#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:18:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179446 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/43/4334316.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_4334316
loop_
_publ_author_name
'Minhak Oh'
'Lalit Rajput'
'Dongwook Kim'
'Dohyun Moon'
'Myoung Soo Lah'
_publ_section_title
;
 Crystal-to-Crystal Transformations of a Series of Isostructural
 Metal-Organic Frameworks with Different Sizes of Ligated Solvent
 Molecules
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3891
_journal_page_last               3899
_journal_paper_doi               10.1021/ic302641v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C21 H36 N O15 Zn2'
_chemical_formula_weight         673.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.385(3)
_cell_length_b                   14.712(3)
_cell_length_c                   15.573(3)
_cell_measurement_reflns_used    18871
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.03
_cell_volume                     3066.6(11)
_computing_cell_refinement       'Rigaku Rapid Auto'
_computing_data_collection       'Rigaku Rapid Auto'
_computing_data_reduction        'Rigaku Rapid Auto'
_computing_molecular_graphics    'Diamond 3,ORTEP3'
_computing_publication_material  WinGX
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'imaging plate'
_diffrn_measurement_method       '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  0.1936
_diffrn_reflns_av_sigmaI/netI    0.1400
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23228
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  0.5839
_exptl_absorpt_correction_T_min  0.4963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rigaku Rapid Auto'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5394
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0973
_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)+(0.1373P)²+5.7827P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2329
_refine_ls_wR_factor_ref         0.2588
_reflns_number_gt                4279
_reflns_number_total             5394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302641v_si_001.cif
_cod_data_source_block           l12_059or
_cod_original_cell_volume        3066.7(11)
_cod_database_code               4334316
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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 -0.21248(9) 0.29730(8) 0.20923(7) 0.0402(3) Uani 1 1 d .
Zn2 Zn -0.04996(9) 0.44806(8) 0.09328(7) 0.0416(3) Uani 1 1 d .
O1 O -0.0932(6) 0.2241(5) 0.1974(5) 0.0491(18) Uani 1 1 d .
O2 O -0.0343(6) 0.3073(5) 0.0871(5) 0.0512(18) Uani 1 1 d .
O3 O 0.2233(6) 0.1842(5) -0.0977(5) 0.0481(17) Uani 1 1 d .
O4 O 0.3006(5) 0.0542(6) -0.0647(5) 0.0507(18) Uani 1 1 d .
O5 O 0.2192(6) -0.0976(5) 0.2156(5) 0.0505(17) Uani 1 1 d .
O6 O 0.0739(5) -0.0593(6) 0.2750(4) 0.0455(16) Uani 1 1 d .
C1 C 0.0439(8) 0.1688(7) 0.1199(6) 0.038(2) Uani 1 1 d .
C2 C 0.1048(8) 0.1744(7) 0.0466(6) 0.040(2) Uani 1 1 d .
H2 H 0.0966 0.2240 0.0082 0.048 Uiso 1 1 calc R
C3 C 0.1755(8) 0.1101(8) 0.0294(7) 0.046(2) Uani 1 1 d .
C4 C 0.1917(8) 0.0387(7) 0.0870(6) 0.042(2) Uani 1 1 d .
H4 H 0.2433 -0.0043 0.0766 0.050 Uiso 1 1 calc R
C5 C 0.1315(8) 0.0309(7) 0.1601(6) 0.041(2) Uani 1 1 d .
C6 C 0.0587(9) 0.0962(8) 0.1756(7) 0.050(3) Uani 1 1 d .
H6 H 0.0182 0.0911 0.2255 0.060 Uiso 1 1 calc R
C7 C -0.0331(8) 0.2392(7) 0.1368(6) 0.042(2) Uani 1 1 d .
C8 C 0.2388(8) 0.1143(8) -0.0495(7) 0.048(3) Uani 1 1 d .
C9 C 0.1437(7) -0.0466(8) 0.2208(7) 0.043(2) Uani 1 1 d .
N1N N -0.3177(8) 0.1924(8) 0.3264(7) 0.059(3) Uani 1 1 d .
O1N O -0.3257(7) 0.2173(6) 0.2498(5) 0.057(2) Uani 1 1 d .
O2N O -0.2422(8) 0.2149(8) 0.3675(6) 0.071(3) Uani 1 1 d .
O3N O -0.3851(10) 0.1481(11) 0.3611(9) 0.115(5) Uani 1 1 d .
O1E O -0.0712(6) 0.5893(5) 0.0920(5) 0.0502(18) Uani 1 1 d .
C1E C 0.0064(11) 0.6601(9) 0.0833(12) 0.068(4) Uani 1 1 d U
H1E1 H 0.0280 0.6637 0.0226 0.082 Uiso 1 1 calc R
H1E2 H 0.0652 0.6432 0.1184 0.082 Uiso 1 1 calc R
C2E C -0.0309(14) 0.7504(12) 0.1114(12) 0.088(5) Uani 1 1 d U
H2E1 H -0.0587 0.7830 0.0619 0.132 Uiso 1 1 calc R
H2E2 H 0.0244 0.7857 0.1358 0.132 Uiso 1 1 calc R
H2E3 H -0.0830 0.7423 0.1549 0.132 Uiso 1 1 calc R
O2E O -0.0124(7) 0.4605(6) -0.0360(5) 0.062(2) Uani 1 1 d .
C3E C 0.0272(13) 0.3919(11) -0.0943(10) 0.076(4) Uani 1 1 d U
H3E1 H 0.0797 0.3561 -0.0650 0.091 Uiso 1 1 calc R
H3E2 H 0.0574 0.4217 -0.1451 0.091 Uiso 1 1 calc R
C4E C -0.0566(19) 0.3303(13) -0.1221(12) 0.106(7) Uani 1 1 d U
H4E1 H -0.0787 0.2935 -0.0732 0.159 Uiso 1 1 calc R
H4E2 H -0.0331 0.2902 -0.1681 0.159 Uiso 1 1 calc R
H4E3 H -0.1126 0.3670 -0.1431 0.159 Uiso 1 1 calc R
O3E O 0.1011(6) 0.4629(8) 0.1208(6) 0.071(3) Uani 1 1 d .
C5E C 0.1527(14) 0.4239(15) 0.1941(12) 0.094(5) Uani 1 1 d DU
H5E1 H 0.1950 0.3732 0.1733 0.113 Uiso 1 1 calc R
H5E2 H 0.1022 0.3976 0.2333 0.113 Uiso 1 1 calc R
C6E C 0.215(3) 0.486(3) 0.243(2) 0.201(16) Uani 1 1 d DU
H6E1 H 0.2647 0.5135 0.2051 0.302 Uiso 1 1 calc R
H6E2 H 0.2496 0.4517 0.2886 0.302 Uiso 1 1 calc R
H6E3 H 0.1736 0.5330 0.2690 0.302 Uiso 1 1 calc R
O1S O 0.2386(10) 0.5476(11) 1.0177(8) 0.106(4) Uani 1 1 d .
H1S H 0.2538 0.5643 1.0676 0.159 Uiso 1 1 calc R
C1S C 0.318(3) 0.513(3) 0.980(3) 0.23(2) Uani 1 1 d U
H1S1 H 0.3777 0.5205 1.0165 0.274 Uiso 1 1 calc R
H1S2 H 0.3302 0.5445 0.9243 0.274 Uiso 1 1 calc R
C2S C 0.296(5) 0.419(5) 0.966(4) 0.35(4) Uani 1 1 d U
H2S1 H 0.3386 0.3824 1.0036 0.524 Uiso 1 1 calc R
H2S2 H 0.3101 0.4038 0.9059 0.524 Uiso 1 1 calc R
H2S3 H 0.2260 0.4077 0.9788 0.524 Uiso 1 1 calc R
O2S O 0.7619(8) 0.6623(8) 0.0178(7) 0.075(3) Uani 1 1 d .
H2S H 0.7523 0.6689 -0.0352 0.113 Uiso 1 1 calc R
C3S C 0.6724(14) 0.6743(18) 0.0614(14) 0.110(7) Uani 1 1 d U
H3S1 H 0.6497 0.7377 0.0527 0.131 Uiso 1 1 calc R
H3S2 H 0.6216 0.6337 0.0358 0.131 Uiso 1 1 calc R
C4S C 0.6773(19) 0.658(3) 0.1475(15) 0.189(18) Uani 1 1 d U
H4S1 H 0.6346 0.6055 0.1616 0.283 Uiso 1 1 calc R
H4S2 H 0.6542 0.7112 0.1792 0.283 Uiso 1 1 calc R
H4S3 H 0.7464 0.6439 0.1637 0.283 Uiso 1 1 calc R
O3S O 0.9155(7) 0.5860(8) 0.8583(6) 0.070(3) Uani 1 1 d .
H3S H 0.8701 0.5642 0.8273 0.105 Uiso 1 1 calc R
C5S C 0.9934(12) 0.6199(12) 0.8055(11) 0.081(5) Uani 1 1 d U
H5S1 H 1.0583 0.6097 0.8345 0.097 Uiso 1 1 calc R
H5S2 H 0.9846 0.6862 0.7981 0.097 Uiso 1 1 calc R
C6S C 0.9958(16) 0.5772(18) 0.7217(13) 0.116(8) Uani 1 1 d U
H6S1 H 1.0076 0.5118 0.7285 0.175 Uiso 1 1 calc R
H6S2 H 1.0497 0.6039 0.6874 0.175 Uiso 1 1 calc R
H6S3 H 0.9318 0.5869 0.6927 0.175 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'
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 122.6(3) . 3
O1 Zn1 O3 110.8(3) . 4_455
O5 Zn1 O3 113.8(3) 3 4_455
O1 Zn1 O1N 108.9(4) . .
O5 Zn1 O1N 103.9(4) 3 .
O3 Zn1 O1N 91.6(3) 4_455 .
O4 Zn2 O3E 174.8(4) 4_455 .
O4 Zn2 O6 93.6(3) 4_455 3
O3E Zn2 O6 87.2(3) . 3
O4 Zn2 O2 94.2(3) 4_455 .
O3E Zn2 O2 90.9(4) . .
O6 Zn2 O2 90.5(3) 3 .
O4 Zn2 O2E 91.5(4) 4_455 .
O3E Zn2 O2E 87.5(4) . .
O6 Zn2 O2E 174.5(4) 3 .
O2 Zn2 O2E 91.0(3) . .
O4 Zn2 O1E 83.2(3) 4_455 .
O3E Zn2 O1E 91.7(4) . .
O6 Zn2 O1E 92.3(3) 3 .
O2 Zn2 O1E 176.3(3) . .
O2E Zn2 O1E 86.4(3) . .
C7 O1 Zn1 120.0(7) . .
C7 O2 Zn2 139.5(7) . .
C8 O3 Zn1 123.8(7) . 4
C8 O4 Zn2 135.0(8) . 4
C9 O5 Zn1 113.4(7) . 3_545
C9 O6 Zn2 139.5(7) . 3_545
C6 C1 C2 117.9(10) . .
C6 C1 C7 121.7(9) . .
C2 C1 C7 120.4(9) . .
C3 C2 C1 121.5(9) . .
C2 C3 C4 120.1(9) . .
C2 C3 C8 121.8(10) . .
C4 C3 C8 118.1(10) . .
C3 C4 C5 119.6(9) . .
C6 C5 C4 119.2(9) . .
C6 C5 C9 119.8(9) . .
C4 C5 C9 121.0(9) . .
C5 C6 C1 121.6(10) . .
O1 C7 O2 126.1(10) . .
O1 C7 C1 116.9(9) . .
O2 C7 C1 117.0(9) . .
O4 C8 O3 124.6(10) . .
O4 C8 C3 120.5(10) . .
O3 C8 C3 114.8(10) . .
O5 C9 O6 122.9(10) . .
O5 C9 C5 120.2(9) . .
O6 C9 C5 116.9(9) . .
O3N N1N O2N 120.6(12) . .
O3N N1N O1N 120.5(12) . .
O2N N1N O1N 118.9(10) . .
N1N O1N Zn1 113.8(7) . .
C1E O1E Zn2 127.2(7) . .
O1E C1E C2E 111.6(12) . .
C3E O2E Zn2 129.0(8) . .
O2E C3E C4E 109.0(14) . .
C5E O3E Zn2 125.7(10) . .
O3E C5E C6E 116(2) . .
O1S C1S C2S 106(3) . .
C4S C3S O2S 114.6(18) . .
O3S C5S C6S 112.7(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.934(7) .
Zn1 O5 1.942(8) 3
Zn1 O3 1.956(7) 4_455
Zn1 O1N 2.020(8) .
Zn2 O4 2.049(7) 4_455
Zn2 O3E 2.078(8) .
Zn2 O6 2.078(7) 3
Zn2 O2 2.083(8) .
Zn2 O2E 2.084(7) .
Zn2 O1E 2.098(8) .
O1 C7 1.261(13) .
O2 C7 1.266(13) .
O3 C8 1.291(14) .
O3 Zn1 1.956(7) 4
O4 C8 1.234(14) .
O4 Zn2 2.049(7) 4
O5 C9 1.261(13) .
O5 Zn1 1.942(8) 3_545
O6 C9 1.273(12) .
O6 Zn2 2.078(7) 3_545
C1 C6 1.391(15) .
C1 C2 1.405(14) .
C1 C7 1.484(15) .
C2 C3 1.365(16) .
C3 C4 1.398(15) .
C3 C8 1.495(16) .
C4 C5 1.400(15) .
C5 C6 1.389(16) .
C5 C9 1.490(14) .
N1N O3N 1.238(15) .
N1N O2N 1.243(14) .
N1N O1N 1.253(13) .
O1E C1E 1.477(15) .
C1E C2E 1.48(2) .
O2E C3E 1.456(16) .
C3E C4E 1.51(3) .
O3E C5E 1.452(19) .
C5E C6E 1.452(19) .
O1S C1S 1.31(4) .
C1S C2S 1.43(8) .
O2S C3S 1.388(19) .
C3S C4S 1.37(3) .
O3S C5S 1.418(17) .
C5S C6S 1.45(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S O3N 0.84 2.42 3.097(19) 138.6 3_556
O1S H1S O2N 0.84 2.44 3.042(18) 129.2 3_556
O2S H2S O2N 0.84 2.29 2.968(14) 138.3 2_564
O3S H3S O5 0.84 2.18 2.874(12) 139.5 4_556
