#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:56:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178761 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/15/4101539.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_4101539
loop_
_publ_author_name
'Dinca, Mircea'
'Yu, Anta F'
'Long, Jeffrey R'
_publ_section_title
;
 Microporous metal-organic frameworks incorporating
 1,4-benzeneditetrazolate: syntheses, structures, and hydrogen storage
 properties.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8904
_journal_page_last               8913
_journal_paper_doi               10.1021/ja061716i
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C40 H55 N29 O8 Zn3'
_chemical_formula_sum            'C40 H55 N29 O8 Zn3'
_chemical_formula_weight         1266.24
_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           SHELXL-97
_cell_angle_alpha                92.869(13)
_cell_angle_beta                 114.443(14)
_cell_angle_gamma                107.988(15)
_cell_formula_units_Z            1
_cell_length_a                   11.5713(19)
_cell_length_b                   11.736(2)
_cell_length_c                   13.619(2)
_cell_measurement_reflns_used    2548
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      48.395
_cell_measurement_theta_min      4.869
_cell_volume                     1567.4(5)
_computing_cell_refinement       'Bruker SAINT v7.07b'
_computing_data_collection       'Bruker SMART v5.054d'
_computing_data_reduction        'Bruker SAINT v7.07b'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       ω/2θ-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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10219
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.535982
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.343
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1460P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2028
_refine_ls_wR_factor_ref         0.2155
_reflns_number_gt                4513
_reflns_number_total             6228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061716isi20060312_073443.cif
_cod_data_source_block           md25f
_cod_database_code               4101539
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 0.0000 0.5000 0.0000 0.0175(2) Uani 1 2 d S
Zn2 Zn -0.10439(6) 0.76608(5) 0.04639(5) 0.0248(2) Uani 1 1 d .
O3 O -0.2840(4) 0.7284(4) 0.0683(4) 0.0462(11) Uani 1 1 d .
O1 O -0.1605(4) 0.8805(3) -0.0640(3) 0.0325(9) Uani 1 1 d .
O2 O -0.0130(5) 0.9202(4) 0.1676(4) 0.0426(10) Uani 1 1 d .
O4 O -0.544(2) 1.1575(19) 0.2535(16) 0.139(6) Uiso 0.50 1 d P
O5 O -0.3043(11) 0.2116(9) -0.3078(8) 0.126(3) Uiso 1 1 d .
C18 C -0.4856(16) 0.6295(14) 0.1389(13) 0.054(4) Uiso 0.50 1 d P
C18A C -0.5190(15) 0.5864(13) 0.0828(12) 0.048(3) Uiso 0.50 1 d P
C17 C -0.351(2) 0.738(2) 0.3098(18) 0.087(6) Uiso 0.50 1 d P
C17A C -0.656(3) 0.578(2) -0.133(2) 0.110(7) Uiso 0.50 1 d P
C16 C -0.2688(10) 0.7638(9) 0.1716(8) 0.027(2) Uiso 0.50 1 d P
C16A C -0.4111(19) 0.6846(17) -0.0333(15) 0.075(5) Uiso 0.50 1 d P
C9 C 0.2630(5) 0.8492(4) 0.0158(4) 0.0241(10) Uani 1 1 d .
C15 C 0.0896(15) 1.1426(10) 0.2946(12) 0.127(5) Uani 1 1 d .
H15A H 0.0076 1.1081 0.2265 0.190 Uiso 1 1 calc R
H15B H 0.1448 1.2202 0.2899 0.190 Uiso 1 1 calc R
H15C H 0.0667 1.1539 0.3537 0.190 Uiso 1 1 calc R
C14 C 0.2965(17) 1.0920(16) 0.4064(11) 0.191(9) Uani 1 1 d .
H14A H 0.2981 1.1259 0.4728 0.287 Uiso 1 1 calc R
H14B H 0.3633 1.1504 0.3917 0.287 Uiso 1 1 calc R
H14C H 0.3167 1.0186 0.4150 0.287 Uiso 1 1 calc R
C5 C -0.0272(5) 0.5578(5) 0.2919(4) 0.0283(11) Uani 1 1 d .
C1 C -0.3291(5) 0.5387(5) -0.2679(5) 0.0297(12) Uani 1 1 d .
C21 C -0.302(2) 1.193(2) 0.4493(18) 0.195(8) Uiso 1 1 d .
C6 C -0.0137(6) 0.5287(5) 0.3986(4) 0.0304(12) Uani 1 1 d .
C22 C -0.402(2) 0.1739(17) -0.3136(16) 0.176(7) Uiso 1 1 d .
H22A H -0.4260 0.2376 -0.2895 0.265 Uiso 1 1 calc R
H22B H -0.4036 0.1143 -0.2680 0.265 Uiso 1 1 calc R
H22C H -0.4664 0.1352 -0.3888 0.265 Uiso 1 1 calc R
C20 C -0.252(3) 1.162(3) 0.302(3) 0.295(14) Uiso 1 1 d .
C2 C -0.4185(5) 0.5170(5) -0.3872(5) 0.0313(12) Uani 1 1 d .
C12 C 0.3968(7) 1.0409(6) -0.0146(9) 0.080(3) Uani 1 1 d .
H12 H 0.3277 1.0707 -0.0250 0.096 Uiso 1 1 calc R
C8 C -0.0708(6) 0.5747(5) 0.4550(5) 0.0390(14) Uani 1 1 d .
H8 H -0.1195 0.6246 0.4250 0.047 Uiso 1 1 calc R
C4 C -0.4114(6) 0.4390(6) -0.4622(5) 0.0429(15) Uani 1 1 d .
H4 H -0.3512 0.3977 -0.4372 0.051 Uiso 1 1 calc R
C7 C 0.0552(6) 0.4536(6) 0.4436(5) 0.0390(14) Uani 1 1 d .
H7 H 0.0923 0.4209 0.4056 0.047 Uiso 1 1 calc R
C10 C 0.3854(5) 0.9275(5) 0.0088(5) 0.0284(11) Uani 1 1 d .
C3 C -0.5077(6) 0.5781(6) -0.4270(5) 0.0413(14) Uani 1 1 d .
H3 H -0.5130 0.6317 -0.3777 0.050 Uiso 1 1 calc R
C11 C 0.4871(7) 0.8875(6) 0.0229(9) 0.078(3) Uani 1 1 d .
H11 H 0.4802 0.8102 0.0386 0.094 Uiso 1 1 calc R
C13 C 0.0956(12) 0.9540(8) 0.2397(8) 0.076(3) Uani 1 1 d .
H13 H 0.1435 0.9016 0.2479 0.092 Uiso 1 1 calc R
N14 N -0.3649(10) 0.7137(9) 0.2000(8) 0.038(2) Uiso 0.50 1 d P
N14A N -0.5214(19) 0.6132(17) -0.0226(15) 0.098(5) Uiso 0.50 1 d P
N4 N -0.3016(4) 0.6363(4) -0.1955(4) 0.0307(10) Uani 1 1 d .
N12 N 0.1703(4) 0.8873(3) 0.0278(4) 0.0252(9) Uani 1 1 d .
N6 N -0.0558(4) 0.6468(4) 0.1576(4) 0.0258(9) Uani 1 1 d .
N8 N -0.0141(4) 0.4895(4) 0.2190(3) 0.0259(9) Uani 1 1 d .
N3 N -0.2100(4) 0.6258(4) -0.0998(4) 0.0271(9) Uani 1 1 d .
N7 N -0.0326(4) 0.5473(3) 0.1355(3) 0.0224(9) Uani 1 1 d .
N11 N 0.0795(4) 0.7871(3) 0.0295(3) 0.0226(9) Uani 1 1 d .
N10 N 0.1153(4) 0.6927(3) 0.0193(3) 0.0204(8) Uani 1 1 d .
N2 N -0.1851(4) 0.5252(3) -0.1142(3) 0.0241(9) Uani 1 1 d .
N9 N 0.2309(4) 0.7282(3) 0.0107(4) 0.0233(9) Uani 1 1 d .
N5 N -0.0534(5) 0.6560(4) 0.2567(4) 0.0334(11) Uani 1 1 d .
N15 N -0.355(4) 1.184(3) 0.315(3) 0.193(12) Uiso 0.50 1 d P
N13 N 0.1619(11) 1.0633(7) 0.3148(8) 0.102(3) Uani 1 1 d .
N1 N -0.2601(4) 0.4677(4) -0.2202(4) 0.0270(9) Uani 1 1 d .
N15A N -0.224(4) 1.130(3) 0.406(3) 0.189(12) Uiso 0.50 1 d P
O4A O -0.056(2) 1.040(2) 0.4702(19) 0.166(8) Uiso 0.50 1 d P
O6 O -0.281(5) 0.797(4) 0.330(4) 0.32(2) Uiso 0.50 1 d P
C19 C -0.480(4) 1.082(3) 0.274(3) 0.158(12) Uiso 0.50 1 d P
C19A C -0.072(3) 1.124(3) 0.545(2) 0.255(11) Uiso 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'
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
N7 Zn1 N7 180.00(9) . 2_565
N7 Zn1 N10 90.99(15) . 2_565
N7 Zn1 N10 89.01(15) 2_565 2_565
N7 Zn1 N10 89.01(15) . .
N7 Zn1 N10 90.99(15) 2_565 .
N10 Zn1 N10 180.0 2_565 .
N7 Zn1 N2 88.90(16) . 2_565
N7 Zn1 N2 91.10(16) 2_565 2_565
N10 Zn1 N2 89.50(14) 2_565 2_565
N10 Zn1 N2 90.50(14) . 2_565
N7 Zn1 N2 91.10(16) . .
N7 Zn1 N2 88.90(16) 2_565 .
N10 Zn1 N2 90.50(14) 2_565 .
N10 Zn1 N2 89.50(14) . .
N2 Zn1 N2 180.0 2_565 .
O2 Zn2 O1 85.85(17) . .
O2 Zn2 O3 88.74(18) . .
O1 Zn2 O3 92.36(15) . .
O2 Zn2 N6 94.75(18) . .
O1 Zn2 N6 177.64(15) . .
O3 Zn2 N6 85.37(15) . .
O2 Zn2 N3 169.87(17) . .
O1 Zn2 N3 84.02(15) . .
O3 Zn2 N3 91.62(17) . .
N6 Zn2 N3 95.37(16) . .
O2 Zn2 N11 93.89(17) . .
O1 Zn2 N11 93.03(15) . .
O3 Zn2 N11 174.16(14) . .
N6 Zn2 N11 89.21(15) . .
N3 Zn2 N11 86.70(15) . .
C16 O3 C16A 126.3(9) . .
C16 O3 Zn2 118.0(5) . .
C16A O3 Zn2 114.9(8) . .
C13 O2 Zn2 127.2(6) . .
C18A C18 N14 135(2) . .
C18 C18A N14A 130(2) . .
C18 C18A N14 29.0(15) . .
N14A C18A N14 107.8(11) . .
O6 C17 N14 93(4) . .
N14 C16 O3 121.3(9) . .
N14A C16A O3 114.6(15) . .
N9 C9 N12 111.4(4) . .
N9 C9 C10 122.9(4) . .
N12 C9 C10 125.7(4) . .
N8 C5 N5 112.3(4) . .
N8 C5 C6 123.5(5) . .
N5 C5 C6 124.1(5) . .
N4 C1 N1 111.9(5) . .
N4 C1 C2 123.5(5) . .
N1 C1 C2 124.4(5) . .
N15A C21 N15 68(2) . .
C7 C6 C8 118.8(5) . .
C7 C6 C5 119.9(5) . .
C8 C6 C5 121.3(5) . .
N15 C20 N15A 82(3) . .
C3 C2 C4 118.3(5) . .
C3 C2 C1 120.7(5) . .
C4 C2 C1 121.0(5) . .
C10 C12 C11 119.8(6) . 2_675
C6 C8 C7 120.0(5) . 2_566
C3 C4 C2 120.6(5) 2_464 .
C6 C7 C8 121.2(5) . 2_566
C11 C10 C12 118.4(5) . .
C11 C10 C9 120.7(5) . .
C12 C10 C9 121.0(5) . .
C4 C3 C2 121.1(6) 2_464 .
C10 C11 C12 121.8(5) . 2_675
O2 C13 N13 127.2(10) . .
C16 N14 C18 128.0(11) . .
C16 N14 C17 124.3(13) . .
C18 N14 C17 107.6(14) . .
C16 N14 O6 95.9(18) . .
C18 N14 O6 136(2) . .
C17 N14 O6 29.0(18) . .
C16 N14 C18A 111.9(9) . .
C18 N14 C18A 16.4(8) . .
C17 N14 C18A 123.3(12) . .
O6 N14 C18A 152.1(18) . .
C16A N14A C18A 124.5(16) . .
C16A N14A C17A 111.4(17) . .
C18A N14A C17A 123.7(17) . .
C1 N4 N3 104.4(4) . .
N11 N12 C9 104.7(4) . .
N7 N6 N5 109.5(4) . .
N7 N6 Zn2 124.8(3) . .
N5 N6 Zn2 125.5(3) . .
N7 N8 C5 104.5(4) . .
N2 N3 N4 109.8(4) . .
N2 N3 Zn2 126.6(3) . .
N4 N3 Zn2 123.2(3) . .
N6 N7 N8 109.8(4) . .
N6 N7 Zn1 125.6(3) . .
N8 N7 Zn1 124.1(3) . .
N10 N11 N12 109.6(3) . .
N10 N11 Zn2 121.3(3) . .
N12 N11 Zn2 129.1(3) . .
N11 N10 N9 110.3(3) . .
N11 N10 Zn1 127.8(3) . .
N9 N10 Zn1 121.5(3) . .
N3 N2 N1 109.2(4) . .
N3 N2 Zn1 122.3(3) . .
N1 N2 Zn1 124.7(3) . .
N10 N9 C9 104.0(4) . .
N6 N5 C5 103.9(4) . .
C20 N15 C19 116(3) . .
C20 N15 C21 102(3) . .
C19 N15 C21 100(3) . .
C20 N15 N15A 50(2) . .
C19 N15 N15A 106(3) . .
C21 N15 N15A 54.0(16) . .
C13 N13 C15 114.4(11) . .
C13 N13 C14 121.7(12) . .
C15 N13 C14 123.9(11) . .
C1 N1 N2 104.6(4) . .
C20 N15A C21 103(3) . .
C20 N15A N15 48(2) . .
C21 N15A N15 57.6(18) . .
C19A O4A O4A 118(2) . 2_576
C17 O6 N14 59(4) . .
O4 C19 N15 89(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N7 2.111(4) .
Zn1 N7 2.111(4) 2_565
Zn1 N10 2.180(4) 2_565
Zn1 N10 2.180(4) .
Zn1 N2 2.185(4) 2_565
Zn1 N2 2.185(4) .
Zn2 O2 2.047(4) .
Zn2 O1 2.102(4) .
Zn2 O3 2.136(4) .
Zn2 N6 2.136(4) .
Zn2 N3 2.141(4) .
Zn2 N11 2.174(4) .
O3 C16 1.370(11) .
O3 C16A 1.455(19) .
O2 C13 1.154(11) .
O4 C19 1.29(4) .
O5 C22 1.047(19) .
C18 C18A 0.766(16) .
C18 N14 1.313(18) .
C18A N14A 1.47(2) .
C18A N14 1.929(18) .
C17 O6 0.82(5) .
C17 N14 1.44(2) .
C17A N14A 1.57(3) .
C16 N14 1.306(14) .
C16A N14A 1.36(2) .
C9 N9 1.342(6) .
C9 N12 1.347(6) .
C9 C10 1.475(7) .
C15 N13 1.399(15) .
C14 N13 1.457(18) .
C5 N8 1.330(6) .
C5 N5 1.342(6) .
C5 C6 1.465(7) .
C1 N4 1.337(7) .
C1 N1 1.337(6) .
C1 C2 1.477(8) .
C21 N15A 1.59(4) .
C21 N15 1.66(3) .
C6 C7 1.369(8) .
C6 C8 1.385(7) .
C20 N15 1.37(4) .
C20 N15A 1.42(4) .
C2 C3 1.380(8) .
C2 C4 1.382(8) .
C12 C10 1.364(8) .
C12 C11 1.400(8) 2_675
C8 C7 1.388(8) 2_566
C4 C3 1.371(9) 2_464
C7 C8 1.388(8) 2_566
C10 C11 1.344(8) .
C3 C4 1.371(9) 2_464
C11 C12 1.400(8) 2_675
C13 N13 1.375(11) .
N14 O6 1.69(5) .
N4 N3 1.338(6) .
N12 N11 1.322(5) .
N6 N7 1.324(5) .
N6 N5 1.336(6) .
N8 N7 1.329(6) .
N3 N2 1.323(5) .
N11 N10 1.317(5) .
N10 N9 1.330(5) .
N2 N1 1.340(6) .
N15 C19 1.42(4) .
N15 N15A 1.83(5) .
O4A C19A 1.49(3) .
O4A O4A 1.77(4) 2_576
