) 0.0448(6) Uani 1 1 d .
H5A H 0.1973 -0.0121 -0.4308 0.054 Uiso 1 1 calc R
C6 C 0.1539(2) -0.1447(3) -0.37994(12) 0.0445(7) Uani 1 1 d .
H6A H 0.0926 -0.0981 -0.3785 0.053 Uiso 1 1 calc R
C7 C 0.1827(2) -0.2639(3) -0.35017(10) 0.0381(6) Uani 1 1 d .
C8 C 0.1185(2) -0.3276(3) -0.31358(11) 0.0431(6) Uani 1 1 d .
C9 C 0.0594(3) -0.4530(4) -0.34412(13) 0.0586(9) Uani 1 1 d .
C10 C 0.0343(3) -0.2264(5) -0.30238(15) 0.0649(10) Uani 1 1 d .
C11 C 0.1917(2) -0.3647(3) -0.25747(11) 0.0390(6) Uani 1 1 d .
C12 C 0.2690(3) -0.2710(3) -0.23273(11) 0.0467(7) Uani 1 1 d .
H12A H 0.2786 -0.1918 -0.2514 0.056 Uiso 1 1 calc R
C13 C 0.3323(3) -0.2931(3) -0.18089(12) 0.0484(7) Uani 1 1 d .
H13A H 0.3829 -0.2279 -0.1647 0.058 Uiso 1 1 calc R
C14 C 0.1800(3) -0.4841(3) -0.22915(12) 0.0488(7) Uani 1 1 d .
H14A H 0.1286 -0.5485 -0.2451 0.059 Uiso 1 1 calc R
C15 C 0.2445(3) -0.5071(3) -0.17759(12) 0.0484(7) Uani 1 1 d .
H15A H 0.2366 -0.5878 -0.1594 0.058 Uiso 1 1 calc R
C16 C 0.3207(2) -0.4122(3) -0.15256(10) 0.0402(6) Uani 1 1 d .
C17 C 0.3872(2) -0.4358(3) -0.09576(11) 0.0435(6) Uani 1 1 d .
C21 C 0.9849(4) -0.8018(5) -0.4754(2) 0.0805(12) Uani 1 1 d .
H21A H 1.0313 -0.8192 -0.4966 0.097 Uiso 1 1 calc R
C22 C 0.9176(3) -0.6898(4) -0.48887(16) 0.0665(10) Uani 1 1 d .
H22A H 0.9202 -0.6340 -0.5181 0.080 Uiso 1 1 calc R
C23 C 0.9226(6) -0.8537(6) -0.4051(4) 0.162(4) Uani 1 1 d .
H23A H 0.9250 -0.9081 -0.3749 0.195 Uiso 1 1 calc R
C24 C 0.8512(5) -0.7462(5) -0.4158(3) 0.125(3) Uani 1 1 d .
H24A H 0.8061 -0.7317 -0.3937 0.150 Uiso 1 1 calc R
C25 C 0.8469(3) -0.6613(3) -0.45890(15) 0.0501(7) Uani 1 1 d .
C26 C 0.7742(2) -0.5418(3) -0.47039(12) 0.0432(6) Uani 1 1 d .
C27 C 0.6899(4) -0.5295(4) -0.4488(2) 0.0888(16) Uani 1 1 d .
H27A H 0.6762 -0.5989 -0.4265 0.107 Uiso 1 1 calc R
C28 C 0.6243(4) -0.4152(4) -0.4595(2) 0.0840(15) Uani 1 1 d .
H28A H 0.5667 -0.4109 -0.4447 0.101 Uiso 1 1 calc R
C29 C 0.7874(4) -0.4367(4) -0.5033(2) 0.0834(14) Uani 1 1 d .
H29A H 0.8431 -0.4396 -0.5197 0.100 Uiso 1 1 calc R
C30 C 0.7193(4) -0.3265(4) -0.5125(2) 0.0829(15) Uani 1 1 d .
H30A H 0.7295 -0.2577 -0.5360 0.099 Uiso 1 1 calc R
O5 O 0.4888(11) -0.0255(12) -0.2119(7) 0.369(7) Uani 1 1 d U
C33 C 0.4512(12) 0.0262(14) -0.2666(7) 0.221(4) Uani 1 1 d U
H33A H 0.4728 -0.0027 -0.2968 0.265 Uiso 1 1 calc R
N3 N 0.3853(12) 0.1157(10) -0.2658(7) 0.226(4) Uani 1 1 d U
C31 C 0.3459(16) 0.1399(14) -0.2198(8) 0.321(7) Uani 1 1 d U
H31A H 0.3821 0.0812 -0.1906 0.481 Uiso 1 1 calc R
H31B H 0.2713 0.1205 -0.2290 0.481 Uiso 1 1 calc R
H31C H 0.3576 0.2345 -0.2089 0.481 Uiso 1 1 calc R
C32 C 0.3519(15) 0.1917(15) -0.3181(8) 0.309(7) Uani 1 1 d U
H32A H 0.3941 0.1623 -0.3417 0.463 Uiso 1 1 calc R
H32B H 0.3615 0.2887 -0.3114 0.463 Uiso 1 1 calc R
H32C H 0.2785 0.1731 -0.3350 0.463 Uiso 1 1 calc 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'
F F 0.0171 0.0103 '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
O1 Zn1 O2 158.90(9) . 3_654
O1 Zn1 N2 101.59(9) . .
O2 Zn1 N2 99.39(9) 3_654 .
O1 Zn1 O4 90.04(10) . 4
O2 Zn1 O4 87.32(10) 3_654 4
N2 Zn1 O4 103.25(9) . 4
O1 Zn1 O3 86.09(11) . 2_654
O2 Zn1 O3 88.92(11) 3_654 2_654
N2 Zn1 O3 97.75(10) . 2_654
O4 Zn1 O3 159.00(9) 4 2_654
O1 Zn1 Zn1 81.07(6) . 3_654
O2 Zn1 Zn1 77.83(6) 3_654 3_654
N2 Zn1 Zn1 172.37(7) . 3_654
O4 Zn1 Zn1 83.81(7) 4 3_654
O3 Zn1 Zn1 75.20(7) 2_654 3_654
C1 O1 Zn1 125.3(2) . .
C1 O2 Zn1 129.0(2) . 3_654
C17 O3 Zn1 133.2(2) . 2_644
C17 O4 Zn1 121.77(19) . 4_556
C21 N1 C23 115.7(4) . .
C28 N2 C30 116.7(3) . .
C28 N2 Zn1 121.9(2) . .
C30 N2 Zn1 121.4(2) . .
O1 C1 O2 126.1(3) . .
O1 C1 C2 117.2(3) . .
O2 C1 C2 116.7(3) . .
C3 C2 C5 118.6(3) . .
C3 C2 C1 120.6(3) . .
C5 C2 C1 120.8(2) . .
C2 C3 C4 120.6(3) . .
C3 C4 C7 120.7(3) . .
C2 C5 C6 121.2(3) . .
C7 C6 C5 120.2(3) . .
C6 C7 C4 118.7(2) . .
C6 C7 C8 123.8(3) . .
C4 C7 C8 117.4(2) . .
C11 C8 C9 113.1(2) . .
C11 C8 C7 110.7(2) . .
C9 C8 C7 107.0(2) . .
C11 C8 C10 105.8(2) . .
C9 C8 C10 107.9(3) . .
C7 C8 C10 112.5(3) . .
F3 C9 F2 106.6(3) . .
F3 C9 F1 106.4(3) . .
F2 C9 F1 106.2(3) . .
F3 C9 C8 112.1(3) . .
F2 C9 C8 114.2(3) . .
F1 C9 C8 111.0(3) . .
F5 C10 F4 107.0(3) . .
F5 C10 F6 107.3(3) . .
F4 C10 F6 106.7(3) . .
F5 C10 C8 112.1(3) . .
F4 C10 C8 111.2(3) . .
F6 C10 C8 112.3(3) . .
C12 C11 C14 118.4(3) . .
C12 C11 C8 118.1(2) . .
C14 C11 C8 123.4(3) . .
C13 C12 C11 121.1(3) . .
C12 C13 C16 120.5(3) . .
C15 C14 C11 120.4(3) . .
C14 C15 C16 121.1(3) . .
C15 C16 C13 118.5(3) . .
C15 C16 C17 120.6(3) . .
C13 C16 C17 121.0(3) . .
O3 C17 O4 125.9(3) . .
O3 C17 C16 116.8(3) . .
O4 C17 C16 117.3(3) . .
N1 C21 C22 124.4(4) . .
C25 C22 C21 119.8(4) . .
N1 C23 C24 124.2(5) . .
C25 C24 C23 120.0(5) . .
C24 C25 C22 115.8(3) . .
C24 C25 C26 121.5(3) . .
C22 C25 C26 122.6(3) . .
C29 C26 C27 115.6(3) . .
C29 C26 C25 122.0(3) . .
C27 C26 C25 122.4(3) . .
C26 C27 C28 121.0(3) . .
N2 C28 C27 122.5(3) . .
C26 C29 C30 120.5(3) . .
N2 C30 C29 123.6(3) . .
O5 C33 N3 106.9(18) . .
C33 N3 C32 112.2(18) . .
C33 N3 C31 122.7(19) . .
C32 N3 C31 125.1(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.027(2) .
Zn1 O2 2.035(2) 3_654
Zn1 N2 2.042(2) .
Zn1 O4 2.042(2) 4
Zn1 O3 2.046(2) 2_654
Zn1 Zn1 2.9774(7) 3_654
F1 C9 1.345(4) .
F2 C9 1.332(4) .
F3 C9 1.334(5) .
F4 C10 1.338(4) .
F5 C10 1.313(5) .
F6 C10 1.341(4) .
O1 C1 1.249(4) .
O2 C1 1.256(3) .
O2 Zn1 2.035(2) 3_654
O3 C17 1.252(4) .
O3 Zn1 2.046(2) 2_644
O4 C17 1.258(4) .
O4 Zn1 2.042(2) 4_556
N1 C21 1.298(6) .
N1 C23 1.316(8) .
N2 C28 1.311(4) .
N2 C30 1.314(4) .
C1 C2 1.499(4) .
C2 C3 1.384(4) .
C2 C5 1.383(4) .
C3 C4 1.383(4) .
C4 C7 1.394(4) .
C5 C6 1.387(4) .
C6 C7 1.381(4) .
C7 C8 1.540(4) .
C8 C11 1.541(4) .
C8 C9 1.540(5) .
C8 C10 1.558(5) .
C11 C12 1.384(4) .
C11 C14 1.395(4) .
C12 C13 1.380(4) .
C13 C16 1.393(4) .
C14 C15 1.382(4) .
C15 C16 1.384(4) .
C16 C17 1.499(4) .
C21 C22 1.385(5) .
C22 C25 1.375(5) .
C23 C24 1.379(6) .
C24 C25 1.363(6) .
C25 C26 1.479(4) .
C26 C29 1.361(5) .
C26 C27 1.361(5) .
C27 C28 1.386(5) .
C29 C30 1.374(5) .
O5 C33 1.444(17) .
C33 N3 1.228(17) .
N3 C32 1.487(18) .
N3 C31 1.42(2) .
