#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:34:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179452 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/49/4334973.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_4334973
loop_
_publ_author_name
'Keunil Hong'
'Woojeong Bak'
'Hyungphil Chun'
_publ_section_title
;
 Unique Coordination-Based Heterometallic Approach for the Stoichiometric
 Inclusion of High-Valent Metal Ions in a Porous Metal-Organic Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5645
_journal_page_last               5647
_journal_paper_doi               10.1021/ic400607w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '[H2N(CH3)2][Zn3(OH)Ti(hbdc)3(HCO2)]'
_chemical_formula_sum            'C27 H19 N O18 Ti Zn3'
_chemical_formula_weight         889.44
_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                 97.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.472(3)
_cell_length_b                   14.628(3)
_cell_length_c                   21.029(4)
_cell_measurement_temperature    100(2)
_cell_volume                     5029.1(17)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Diamond 3'
_computing_structure_refinement  'Bruker SHELXTL-XL'
_computing_structure_solution    'Bruker SHELXTL-XS'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            58483
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  0.9154
_exptl_absorpt_correction_T_min  0.8645
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       Polyhedra
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.956
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.0304(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         16890
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1538P)²+0.5404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2151
_reflns_number_gt                13379
_reflns_number_total             16890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400607w_si_001.cif
_cod_data_source_block           ZTOF-1
_cod_database_code               4334973
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 0.205857(19) -1.14160(2) -1.954825(13) 0.03522(10) Uani 1 1 d .
Zn2 Zn 0.252683(17) -0.95330(2) -1.884900(14) 0.03545(10) Uani 1 1 d .
Zn3 Zn 0.055800(16) -0.99262(2) -1.927304(13) 0.03192(10) Uani 1 1 d .
Ti1 Ti 0.21343(3) -1.00235(3) -2.13111(2) 0.03404(12) Uani 1 1 d .
O1 O 0.28345(13) -0.85911(14) -1.96202(10) 0.0422(4) Uani 1 1 d .
O2 O 0.22826(10) -0.92601(12) -2.05114(8) 0.0352(3) Uani 1 1 d .
O3 O 0.32865(11) -1.00637(13) -2.12212(9) 0.0386(4) Uani 1 1 d .
O4 O 0.20657(11) -0.90463(14) -2.18868(9) 0.0391(4) Uani 1 1 d .
O5 O 0.09345(11) -0.98027(13) -2.12639(9) 0.0369(4) Uani 1 1 d .
O6 O 0.20235(13) -1.09415(13) -2.19345(8) 0.0399(4) Uani 1 1 d .
O7 O 0.20023(11) -1.10689(12) -2.06935(8) 0.0353(3) Uani 1 1 d .
O8 O 0.22865(17) -1.23808(15) -2.02194(9) 0.0517(5) Uani 1 1 d .
O9 O 0.08630(15) -1.20324(15) -1.97582(11) 0.0512(5) Uani 1 1 d .
O10 O 0.21550(14) -1.18224(14) -1.86493(9) 0.0440(4) Uani 1 1 d .
O11 O 0.22781(12) -1.04520(14) -1.81600(9) 0.0414(4) Uani 1 1 d .
O12 O 0.07395(13) -0.88935(16) -1.86423(10) 0.0484(5) Uani 1 1 d .
O13 O 0.20650(13) -0.85154(14) -1.84127(10) 0.0444(5) Uani 1 1 d .
O14 O 0.36679(13) -0.99487(16) -1.88330(12) 0.0512(5) Uani 1 1 d .
O15 O 0.32667(13) -1.1045(2) -1.95314(12) 0.0594(6) Uani 1 1 d .
O16 O 0.02919(11) -1.08318(14) -1.86288(9) 0.0386(4) Uani 1 1 d .
O17 O 0.16792(10) -1.01172(12) -1.94943(8) 0.0319(3) Uani 1 1 d .
H17O H 0.1709 -0.9866 -1.9855 0.048 Uiso 1 1 calc R
O18 O -0.00673(12) -0.91521(15) -1.99524(9) 0.0417(4) Uani 1 1 d .
C1 C 0.29069(16) -0.89308(17) -2.01503(12) 0.0363(5) Uani 1 1 d .
C2 C 0.37341(16) -0.89955(19) -2.03750(13) 0.0381(5) Uani 1 1 d .
C3 C 0.43826(19) -0.8526(2) -2.00379(16) 0.0488(7) Uani 1 1 d .
H3 H 0.4281 -0.8125 -1.9701 0.059 Uiso 1 1 calc R
C4 C 0.51648(19) -0.8631(2) -2.01812(16) 0.0494(7) Uani 1 1 d .
H4 H 0.5600 -0.8297 -1.9951 0.059 Uiso 1 1 calc R
C5 C 0.53244(16) -0.9238(2) -2.06727(14) 0.0437(6) Uani 1 1 d .
C6 C 0.46894(16) -0.9699(2) -2.10178(13) 0.0413(5) Uani 1 1 d .
H6 H 0.4797 -1.0099 -2.1353 0.050 Uiso 1 1 calc R
C7 C 0.38806(16) -0.95817(18) -2.08782(12) 0.0369(5) Uani 1 1 d .
C8 C 0.62060(17) -0.9429(2) -2.07882(14) 0.0459(6) Uani 1 1 d .
C9 C 0.14713(14) -0.84986(17) -2.21520(11) 0.0333(4) Uani 1 1 d .
C10 C 0.16702(15) -0.78458(18) -2.25975(12) 0.0363(5) Uani 1 1 d .
H10 H 0.2215 -0.7806 -2.2701 0.044 Uiso 1 1 calc R
C11 C 0.10807(16) -0.72645(19) -2.28850(13) 0.0400(5) Uani 1 1 d .
C12 C 0.02778(18) -0.7308(2) -2.27378(16) 0.0524(7) Uani 1 1 d .
H12 H -0.0129 -0.6910 -2.2942 0.063 Uiso 1 1 calc R
C13 C 0.00828(17) -0.7940(2) -2.22888(16) 0.0500(7) Uani 1 1 d .
H13 H -0.0460 -0.7962 -2.2181 0.060 Uiso 1 1 calc R
C14 C 0.06700(15) -0.85453(18) -2.19906(12) 0.0366(5) Uani 1 1 d .
C15 C 0.04234(14) -0.92047(18) -2.15172(11) 0.0332(4) Uani 1 1 d .
C16 C 0.21042(16) -1.18435(18) -2.19229(11) 0.0371(5) Uani 1 1 d .
C17 C 0.21206(15) -1.22977(19) -2.25073(11) 0.0371(5) Uani 1 1 d .
H17 H 0.2075 -1.1954 -2.2893 0.045 Uiso 1 1 calc R
C18 C 0.22011(18) -1.3228(2) -2.25327(12) 0.0417(5) Uani 1 1 d .
C19 C 0.2277(3) -1.3742(2) -2.19706(14) 0.0618(10) Uani 1 1 d .
H19 H 0.2339 -1.4387 -2.1987 0.074 Uiso 1 1 calc R
C20 C 0.2259(3) -1.3305(2) -2.13892(14) 0.0615(10) Uani 1 1 d .
H20 H 0.2295 -1.3657 -2.1007 0.074 Uiso 1 1 calc R
C21 C 0.2192(2) -1.23611(19) -2.13546(12) 0.0429(6) Uani 1 1 d .
C22 C 0.21698(19) -1.19249(18) -2.07264(12) 0.0399(5) Uani 1 1 d .
C23 C 0.0254(2) -1.1693(2) -2.00594(16) 0.0494(7) Uani 1 1 d .
H23 H -0.0104 -1.2087 -2.0320 0.059 Uiso 1 1 calc R
C24 C 0.22078(16) -1.1304(2) -1.81673(12) 0.0385(5) Uani 1 1 d .
C25 C 0.13142(18) -0.84404(19) -1.83514(12) 0.0389(5) Uani 1 1 d .
N1S N 0.3833(6) -0.7942(9) -1.7443(5) 0.229(5) Uani 1 1 d DU
H1S1 H 0.4336 -0.7860 -1.7582 0.275 Uiso 1 1 calc R
H1S2 H 0.3426 -0.7752 -1.7753 0.275 Uiso 1 1 calc R
C1S C 0.3777(6) -0.7478(8) -1.6792(5) 0.179(4) Uani 1 1 d D
H1S3 H 0.3847 -0.6816 -1.6835 0.269 Uiso 1 1 calc R
H1S4 H 0.4208 -0.7718 -1.6473 0.269 Uiso 1 1 calc R
H1S5 H 0.3241 -0.7604 -1.6654 0.269 Uiso 1 1 calc R
C2S C 0.3694(6) -0.9010(9) -1.7208(6) 0.192(5) Uani 1 1 d D
H2S1 H 0.3713 -0.9426 -1.7571 0.289 Uiso 1 1 calc R
H2S2 H 0.3161 -0.9061 -1.7049 0.289 Uiso 1 1 calc R
H2S3 H 0.4127 -0.9174 -1.6865 0.289 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 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2937 1.3977 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2746 0.4347 '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
O10 Zn1 O17 102.74(8) . .
O10 Zn1 O15 95.66(10) . .
O17 Zn1 O15 93.23(10) . .
O10 Zn1 O8 116.76(8) . .
O17 Zn1 O8 140.36(7) . .
O15 Zn1 O8 86.33(11) . .
O10 Zn1 O9 92.00(9) . .
O17 Zn1 O9 97.13(8) . .
O15 Zn1 O9 165.45(10) . .
O8 Zn1 O9 79.18(10) . .
O10 Zn1 O7 173.84(8) . .
O17 Zn1 O7 83.39(6) . .
O15 Zn1 O7 83.27(9) . .
O8 Zn1 O7 57.16(7) . .
O9 Zn1 O7 87.79(8) . .
O13 Zn2 O14 130.75(10) . .
O13 Zn2 O17 111.25(8) . .
O14 Zn2 O17 117.48(9) . .
O13 Zn2 O11 92.57(9) . .
O14 Zn2 O11 93.32(9) . .
O17 Zn2 O11 90.92(8) . .
O13 Zn2 O1 90.39(9) . .
O14 Zn2 O1 84.39(9) . .
O17 Zn2 O1 88.43(7) . .
O11 Zn2 O1 177.00(8) . .
O17 Zn3 O16 110.92(8) . .
O17 Zn3 O18 108.97(8) . .
O16 Zn3 O18 136.63(8) . .
O17 Zn3 O12 101.16(8) . .
O16 Zn3 O12 94.52(9) . .
O18 Zn3 O12 93.89(9) . .
O17 Zn3 O18 90.49(8) . 3_531
O16 Zn3 O18 90.26(8) . 3_531
O18 Zn3 O18 72.98(10) . 3_531
O12 Zn3 O18 164.84(9) . 3_531
O4 Ti1 O6 95.86(9) . .
O4 Ti1 O3 93.98(9) . .
O6 Ti1 O3 93.38(9) . .
O4 Ti1 O2 96.25(9) . .
O6 Ti1 O2 167.87(8) . .
O3 Ti1 O2 85.14(8) . .
O4 Ti1 O5 85.82(8) . .
O6 Ti1 O5 97.88(9) . .
O3 Ti1 O5 168.71(9) . .
O2 Ti1 O5 83.66(8) . .
O4 Ti1 O7 170.42(8) . .
O6 Ti1 O7 84.19(8) . .
O3 Ti1 O7 95.58(8) . .
O2 Ti1 O7 83.97(7) . .
O5 Ti1 O7 84.68(8) . .
C1 O1 Zn2 117.46(17) . .
C1 O2 Ti1 134.81(16) . .
C7 O3 Ti1 134.14(16) . .
C9 O4 Ti1 135.58(15) . .
C15 O5 Ti1 133.28(16) . .
C16 O6 Ti1 134.49(16) . .
C22 O7 Ti1 131.09(16) . .
C22 O7 Zn1 82.44(14) . .
Ti1 O7 Zn1 142.02(9) . .
C22 O8 Zn1 101.32(17) . .
C23 O9 Zn1 127.2(2) . .
C24 O10 Zn1 125.43(18) . .
C24 O11 Zn2 132.01(18) . .
C25 O12 Zn3 139.76(19) . .
C25 O13 Zn2 123.84(18) . .
C8 O14 Zn2 116.6(2) 3_631 .
C8 O15 Zn1 140.1(2) 3_631 .
C15 O16 Zn3 115.58(17) 3_531 .
Zn3 O17 Zn1 116.93(8) . .
Zn3 O17 Zn2 111.82(8) . .
Zn1 O17 Zn2 104.16(8) . .
C23 O18 Zn3 129.6(2) 3_531 .
C23 O18 Zn3 122.88(19) 3_531 3_531
Zn3 O18 Zn3 107.02(10) . 3_531
O1 C1 O2 121.3(2) . .
O1 C1 C2 120.0(2) . .
O2 C1 C2 118.6(2) . .
C3 C2 C7 119.6(2) . .
C3 C2 C1 118.7(2) . .
C7 C2 C1 121.5(2) . .
C4 C3 C2 121.2(3) . .
C3 C4 C5 119.8(3) . .
C6 C5 C4 119.8(3) . .
C6 C5 C8 120.2(3) . .
C4 C5 C8 119.8(3) . .
C5 C6 C7 120.5(3) . .
O3 C7 C2 123.0(2) . .
O3 C7 C6 118.0(2) . .
C2 C7 C6 119.0(3) . .
O15 C8 O14 126.5(3) 3_631 3_631
O15 C8 C5 115.3(3) 3_631 .
O14 C8 C5 118.2(3) 3_631 .
O4 C9 C14 122.2(2) . .
O4 C9 C10 117.9(2) . .
C14 C9 C10 119.8(2) . .
C11 C10 C9 120.3(2) . .
C10 C11 C12 120.8(2) . .
C10 C11 C25 119.2(2) . 4_545
C12 C11 C25 120.0(2) . 4_545
C13 C12 C11 119.1(3) . .
C12 C13 C14 121.4(2) . .
C13 C14 C9 118.6(2) . .
C13 C14 C15 118.8(2) . .
C9 C14 C15 122.6(2) . .
O16 C15 O5 121.0(2) 3_531 .
O16 C15 C14 118.7(2) 3_531 .
O5 C15 C14 120.3(2) . .
O6 C16 C17 118.0(2) . .
O6 C16 C21 123.4(2) . .
C17 C16 C21 118.6(2) . .
C18 C17 C16 121.2(2) . .
C17 C18 C19 120.1(2) . .
C17 C18 C24 120.0(2) . 4_535
C19 C18 C24 119.9(3) . 4_535
C20 C19 C18 119.4(3) . .
C19 C20 C21 121.1(3) . .
C20 C21 C16 119.4(2) . .
C20 C21 C22 119.3(2) . .
C16 C21 C22 121.2(3) . .
O8 C22 O7 119.0(2) . .
O8 C22 C21 121.0(2) . .
O7 C22 C21 120.0(2) . .
O9 C23 O18 124.6(3) . 3_531
O11 C24 O10 127.3(2) . .
O11 C24 C18 117.0(2) . 4_536
O10 C24 C18 115.7(2) . 4_536
O12 C25 O13 126.5(2) . .
O12 C25 C11 116.3(2) . 4_546
O13 C25 C11 117.2(2) . 4_546
C1S N1S C2S 97.2(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O10 1.9696(19) .
Zn1 O17 2.0076(18) .
Zn1 O15 2.059(2) .
Zn1 O8 2.063(2) .
Zn1 O9 2.162(2) .
Zn1 O7 2.4520(18) .
Zn2 O13 1.9510(19) .
Zn2 O14 1.972(2) .
Zn2 O17 2.0146(19) .
Zn2 O11 2.0541(19) .
Zn2 O1 2.233(2) .
Zn3 O17 1.9786(17) .
Zn3 O16 1.9817(19) .
Zn3 O18 2.006(2) .
Zn3 O12 2.008(2) .
Zn3 O18 2.192(2) 3_531
Ti1 O4 1.8677(18) .
Ti1 O6 1.870(2) .
Ti1 O3 1.8852(19) .
Ti1 O2 2.0086(19) .
Ti1 O5 2.0168(19) .
Ti1 O7 2.0351(18) .
O1 C1 1.239(3) .
O2 C1 1.294(3) .
O3 C7 1.343(3) .
O4 C9 1.333(3) .
O5 C15 1.284(3) .
O6 C16 1.326(3) .
O7 C22 1.286(3) .
O8 C22 1.252(3) .
O9 C23 1.224(4) .
O10 C24 1.260(3) .
O11 C24 1.251(4) .
O12 C25 1.252(3) .
O13 C25 1.264(3) .
O14 C8 1.244(4) 3_631
O15 C8 1.243(4) 3_631
O16 C15 1.255(3) 3_531
O18 C23 1.275(4) 3_531
O18 Zn3 2.191(2) 3_531
C1 C2 1.499(3) .
C2 C3 1.389(4) .
C2 C7 1.406(4) .
C3 C4 1.367(4) .
C4 C5 1.411(5) .
C5 C6 1.375(4) .
C5 C8 1.527(4) .
C6 C7 1.409(4) .
C8 O15 1.242(4) 3_631
C8 O14 1.244(4) 3_631
C9 C14 1.404(3) .
C9 C10 1.404(3) .
C10 C11 1.374(4) .
C11 C12 1.396(4) .
C11 C25 1.505(4) 4_545
C12 C13 1.386(4) .
C13 C14 1.402(4) .
C14 C15 1.478(3) .
C15 O16 1.255(3) 3_531
C16 C17 1.400(3) .
C16 C21 1.407(3) .
C17 C18 1.369(4) .
C18 C19 1.394(4) .
C18 C24 1.501(4) 4_535
C19 C20 1.383(4) .
C20 C21 1.388(4) .
C21 C22 1.472(3) .
C23 O18 1.275(4) 3_531
C24 C18 1.501(4) 4_536
C25 C11 1.505(3) 4_546
N1S C1S 1.540(13) .
N1S C2S 1.663(15) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.177 0.085 0.353 2476.1 216.4
