#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:18:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178808 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/62/4106239.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_4106239
loop_
_publ_author_name
'Joobeom Seo'
'Charlotte Bonneau'
'Ryotaro Matsuda'
'Masaki Takata'
'Susumu Kitagawa'
_publ_section_title
;
 Soft Secondary Building Unit: Dynamic Bond Rearrangement on Multinuclear
 Core of Porous Coordination Polymers in Gas Media
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9005
_journal_page_last               9013
_journal_paper_doi               10.1021/ja201484s
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C32 H18 F2 N2 O8 Zn2'
_chemical_formula_weight         727.22
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                97.76(3)
_cell_angle_beta                 91.69(3)
_cell_angle_gamma                100.83(3)
_cell_formula_units_Z            2
_cell_length_a                   9.845(2)
_cell_length_b                   10.409(2)
_cell_length_c                   14.986(3)
_cell_measurement_reflns_used    4118
_cell_measurement_temperature    378.15
_cell_measurement_theta_max      27.5904
_cell_measurement_theta_min      3.0351
_cell_volume                     1492.2(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      378.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type
; 
Saturn724+ (4x4 bin mode) 
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6606
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.5904
_diffrn_reflns_theta_min         3.0351
_exptl_absorpt_coefficient_mu    1.676
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8872
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private commu1nication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0603
_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)+(0.0309P)²+1.9675P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                4466
_reflns_number_total             6606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201484s_si_002_5.cif
_cod_data_source_block           compound2d
_cod_original_cell_volume        1492.2(5)
_cod_database_code               4106239
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.54629(5) 0.73603(4) 0.60852(4) 0.03803(16) Uani 1 1 d .
Zn2 Zn 0.54213(6) 0.77514(4) 0.83953(4) 0.03893(16) Uani 1 1 d .
O1 O 0.2897(4) 0.8532(4) 0.5624(3) 0.0817(14) Uani 1 1 d .
O2 O 0.3520(3) 0.6867(3) 0.6201(3) 0.0565(10) Uani 1 1 d .
O3 O -0.2626(3) 0.8221(3) 0.8469(3) 0.0594(10) Uani 1 1 d .
O4 O -0.2069(4) 0.6448(4) 0.8956(3) 0.0847(14) Uani 1 1 d .
O5 O 0.6085(3) 0.5881(3) 0.6578(2) 0.0455(8) Uani 1 1 d .
O6 O 0.4934(3) 0.5895(3) 0.7842(2) 0.0487(9) Uani 1 1 d .
O7 O 0.6133(3) -0.0792(3) 0.6620(2) 0.0461(8) Uani 1 1 d .
O8 O 0.5011(3) -0.0707(3) 0.7889(2) 0.0477(9) Uani 1 1 d .
N1 N 0.6546(4) 0.7369(3) 0.4980(2) 0.0384(9) Uani 1 1 d .
N2 N 1.3986(4) 0.7687(3) -0.0665(2) 0.0390(9) Uani 1 1 d .
F1 F 0.8007(3) 0.9009(3) 0.2016(2) 0.0757(10) Uani 1 1 d .
F2 F 0.9668(3) 0.9045(3) 0.0696(2) 0.0744(10) Uani 1 1 d .
C1 C 0.1498(5) 0.7564(4) 0.6722(3) 0.0448(12) Uani 1 1 d .
C2 C 0.1517(5) 0.6903(4) 0.7466(3) 0.0443(11) Uani 1 1 d .
H2B H 0.2253 0.6493 0.7576 0.053 Uiso 1 1 calc R
C3 C 0.0443(5) 0.6854(5) 0.8044(3) 0.0497(12) Uani 1 1 d .
H3A H 0.0461 0.6402 0.8537 0.060 Uiso 1 1 calc R
C4 C -0.0655(5) 0.7467(4) 0.7896(3) 0.0463(12) Uani 1 1 d .
C5 C -0.0672(5) 0.8135(5) 0.7156(4) 0.0560(14) Uani 1 1 d .
H5A H -0.1401 0.8559 0.7053 0.067 Uiso 1 1 calc R
C6 C 0.0395(5) 0.8172(5) 0.6570(4) 0.0585(14) Uani 1 1 d .
H6A H 0.0369 0.8610 0.6070 0.070 Uiso 1 1 calc R
C7 C 0.2703(5) 0.7681(5) 0.6120(4) 0.0520(13) Uani 1 1 d .
C8 C -0.1850(5) 0.7351(5) 0.8514(4) 0.0545(14) Uani 1 1 d .
C9 C 0.5620(4) 0.3920(4) 0.7243(3) 0.0343(10) Uani 1 1 d .
C10 C 0.6196(5) 0.3215(4) 0.6548(3) 0.0403(11) Uani 1 1 d .
H10A H 0.6564 0.3632 0.6073 0.048 Uiso 1 1 calc R
C11 C 0.6225(5) 0.1886(4) 0.6560(3) 0.0401(11) Uani 1 1 d .
H11A H 0.6614 0.1415 0.6096 0.048 Uiso 1 1 calc R
C12 C 0.5667(4) 0.1264(4) 0.7270(3) 0.0340(10) Uani 1 1 d .
C13 C 0.5116(5) 0.1985(4) 0.7973(3) 0.0407(11) Uani 1 1 d .
H13A H 0.4761 0.1580 0.8456 0.049 Uiso 1 1 calc R
C14 C 0.5100(5) 0.3296(4) 0.7951(3) 0.0410(11) Uani 1 1 d .
H14A H 0.4731 0.3773 0.8422 0.049 Uiso 1 1 calc R
C15 C 0.5550(4) 0.5341(4) 0.7222(3) 0.0355(10) Uani 1 1 d .
C16 C 0.5602(5) -0.0186(4) 0.7260(3) 0.0373(10) Uani 1 1 d .
C17 C 0.6999(5) 0.6302(4) 0.4598(3) 0.0453(12) Uani 1 1 d .
H17A H 0.6770 0.5527 0.4851 0.054 Uiso 1 1 calc R
C18 C 0.7775(5) 0.6283(4) 0.3859(3) 0.0495(13) Uani 1 1 d .
H18A H 0.8059 0.5510 0.3620 0.059 Uiso 1 1 calc R
C19 C 0.8141(5) 0.7433(4) 0.3463(3) 0.0441(11) Uani 1 1 d .
C20 C 0.7651(5) 0.8531(4) 0.3852(3) 0.0503(13) Uani 1 1 d .
H20A H 0.7853 0.9316 0.3608 0.060 Uiso 1 1 calc R
C21 C 0.6872(5) 0.8468(4) 0.4591(3) 0.0475(13) Uani 1 1 d .
H21A H 0.6553 0.9219 0.4835 0.057 Uiso 1 1 calc R
C22 C 0.9045(5) 0.7454(4) 0.2688(3) 0.0447(12) Uani 1 1 d .
C23 C 1.0042(5) 0.6665(5) 0.2600(3) 0.0544(14) Uani 1 1 d .
H23A H 1.0118 0.6108 0.3027 0.065 Uiso 1 1 calc R
C24 C 1.0909(5) 0.6681(5) 0.1909(3) 0.0544(14) Uani 1 1 d .
H24A H 1.1555 0.6132 0.1877 0.065 Uiso 1 1 calc R
C25 C 1.0859(5) 0.7496(4) 0.1247(3) 0.0427(11) Uani 1 1 d .
C26 C 0.9852(5) 0.8265(5) 0.1323(3) 0.0504(13) Uani 1 1 d .
C27 C 0.8953(5) 0.8229(5) 0.2017(3) 0.0503(13) Uani 1 1 d .
C28 C 1.1883(5) 0.7567(4) 0.0547(3) 0.0409(11) Uani 1 1 d .
C29 C 1.2437(5) 0.6455(4) 0.0236(3) 0.0457(12) Uani 1 1 d .
H29A H 1.2100 0.5648 0.0429 0.055 Uiso 1 1 calc R
C30 C 1.3477(5) 0.6561(4) -0.0352(3) 0.0443(12) Uani 1 1 d .
H30A H 1.3845 0.5817 -0.0541 0.053 Uiso 1 1 calc R
C31 C 1.3443(5) 0.8742(4) -0.0388(3) 0.0468(12) Uani 1 1 d .
H31A H 1.3780 0.9528 -0.0607 0.056 Uiso 1 1 calc R
C32 C 1.2404(5) 0.8720(4) 0.0209(3) 0.0481(12) Uani 1 1 d .
H32A H 1.2054 0.9480 0.0384 0.058 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'
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'
F F 0.0171 0.0103 '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 O7 110.42(13) . 1_565
O2 Zn1 O5 99.47(14) . .
O7 Zn1 O5 121.81(15) 1_565 .
O2 Zn1 N1 129.92(17) . .
O7 Zn1 N1 98.18(13) 1_565 .
O5 Zn1 N1 98.91(13) . .
O3 Zn2 O6 107.01(14) 1_655 .
O3 Zn2 O8 98.47(14) 1_655 1_565
O6 Zn2 O8 126.94(15) . 1_565
O3 Zn2 N2 133.05(16) 1_655 1_456
O6 Zn2 N2 97.75(13) . 1_456
O8 Zn2 N2 97.38(13) 1_565 1_456
C7 O2 Zn1 121.4(3) . .
C8 O3 Zn2 121.8(3) . 1_455
C15 O5 Zn1 124.6(3) . .
C15 O6 Zn2 126.2(3) . .
C16 O7 Zn1 125.2(3) . 1_545
C16 O8 Zn2 126.8(3) . 1_545
C17 N1 C21 116.7(3) . .
C17 N1 Zn1 122.3(3) . .
C21 N1 Zn1 120.9(3) . .
C31 N2 C30 117.7(4) . .
C31 N2 Zn2 121.0(3) . 1_654
C30 N2 Zn2 121.2(3) . 1_654
C6 C1 C2 119.0(4) . .
C6 C1 C7 120.6(5) . .
C2 C1 C7 120.2(4) . .
C3 C2 C1 120.3(4) . .
C4 C3 C2 120.8(5) . .
C3 C4 C5 119.1(4) . .
C3 C4 C8 119.9(5) . .
C5 C4 C8 120.9(4) . .
C4 C5 C6 120.2(5) . .
C1 C6 C5 120.6(5) . .
O1 C7 O2 123.6(4) . .
O1 C7 C1 121.1(4) . .
O2 C7 C1 115.2(4) . .
O4 C8 O3 125.1(5) . .
O4 C8 C4 120.2(4) . .
O3 C8 C4 114.5(4) . .
C14 C9 C10 119.4(4) . .
C14 C9 C15 120.1(4) . .
C10 C9 C15 120.5(4) . .
C9 C10 C11 120.2(4) . .
C10 C11 C12 119.7(4) . .
C13 C12 C11 119.7(4) . .
C13 C12 C16 120.0(4) . .
C11 C12 C16 120.2(4) . .
C14 C13 C12 119.8(4) . .
C13 C14 C9 121.2(4) . .
O6 C15 O5 125.1(4) . .
O6 C15 C9 117.2(3) . .
O5 C15 C9 117.8(3) . .
O8 C16 O7 124.9(4) . .
O8 C16 C12 117.3(3) . .
O7 C16 C12 117.7(4) . .
N1 C17 C18 123.9(4) . .
C17 C18 C19 119.5(4) . .
C20 C19 C18 116.4(4) . .
C20 C19 C22 123.1(4) . .
C18 C19 C22 120.4(4) . .
C21 C20 C19 120.5(4) . .
N1 C21 C20 122.9(4) . .
C27 C22 C23 116.2(4) . .
C27 C22 C19 123.2(4) . .
C23 C22 C19 120.5(4) . .
C24 C23 C22 122.1(4) . .
C23 C24 C25 122.1(5) . .
C26 C25 C24 116.0(4) . .
C26 C25 C28 123.2(4) . .
C24 C25 C28 120.7(4) . .
F2 C26 C25 121.0(4) . .
F2 C26 C27 117.0(4) . .
C25 C26 C27 121.9(4) . .
F1 C27 C22 121.7(4) . .
F1 C27 C26 116.6(4) . .
C22 C27 C26 121.6(4) . .
C32 C28 C29 116.8(4) . .
C32 C28 C25 123.0(4) . .
C29 C28 C25 120.1(4) . .
C30 C29 C28 119.7(4) . .
N2 C30 C29 122.9(4) . .
N2 C31 C32 122.9(4) . .
C31 C32 C28 119.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 1.904(3) .
Zn1 O7 1.963(3) 1_565
Zn1 O5 1.981(3) .
Zn1 N1 1.996(3) .
Zn2 O3 1.888(3) 1_655
Zn2 O6 1.962(3) .
Zn2 O8 1.967(3) 1_565
Zn2 N2 2.023(3) 1_456
O1 C7 1.223(6) .
O2 C7 1.287(5) .
O3 C8 1.297(6) .
O3 Zn2 1.888(3) 1_455
O4 C8 1.212(6) .
O5 C15 1.261(5) .
O6 C15 1.258(5) .
O7 C16 1.258(5) .
O7 Zn1 1.963(3) 1_545
O8 C16 1.254(5) .
O8 Zn2 1.967(3) 1_545
N1 C17 1.337(5) .
N1 C21 1.344(5) .
N2 C31 1.332(5) .
N2 C30 1.337(5) .
N2 Zn2 2.023(3) 1_654
F1 C27 1.346(5) .
F2 C26 1.351(5) .
C1 C6 1.383(6) .
C1 C2 1.388(6) .
C1 C7 1.508(6) .
C2 C3 1.384(6) .
C3 C4 1.382(6) .
C4 C5 1.387(7) .
C4 C8 1.516(6) .
C5 C6 1.388(7) .
C9 C14 1.380(5) .
C9 C10 1.389(5) .
C9 C15 1.498(5) .
C10 C11 1.391(5) .
C11 C12 1.393(5) .
C12 C13 1.393(5) .
C12 C16 1.496(5) .
C13 C14 1.373(5) .
C17 C18 1.364(6) .
C18 C19 1.399(6) .
C19 C20 1.387(6) .
C19 C22 1.485(5) .
C20 C21 1.367(6) .
C22 C27 1.382(6) .
C22 C23 1.391(6) .
C23 C24 1.362(6) .
C24 C25 1.394(6) .
C25 C26 1.384(6) .
C25 C28 1.477(5) .
C26 C27 1.385(6) .
C28 C32 1.382(6) .
C28 C29 1.400(6) .
C29 C30 1.369(6) .
C31 C32 1.377(6) .
