#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:18:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178808 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/62/4106240.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_4106240
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 H20 F2 N2 O9 Zn2'
_chemical_formula_weight         745.24
_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           SHELXTL
_cell_angle_alpha                98.19(3)
_cell_angle_beta                 95.00(3)
_cell_angle_gamma                102.13(3)
_cell_formula_units_Z            2
_cell_length_a                   9.824(2)
_cell_length_b                   10.461(2)
_cell_length_c                   14.573(3)
_cell_measurement_reflns_used    4160
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      27.4430
_cell_measurement_theta_min      3.2062
_cell_volume                     1438.6(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      93.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11695
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8830
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.049
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0623P)²+8.2440P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1906
_reflns_number_gt                4356
_reflns_number_total             6304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201484s_si_002_6.cif
_cod_data_source_block           compound2e
_cod_original_cell_volume        1438.6(5)
_cod_database_code               4106240
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 0.54627(8) 0.73401(7) 0.61120(5) 0.0215(2) Uani 1 1 d .
Zn2 Zn 0.54647(8) 0.77277(7) 0.85335(6) 0.0272(2) Uani 1 1 d .
O1 O 0.3458(5) 0.6837(4) 0.6091(3) 0.0252(10) Uani 1 1 d .
O2 O 0.2877(5) 0.8560(5) 0.5521(4) 0.0364(12) Uani 1 1 d .
O3 O -0.2544(5) 0.8193(4) 0.8390(4) 0.0295(11) Uani 1 1 d .
O4 O -0.1857(6) 0.6511(5) 0.8952(3) 0.0372(13) Uani 1 1 d .
O5 O 0.6116(5) 0.9204(4) 0.6688(3) 0.0223(9) Uani 1 1 d .
O6 O 0.5075(5) 0.9290(4) 0.8000(3) 0.0299(11) Uani 1 1 d .
O7 O 0.6019(5) 1.5839(4) 0.6615(3) 0.0214(9) Uani 1 1 d .
O8 O 0.4895(5) 1.5862(4) 0.7897(3) 0.0233(10) Uani 1 1 d .
N1 N 0.6573(6) 0.7362(5) 0.5018(4) 0.0216(11) Uani 1 1 d .
N2 N 1.3816(6) 0.7641(5) -0.0685(4) 0.0224(12) Uani 1 1 d .
F1 F 0.7968(4) 0.9016(4) 0.1991(3) 0.0312(9) Uani 1 1 d .
F2 F 0.9561(4) 0.9048(4) 0.0652(3) 0.0287(9) Uani 1 1 d .
C1 C 0.1501(7) 0.7554(6) 0.6599(5) 0.0264(14) Uani 1 1 d .
C2 C 0.1514(7) 0.6874(6) 0.7350(5) 0.0257(14) Uani 1 1 d .
H2B H 0.2231 0.6438 0.7456 0.031 Uiso 1 1 calc R
C3 C 0.0484(7) 0.6828(6) 0.7948(5) 0.0258(14) Uani 1 1 d .
H3A H 0.0518 0.6367 0.8447 0.031 Uiso 1 1 calc R
C4 C -0.0603(7) 0.7474(6) 0.7798(5) 0.0284(15) Uani 1 1 d .
C5 C -0.0640(7) 0.8154(6) 0.7045(5) 0.0273(15) Uani 1 1 d .
H5A H -0.1357 0.8592 0.6943 0.033 Uiso 1 1 calc R
C6 C 0.0383(7) 0.8183(6) 0.6444(5) 0.0286(15) Uani 1 1 d .
H6A H 0.0333 0.8622 0.5935 0.034 Uiso 1 1 calc R
C7 C 0.2681(7) 0.7689(6) 0.6015(5) 0.0277(15) Uani 1 1 d .
C8 C -0.1744(7) 0.7365(6) 0.8435(5) 0.0272(15) Uani 1 1 d .
C9 C 0.5672(7) 1.1270(6) 0.7354(5) 0.0246(14) Uani 1 1 d .
C10 C 0.5155(7) 1.1997(6) 0.8071(5) 0.0256(14) Uani 1 1 d .
H10A H 0.4837 1.1600 0.8568 0.031 Uiso 1 1 calc R
C11 C 0.5117(7) 1.3289(6) 0.8043(4) 0.0225(13) Uani 1 1 d .
H11A H 0.4771 1.3768 0.8521 0.027 Uiso 1 1 calc R
C12 C 0.5597(7) 1.3897(6) 0.7295(4) 0.0219(13) Uani 1 1 d .
C13 C 0.6144(7) 1.3193(6) 0.6592(4) 0.0225(13) Uani 1 1 d .
H13A H 0.6496 1.3607 0.6110 0.027 Uiso 1 1 calc R
C14 C 0.6168(7) 1.1871(6) 0.6607(5) 0.0231(13) Uani 1 1 d .
H14A H 0.6508 1.1390 0.6128 0.028 Uiso 1 1 calc R
C15 C 0.5615(7) 0.9824(6) 0.7347(5) 0.0232(14) Uani 1 1 d .
C16 C 0.5510(6) 1.5308(6) 0.7273(4) 0.0185(12) Uani 1 1 d .
C17 C 0.6891(7) 0.8476(6) 0.4625(5) 0.0258(14) Uani 1 1 d .
H17A H 0.6582 0.9220 0.4871 0.031 Uiso 1 1 calc R
C18 C 0.7656(7) 0.8547(6) 0.3872(5) 0.0257(14) Uani 1 1 d .
H18A H 0.7853 0.9324 0.3620 0.031 Uiso 1 1 calc R
C19 C 0.8131(7) 0.7440(6) 0.3495(5) 0.0242(14) Uani 1 1 d .
C20 C 0.7794(7) 0.6303(6) 0.3903(4) 0.0235(14) Uani 1 1 d .
H20A H 0.8086 0.5544 0.3669 0.028 Uiso 1 1 calc R
C21 C 0.7028(7) 0.6305(6) 0.4654(5) 0.0239(14) Uani 1 1 d .
H21A H 0.6819 0.5538 0.4917 0.029 Uiso 1 1 calc R
C22 C 0.8997(7) 0.7457(6) 0.2698(4) 0.0203(12) Uani 1 1 d .
C23 C 0.8910(7) 0.8252(6) 0.2012(4) 0.0228(13) Uani 1 1 d .
C24 C 0.9753(7) 0.8256(6) 0.1295(4) 0.0239(14) Uani 1 1 d .
C25 C 1.0730(7) 0.7474(6) 0.1224(4) 0.0238(14) Uani 1 1 d .
C26 C 1.0810(7) 0.6652(6) 0.1897(4) 0.0245(14) Uani 1 1 d .
H26A H 1.1428 0.6089 0.1860 0.029 Uiso 1 1 calc R
C27 C 0.9968(7) 0.6669(6) 0.2625(4) 0.0241(14) Uani 1 1 d .
H27A H 1.0064 0.6134 0.3073 0.029 Uiso 1 1 calc R
C28 C 1.1709(7) 0.7519(6) 0.0491(4) 0.0243(14) Uani 1 1 d .
C29 C 1.2291(7) 0.8715(6) 0.0182(5) 0.0267(15) Uani 1 1 d .
H29A H 1.1980 0.9480 0.0370 0.032 Uiso 1 1 calc R
C30 C 1.3321(7) 0.8732(6) -0.0397(5) 0.0269(15) Uani 1 1 d .
H30A H 1.3695 0.9520 -0.0600 0.032 Uiso 1 1 calc R
C31 C 1.3272(7) 0.6514(7) -0.0392(5) 0.0284(15) Uani 1 1 d .
H31A H 1.3611 0.5767 -0.0586 0.034 Uiso 1 1 calc R
C32 C 1.2228(7) 0.6406(6) 0.0188(4) 0.0241(14) Uani 1 1 d .
H32A H 1.1874 0.5600 0.0375 0.029 Uiso 1 1 calc R
O1W O 0.6421(9) 0.7177(9) 0.9930(6) 0.091(3) 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'
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
O1 Zn1 O5 108.92(18) . .
O1 Zn1 O7 100.36(18) . 1_545
O5 Zn1 O7 124.65(19) . 1_545
O1 Zn1 N1 127.8(2) . .
O5 Zn1 N1 98.67(19) . .
O7 Zn1 N1 98.74(19) 1_545 .
O3 Zn2 O8 102.51(19) 1_655 1_545
O3 Zn2 O6 92.88(19) 1_655 .
O8 Zn2 O6 125.3(2) 1_545 .
O3 Zn2 N2 152.5(2) 1_655 1_456
O8 Zn2 N2 95.92(19) 1_545 1_456
O6 Zn2 N2 92.9(2) . 1_456
O3 Zn2 O1W 80.2(3) 1_655 .
O8 Zn2 O1W 93.8(3) 1_545 .
O6 Zn2 O1W 140.8(3) . .
N2 Zn2 O1W 78.3(3) 1_456 .
C7 O1 Zn1 121.2(4) . .
C8 O3 Zn2 122.4(4) . 1_455
C15 O5 Zn1 127.2(4) . .
C15 O6 Zn2 129.0(4) . .
C16 O7 Zn1 125.7(4) . 1_565
C16 O8 Zn2 126.3(4) . 1_565
C21 N1 C17 117.7(5) . .
C21 N1 Zn1 122.0(4) . .
C17 N1 Zn1 120.3(4) . .
C31 N2 C30 118.3(6) . .
C31 N2 Zn2 119.7(4) . 1_654
C30 N2 Zn2 121.8(4) . 1_654
C2 C1 C6 117.8(6) . .
C2 C1 C7 120.8(6) . .
C6 C1 C7 121.2(6) . .
C3 C2 C1 121.7(6) . .
C2 C3 C4 119.9(6) . .
C5 C4 C3 119.3(7) . .
C5 C4 C8 121.7(6) . .
C3 C4 C8 118.9(6) . .
C6 C5 C4 120.6(6) . .
C5 C6 C1 120.7(7) . .
O2 C7 O1 124.7(7) . .
O2 C7 C1 121.1(6) . .
O1 C7 C1 114.2(6) . .
O4 C8 O3 124.8(7) . .
O4 C8 C4 119.5(6) . .
O3 C8 C4 115.7(6) . .
C10 C9 C14 120.1(6) . .
C10 C9 C15 120.1(6) . .
C14 C9 C15 119.7(6) . .
C11 C10 C9 120.2(6) . .
C10 C11 C12 120.3(6) . .
C13 C12 C11 120.0(6) . .
C13 C12 C16 121.0(6) . .
C11 C12 C16 119.0(5) . .
C12 C13 C14 120.1(6) . .
C13 C14 C9 119.4(6) . .
O6 C15 O5 123.8(5) . .
O6 C15 C9 118.1(6) . .
O5 C15 C9 118.1(5) . .
O7 C16 O8 125.1(5) . .
O7 C16 C12 117.0(5) . .
O8 C16 C12 117.8(5) . .
N1 C17 C18 122.6(6) . .
C17 C18 C19 119.4(6) . .
C18 C19 C20 117.4(6) . .
C18 C19 C22 122.3(6) . .
C20 C19 C22 120.3(6) . .
C21 C20 C19 120.0(6) . .
N1 C21 C20 122.8(6) . .
C27 C22 C23 116.5(6) . .
C27 C22 C19 119.8(5) . .
C23 C22 C19 123.7(6) . .
F1 C23 C24 116.5(5) . .
F1 C23 C22 121.7(6) . .
C24 C23 C22 121.7(6) . .
F2 C24 C25 121.3(6) . .
F2 C24 C23 116.9(6) . .
C25 C24 C23 121.8(6) . .
C24 C25 C26 117.0(6) . .
C24 C25 C28 122.8(6) . .
C26 C25 C28 120.1(6) . .
C25 C26 C27 120.7(6) . .
C22 C27 C26 122.1(6) . .
C32 C28 C29 117.5(6) . .
C32 C28 C25 120.0(5) . .
C29 C28 C25 121.8(6) . .
C30 C29 C28 119.2(6) . .
N2 C30 C29 122.6(6) . .
N2 C31 C32 123.0(6) . .
C31 C32 C28 119.4(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.925(4) .
Zn1 O5 1.958(4) .
Zn1 O7 1.980(4) 1_545
Zn1 N1 2.009(5) .
Zn2 O3 1.951(5) 1_655
Zn2 O8 1.980(4) 1_545
Zn2 O6 1.998(5) .
Zn2 N2 2.054(5) 1_456
Zn2 O1W 2.364(9) .
O1 C7 1.301(8) .
O2 C7 1.233(8) .
O3 C8 1.291(8) .
O3 Zn2 1.951(5) 1_455
O4 C8 1.242(8) .
O5 C15 1.274(7) .
O6 C15 1.271(8) .
O7 C16 1.263(7) .
O7 Zn1 1.980(4) 1_565
O8 C16 1.273(7) .
O8 Zn2 1.980(4) 1_565
N1 C21 1.337(8) .
N1 C17 1.361(8) .
N2 C31 1.333(8) .
N2 C30 1.359(8) .
N2 Zn2 2.054(5) 1_654
F1 C23 1.344(7) .
F2 C24 1.363(7) .
C1 C2 1.389(9) .
C1 C6 1.411(9) .
C1 C7 1.491(10) .
C2 C3 1.389(9) .
C3 C4 1.396(9) .
C4 C5 1.392(9) .
C4 C8 1.513(10) .
C5 C6 1.388(10) .
C9 C10 1.399(9) .
C9 C14 1.405(9) .
C9 C15 1.501(8) .
C10 C11 1.366(8) .
C11 C12 1.406(8) .
C12 C13 1.388(9) .
C12 C16 1.501(8) .
C13 C14 1.392(8) .
C17 C18 1.384(9) .
C18 C19 1.396(9) .
C19 C20 1.396(8) .
C19 C22 1.499(8) .
C20 C21 1.381(9) .
C22 C27 1.388(9) .
C22 C23 1.396(8) .
C23 C24 1.389(9) .
C24 C25 1.387(9) .
C25 C26 1.401(9) .
C25 C28 1.497(8) .
C26 C27 1.400(9) .
C28 C32 1.398(9) .
C28 C29 1.414(8) .
C29 C30 1.371(9) .
C31 C32 1.381(9) .
