#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:46:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179393 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/90/4329014.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_4329014
loop_
_publ_author_name
'Zhangjing Zhang'
'Shengchang Xiang'
'Kunlun Hong'
'Madhab, C. Das'
'Hadi D. Arman'
'Maya Garcia'
'Jalal U. Mondal'
'K. Mark Thomas'
'Banglin Chen'
_publ_section_title
;
 Triple Framework Interpenetration and Immobilization of Open Metal Sites
 within a Microporous Mixed Metal-Organic Framework for Highly Selective
 Gas Adsorption
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4947
_journal_page_last               4953
_journal_paper_doi               10.1021/ic2021275
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C44 H32 Cu N4 O10 Zn2'
_chemical_formula_weight         971.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 129.76(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.564(4)
_cell_length_b                   20.405(4)
_cell_length_c                   14.919(3)
_cell_measurement_temperature    173(2)
_cell_volume                     5280(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Saturn724 (2x2 bin mode)'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.1150
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14954
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_T_max  0.8768
_exptl_absorpt_correction_T_min  0.7288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         2.171
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4794
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0829
_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)+(0.1372P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2185
_refine_ls_wR_factor_ref         0.2447
_reflns_number_gt                3367
_reflns_number_total             4794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2021275_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        5280.4(28)
_cod_database_code               4329014
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_group
Zn1 Zn -0.44560(3) 0.80450(2) -0.62112(5) 0.0308(3) Uani 1 1 d . .
O1 O -0.3965(2) 0.72913(18) -0.6403(4) 0.0516(10) Uani 1 1 d . .
O2 O -0.4666(2) 0.74397(19) -0.8316(4) 0.0559(11) Uani 1 1 d . .
O3 O -0.0139(2) 0.38091(17) -0.6519(3) 0.0466(9) Uani 1 1 d . .
O4 O -0.1086(2) 0.36579(17) -0.8439(3) 0.0448(9) Uani 1 1 d . .
C1 C -0.4122(3) 0.7174(3) -0.7369(5) 0.0437(13) Uani 1 1 d . .
C2 C -0.3640(4) 0.6692(3) -0.7382(5) 0.0511(14) Uani 1 1 d . .
C3 C -0.2990(4) 0.6411(3) -0.6337(5) 0.0585(16) Uani 1 1 d . .
H3A H -0.2861 0.6532 -0.5615 0.070 Uiso 1 1 calc R .
C4 C -0.2538(4) 0.5959(3) -0.6352(5) 0.0581(17) Uani 1 1 d . .
H4A H -0.2113 0.5763 -0.5643 0.070 Uiso 1 1 calc R .
C5 C -0.2699(3) 0.5787(3) -0.7399(5) 0.0529(15) Uani 1 1 d . .
C6 C -0.3314(4) 0.6094(4) -0.8414(6) 0.075(2) Uani 1 1 d . .
H6A H -0.3419 0.5996 -0.9126 0.090 Uiso 1 1 calc R .
C7 C -0.3788(4) 0.6547(4) -0.8418(6) 0.076(2) Uani 1 1 d . .
H7A H -0.4206 0.6751 -0.9125 0.091 Uiso 1 1 calc R .
C8 C -0.2209(3) 0.5321(3) -0.7429(5) 0.0500(14) Uani 1 1 d . .
C9 C -0.1452(4) 0.5176(3) -0.6401(6) 0.075(2) Uani 1 1 d . .
H9A H -0.1253 0.5386 -0.5689 0.090 Uiso 1 1 calc R .
C10 C -0.1003(4) 0.4733(3) -0.6426(6) 0.070(2) Uani 1 1 d . .
H10A H -0.0499 0.4636 -0.5728 0.084 Uiso 1 1 calc R .
C11 C -0.1280(3) 0.4424(2) -0.7465(4) 0.0385(12) Uani 1 1 d . .
C12 C -0.2028(3) 0.4549(3) -0.8455(5) 0.0610(18) Uani 1 1 d . .
H12A H -0.2237 0.4322 -0.9158 0.073 Uiso 1 1 calc R .
C13 C -0.2478(3) 0.5005(3) -0.8435(5) 0.0642(19) Uani 1 1 d . .
H13A H -0.2982 0.5099 -0.9134 0.077 Uiso 1 1 calc R .
C14 C -0.0796(3) 0.3930(2) -0.7477(5) 0.0373(11) Uani 1 1 d . .
Cu1 Cu -0.2238(2) 0.71920(17) 0.0008(2) 0.1522(17) Uani 0.50 1 d PU .
N1 N -0.3853(3) 0.7968(2) -0.4494(4) 0.0419(11) Uani 1 1 d U .
O21 O -0.2518(10) 0.7576(8) -0.0988(11) 0.139(7) Uani 0.541(15) 1 d PU 1
O21A O -0.2967(13) 0.7839(9) -0.1131(15) 0.140(9) Uani 0.459(15) 1 d PU 2
C21 C -0.4076(6) 0.8259(5) -0.3970(7) 0.088(2) Uani 1 1 d U .
H21A H -0.4508 0.8545 -0.4420 0.105 Uiso 1 1 calc R .
C22 C -0.3723(9) 0.8176(6) -0.2796(10) 0.122(4) Uani 1 1 d U .
C23 C -0.3060(8) 0.7787(7) -0.2106(9) 0.129(4) Uani 1 1 d U .
C24 C -0.2836(6) 0.7457(4) -0.2669(7) 0.095(3) Uani 1 1 d U .
C25 C -0.3238(4) 0.7566(3) -0.3840(6) 0.0657(18) Uani 1 1 d U .
H25A H -0.3073 0.7345 -0.4206 0.079 Uiso 1 1 calc R .
C26 C -0.4082(10) 0.8608(7) -0.2374(12) 0.191(7) Uani 1 1 d U .
H26A H -0.3815 0.8560 -0.1556 0.229 Uiso 1 1 d R .
H26B H -0.4053 0.9056 -0.2540 0.229 Uiso 1 1 d R .
H26C H -0.4613 0.8485 -0.2812 0.229 Uiso 1 1 d R .
C27 C -0.2191(8) 0.7016(6) -0.2017(10) 0.142(5) Uani 1 1 d U .
H27A H -0.1994 0.6792 -0.2335 0.170 Uiso 1 1 calc R .
N2 N -0.1901(14) 0.6958(12) -0.0909(16) 0.174(11) Uani 0.50 1 d PU .
C28 C -0.122(2) 0.6539(18) -0.021(2) 0.246(18) Uani 0.50 1 d PU .
H28A H -0.0751 0.6806 0.0331 0.295 Uiso 0.50 1 calc PR .
H28B H -0.1167 0.6285 -0.0720 0.295 Uiso 0.50 1 calc PR .
N3 N -0.1505(16) 0.6534(13) 0.1073(18) 0.199(14) Uani 0.50 1 d PU .
C29 C -0.1352(17) 0.6046(15) 0.0514(19) 0.208(14) Uani 0.50 1 d PU .
H29A H -0.1797 0.5751 -0.0011 0.250 Uiso 0.50 1 calc PR .
H29B H -0.0885 0.5784 0.1095 0.250 Uiso 0.50 1 calc PR .
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'
Cu Cu 0.3201 1.2651 '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
N1 Zn1 O1 97.85(18) . .
N1 Zn1 O3 98.44(18) . 3_455
O1 Zn1 O3 163.67(17) . 3_455
N1 Zn1 O4 110.41(17) . 4_453
O1 Zn1 O4 87.60(17) . 4_453
O3 Zn1 O4 87.89(16) 3_455 4_453
N1 Zn1 O2 96.33(19) . 2_453
O1 Zn1 O2 89.41(18) . 2_453
O3 Zn1 O2 87.59(17) 3_455 2_453
O4 Zn1 O2 153.25(17) 4_453 2_453
N1 Zn1 Zn1 170.90(14) . 2_453
O1 Zn1 Zn1 83.70(12) . 2_453
O3 Zn1 Zn1 80.02(11) 3_455 2_453
O4 Zn1 Zn1 78.57(11) 4_453 2_453
O2 Zn1 Zn1 74.67(13) 2_453 2_453
C1 O1 Zn1 121.6(3) . .
C1 O2 Zn1 133.1(4) . 2_453
C14 O3 Zn1 125.4(3) . 3_545
C14 O4 Zn1 127.0(3) . 4_443
O2 C1 O1 124.0(5) . .
O2 C1 C2 118.1(5) . .
O1 C1 C2 117.9(5) . .
C7 C2 C3 118.9(5) . .
C7 C2 C1 120.2(5) . .
C3 C2 C1 120.8(5) . .
C4 C3 C2 120.6(5) . .
C3 C4 C5 121.0(5) . .
C6 C5 C4 117.9(5) . .
C6 C5 C8 120.1(6) . .
C4 C5 C8 121.9(5) . .
C5 C6 C7 121.8(6) . .
C2 C7 C6 119.6(6) . .
C13 C8 C9 118.1(5) . .
C13 C8 C5 121.3(5) . .
C9 C8 C5 120.6(5) . .
C10 C9 C8 120.5(5) . .
C9 C10 C11 120.8(5) . .
C12 C11 C10 118.5(5) . .
C12 C11 C14 120.9(5) . .
C10 C11 C14 120.4(5) . .
C11 C12 C13 120.6(5) . .
C8 C13 C12 121.4(5) . .
O3 C14 O4 125.4(4) . .
O3 C14 C11 117.2(4) . .
O4 C14 C11 117.3(4) . .
O21 Cu1 O21A 147.8(8) . 7_465
O21 Cu1 Cu1 75.0(7) . 7_465
O21A Cu1 Cu1 75.6(7) 7_465 7_465
O21 Cu1 O21 120.5(5) . 7_465
O21A Cu1 O21 32.1(7) 7_465 7_465
Cu1 Cu1 O21 45.5(4) 7_465 7_465
O21 Cu1 N3 145.1(9) . .
O21A Cu1 N3 62.4(8) 7_465 .
Cu1 Cu1 N3 138.0(6) 7_465 .
O21 Cu1 N3 93.3(7) 7_465 .
O21 Cu1 O21A 31.6(7) . .
O21A Cu1 O21A 121.0(5) 7_465 .
Cu1 Cu1 O21A 45.4(5) 7_465 .
O21 Cu1 O21A 90.2(5) 7_465 .
N3 Cu1 O21A 176.5(7) . .
O21 Cu1 N2 61.7(8) . .
O21A Cu1 N2 144.3(9) 7_465 .
Cu1 Cu1 N2 136.5(5) 7_465 .
O21 Cu1 N2 175.8(9) 7_465 .
N3 Cu1 N2 84.0(7) . .
O21A Cu1 N2 92.5(7) . .
C21 N1 C25 116.9(6) . .
C21 N1 Zn1 121.6(5) . .
C25 N1 Zn1 121.2(4) . .
C23 O21 Cu1 154.8(17) . .
C23 O21 N2 110.4(12) . .
Cu1 O21 N2 75.0(8) . .
C23 O21 Cu1 112.5(12) . 7_465
Cu1 O21 Cu1 59.5(5) . 7_465
N2 O21 Cu1 134.3(8) . 7_465
C23 O21A Cu1 169.7(15) . 7_465
C23 O21A N3 117.7(12) . 7_465
Cu1 O21A N3 72.6(9) 7_465 7_465
C23 O21A Cu1 110.8(11) . .
Cu1 O21A Cu1 59.0(5) 7_465 .
N3 O21A Cu1 131.5(10) 7_465 .
N1 C21 C22 124.4(9) . .
C21 C22 C23 118.4(10) . .
C21 C22 C26 114.0(11) . .
C23 C22 C26 127.3(11) . .
O21A C23 O21 45.4(8) . .
O21A C23 C24 145.9(12) . .
O21 C23 C24 101.4(12) . .
O21A C23 C22 96.0(12) . .
O21 C23 C22 141.3(13) . .
C24 C23 C22 117.3(9) . .
C25 C24 C23 119.2(8) . .
C25 C24 C27 121.3(10) . .
C23 C24 C27 119.6(9) . .
N1 C25 C24 123.6(7) . .
N3 C26 C22 98.7(12) 7_465 .
N2 C27 C24 112.0(13) . .
C27 N2 C28 113.2(15) . .
C27 N2 O21 96.2(11) . .
C28 N2 O21 149.5(16) . .
C27 N2 Cu1 136.3(14) . .
C28 N2 Cu1 109.8(12) . .
O21 N2 Cu1 43.3(5) . .
N2 C28 C29 106(2) . .
C29 N3 C26 105.4(14) . 7_465
C29 N3 O21A 156.2(18) . 7_465
C26 N3 O21A 97.9(13) 7_465 7_465
C29 N3 Cu1 113.1(13) . .
C26 N3 Cu1 140.6(16) 7_465 .
O21A N3 Cu1 45.0(6) 7_465 .
N3 C29 C28 100(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 1.995(5) .
Zn1 O1 2.019(4) .
Zn1 O3 2.027(3) 3_455
Zn1 O4 2.036(3) 4_453
Zn1 O2 2.040(4) 2_453
Zn1 Zn1 2.9562(18) 2_453
O1 C1 1.268(7) .
O2 C1 1.256(7) .
O2 Zn1 2.040(4) 2_453
O3 C14 1.262(6) .
O3 Zn1 2.027(3) 3_545
O4 C14 1.264(6) .
O4 Zn1 2.036(3) 4_443
C1 C2 1.475(7) .
C2 C7 1.390(9) .
C2 C3 1.410(8) .
C3 C4 1.385(8) .
C4 C5 1.403(8) .
C5 C6 1.387(8) .
C5 C8 1.481(8) .
C6 C7 1.410(8) .
C8 C13 1.368(8) .
C8 C9 1.416(8) .
C9 C10 1.375(8) .
C10 C11 1.397(8) .
C11 C12 1.380(7) .
C11 C14 1.494(6) .
C12 C13 1.392(8) .
Cu1 O21 1.420(12) .
Cu1 O21A 1.427(14) 7_465
Cu1 Cu1 1.716(4) 7_465
Cu1 O21 1.923(15) 7_465
Cu1 N3 1.924(17) .
Cu1 O21A 1.939(15) .
Cu1 N2 2.001(17) .
N1 C21 1.312(9) .
N1 C25 1.350(8) .
O21 C23 1.362(15) .
O21 N2 1.82(2) .
O21 Cu1 1.923(15) 7_465
O21A C23 1.335(17) .
O21A Cu1 1.427(14) 7_465
O21A N3 1.79(2) 7_465
C21 C22 1.395(12) .
C22 C23 1.399(16) .
C22 C26 1.575(15) .
C23 C24 1.398(15) .
C24 C25 1.376(10) .
C24 C27 1.437(14) .
C26 N3 1.52(2) 7_465
C27 N2 1.340(19) .
N2 C28 1.46(3) .
C28 C29 1.63(4) .
N3 C29 1.47(3) .
N3 C26 1.52(2) 7_465
N3 O21A 1.79(2) 7_465
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
_platon_squeeze_void_content
1 0.000 0.000 -0.010 839 166 ' '
2 0.500 0.500 -0.039 839 166 ' '
3 0.500 0.011 0.250 14 2 ' '
4 1.000 0.511 0.250 14 2 ' '
5 1.000 0.489 0.750 14 4 ' '
6 0.500 0.989 0.750 14 4 ' '
