#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:43:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179344 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/41/4324194.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_4324194
loop_
_publ_author_name
'Zeric Hulvey'
'Dorina A. Sava'
'Juergen Eckert'
'Anthony K. Cheetham'
_publ_section_title
;
 Hydrogen Storage in a Highly Interpenetrated and Partially Fluorinated
 Metal-Organic Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              403
_journal_page_last               405
_journal_paper_doi               10.1021/ic101153c
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C60 H36 F12 N6 O12 Zn3'
_chemical_formula_weight         1457.12
_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                102.902(4)
_cell_angle_beta                 110.679(4)
_cell_angle_gamma                107.159(4)
_cell_formula_units_Z            1
_cell_length_a                   10.395(3)
_cell_length_b                   11.790(3)
_cell_length_c                   13.331(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1359.0(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      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11299
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         5332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0698
_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)+(0.0834P)²+0.9489P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1768
_reflns_number_gt                3151
_reflns_number_total             5332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101153c_si_002_1.cif
_cod_data_source_block           compound_1
_cod_database_code               4324194
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 0.5000 0.5000 0.5000 0.0258(3) Uani 1 2 d S
Zn2 Zn 0.44993(7) 0.67162(6) 0.24741(6) 0.0288(2) Uani 1 1 d .
C1 C 0.2624(6) 0.6047(6) 0.3693(5) 0.0291(14) Uani 1 1 d .
C2 C 0.1136(6) 0.5891(5) 0.3734(5) 0.0289(14) Uani 1 1 d .
C3 C -0.0238(6) 0.5108(6) 0.2799(6) 0.0330(15) Uani 1 1 d .
C4 C 0.1092(7) 0.6598(7) 0.4680(6) 0.0421(17) Uani 1 1 d .
C5 C -0.1569(6) 0.5085(6) 0.2794(5) 0.0345(15) Uani 1 1 d .
C6 C -0.0250(7) 0.6573(7) 0.4671(5) 0.0400(16) Uani 1 1 d .
C7 C -0.1621(6) 0.5833(6) 0.3715(5) 0.0306(14) Uani 1 1 d .
C8 C -0.3067(6) 0.5936(5) 0.3644(5) 0.0299(14) Uani 1 1 d .
C9 C 0.4159(8) 0.8365(6) 0.1246(6) 0.0391(16) Uani 1 1 d .
C10 C 0.4596(7) 0.9178(6) 0.0584(6) 0.0359(15) Uani 1 1 d .
C11 C 0.3606(6) 0.9073(6) -0.0481(6) 0.0388(16) Uani 1 1 d .
C12 C 0.6028(7) 1.0148(6) 0.1048(5) 0.0377(16) Uani 1 1 d .
C13 C 0.4239(7) 0.2819(6) 0.2847(6) 0.0390(16) Uani 1 1 d .
H13 H 0.5281 0.3111 0.3145 0.05(2) Uiso 1 1 calc R
C14 C 0.2172(7) 0.2953(6) 0.2991(6) 0.0431(17) Uani 1 1 d .
H14 H 0.1745 0.3349 0.3382 0.038(18) Uiso 1 1 calc R
C15 C 0.3368(7) 0.1808(6) 0.1827(6) 0.0415(17) Uani 1 1 d .
H15 H 0.3826 0.1443 0.1445 0.031(16) Uiso 1 1 calc R
C16 C 0.1243(7) 0.1940(7) 0.1996(6) 0.0438(17) Uani 1 1 d .
H16 H 0.0205 0.1651 0.1734 0.05(2) Uiso 1 1 calc R
C17 C 0.1811(7) 0.1319(6) 0.1353(5) 0.0373(16) Uani 1 1 d .
C18 C 0.0862(7) 0.0197(6) 0.0242(6) 0.0429(17) Uani 1 1 d .
H18A H 0.1072 -0.0527 0.0353 0.05(2) Uiso 1 1 calc R
H18B H 0.1167 0.0389 -0.0331 0.037(18) Uiso 1 1 calc R
C19 C 0.3700(7) 0.4293(6) 0.0503(6) 0.0418(17) Uani 1 1 d .
H19 H 0.4743 0.4567 0.0844 0.05(2) Uiso 1 1 calc R
C20 C 0.1634(7) 0.4504(7) 0.0503(6) 0.0469(18) Uani 1 1 d .
H20 H 0.1184 0.4945 0.0829 0.07(3) Uiso 1 1 calc R
C21 C 0.2883(8) 0.3227(7) -0.0479(6) 0.0492(19) Uani 1 1 d .
H21 H 0.3361 0.2822 -0.0807 0.05(2) Uiso 1 1 calc R
C22 C 0.0718(7) 0.3436(7) -0.0453(6) 0.053(2) Uani 1 1 d .
H22 H -0.0323 0.3159 -0.0754 0.06(2) Uiso 1 1 calc R
C23 C 0.1329(8) 0.2764(7) -0.0974(6) 0.0473(19) Uani 1 1 d .
C24 C 0.0336(11) 0.1573(10) -0.2065(8) 0.089(4) Uani 1 1 d .
H24A H 0.0974 0.1371 -0.2394 0.15(5) Uiso 1 1 calc R
H24B H -0.0069 0.0871 -0.1843 0.32(12) Uiso 1 1 calc R
C25 C 0.7273(8) 0.9100(7) 0.4157(7) 0.064(2) Uani 1 1 d .
H25 H 0.7496 0.8875 0.3544 0.05(2) Uiso 1 1 calc R
C26 C 0.5712(10) 0.8744(7) 0.4923(7) 0.068(3) Uani 1 1 d .
H26 H 0.4780 0.8279 0.4869 0.10(3) Uiso 1 1 calc R
C27 C 0.8338(9) 1.0132(8) 0.5092(9) 0.090(4) Uani 1 1 d .
H27 H 0.9232 1.0602 0.5094 0.08(3) Uiso 1 1 calc R
C28 C 0.6734(13) 0.9756(8) 0.5928(7) 0.080(3) Uani 1 1 d .
H28 H 0.6492 0.9943 0.6536 0.05(2) Uiso 1 1 calc R
C29 C 0.8103(10) 1.0490(7) 0.6040(7) 0.064(3) Uani 1 1 d .
C30 C 0.9181(15) 1.1619(11) 0.7107(10) 0.136(6) Uani 1 1 d .
H30A H 0.9607 1.2300 0.6871 0.43(18) Uiso 1 1 calc R
H30B H 0.8595 1.1882 0.7462 0.18(6) Uiso 1 1 calc R
N1 N 0.3674(5) 0.3414(4) 0.3442(4) 0.0286(11) Uani 1 1 d .
N2 N 0.3138(5) 0.4970(5) 0.1009(4) 0.0325(12) Uani 1 1 d .
N3 N 0.5966(6) 0.8392(5) 0.4033(4) 0.0338(12) Uani 1 1 d .
F1 F -0.0297(4) 0.4370(4) 0.1848(3) 0.0518(11) Uani 1 1 d .
F2 F 0.2380(4) 0.7388(5) 0.5636(3) 0.0743(15) Uani 1 1 d .
F3 F -0.2867(4) 0.4290(4) 0.1836(3) 0.0535(11) Uani 1 1 d .
F4 F -0.0183(4) 0.7353(5) 0.5616(3) 0.0689(14) Uani 1 1 d .
F5 F 0.2206(4) 0.8132(4) -0.0993(4) 0.0587(12) Uani 1 1 d .
F6 F 0.7077(4) 1.0360(4) 0.2086(4) 0.0650(13) Uani 1 1 d .
O1 O 0.3559(5) 0.5900(4) 0.4460(4) 0.0480(12) Uani 1 1 d .
O2 O 0.2749(4) 0.6373(4) 0.2894(4) 0.0400(11) Uani 1 1 d .
O3 O -0.3419(5) 0.5809(5) 0.4415(4) 0.0498(13) Uani 1 1 d .
O4 O -0.3741(5) 0.6175(4) 0.2798(4) 0.0414(11) Uani 1 1 d .
O5 O 0.4904(5) 0.7723(4) 0.1506(4) 0.0384(11) Uani 1 1 d .
O6 O 0.3130(6) 0.8419(6) 0.1474(5) 0.0756(18) 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'
F F 0.0171 0.0103 '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 O1 180.000(1) . 2_666
O1 Zn1 N1 91.01(18) . .
O1 Zn1 N1 88.99(18) 2_666 .
O1 Zn1 N1 88.99(18) . 2_666
O1 Zn1 N1 91.01(18) 2_666 2_666
N1 Zn1 N1 180.000(1) . 2_666
O1 Zn1 O3 98.17(19) . 1_655
O1 Zn1 O3 81.83(19) 2_666 1_655
N1 Zn1 O3 92.43(18) . 1_655
N1 Zn1 O3 87.57(18) 2_666 1_655
O1 Zn1 O3 81.83(19) . 2_566
O1 Zn1 O3 98.17(19) 2_666 2_566
N1 Zn1 O3 87.57(18) . 2_566
N1 Zn1 O3 92.43(18) 2_666 2_566
O3 Zn1 O3 180.000(1) 1_655 2_566
O5 Zn2 O2 126.83(19) . .
O5 Zn2 O4 98.88(19) . 1_655
O2 Zn2 O4 134.27(19) . 1_655
O5 Zn2 N2 92.64(18) . .
O2 Zn2 N2 88.08(18) . .
O4 Zn2 N2 88.38(18) 1_655 .
O5 Zn2 N3 90.92(18) . .
O2 Zn2 N3 92.51(18) . .
O4 Zn2 N3 87.70(18) 1_655 .
N2 Zn2 N3 175.07(19) . .
O1 C1 O2 128.2(6) . .
O1 C1 C2 117.4(6) . .
O2 C1 C2 114.2(5) . .
C4 C2 C3 116.1(6) . .
C4 C2 C1 121.6(5) . .
C3 C2 C1 122.2(5) . .
F1 C3 C5 118.2(5) . .
F1 C3 C2 120.0(5) . .
C5 C3 C2 121.8(6) . .
F2 C4 C2 120.2(6) . .
F2 C4 C6 117.9(6) . .
C2 C4 C6 121.8(6) . .
F3 C5 C7 119.6(5) . .
F3 C5 C3 117.9(6) . .
C7 C5 C3 122.5(6) . .
F4 C6 C7 120.0(6) . .
F4 C6 C4 117.8(6) . .
C7 C6 C4 122.1(6) . .
C5 C7 C6 115.6(6) . .
C5 C7 C8 122.0(5) . .
C6 C7 C8 122.2(6) . .
O3 C8 O4 128.0(6) . .
O3 C8 C7 118.3(6) . .
O4 C8 C7 113.7(5) . .
O6 C9 O5 127.4(6) . .
O6 C9 C10 116.5(6) . .
O5 C9 C10 116.0(6) . .
C11 C10 C12 114.6(5) . .
C11 C10 C9 123.7(6) . .
C12 C10 C9 121.7(6) . .
F5 C11 C12 118.5(6) . 2_675
F5 C11 C10 117.7(6) . .
C12 C11 C10 123.8(5) 2_675 .
F6 C12 C11 118.2(5) . 2_675
F6 C12 C10 120.1(6) . .
C11 C12 C10 121.7(6) 2_675 .
N1 C13 C15 123.5(6) . .
N1 C13 H13 118.3 . .
C15 C13 H13 118.3 . .
N1 C14 C16 123.3(6) . .
N1 C14 H14 118.3 . .
C16 C14 H14 118.3 . .
C13 C15 C17 120.7(6) . .
C13 C15 H15 119.6 . .
C17 C15 H15 119.6 . .
C14 C16 C17 121.2(6) . .
C14 C16 H16 119.4 . .
C17 C16 H16 119.4 . .
C15 C17 C16 114.9(6) . .
C15 C17 C18 120.4(6) . .
C16 C17 C18 124.6(6) . .
C17 C18 C18 115.4(7) . 2
C17 C18 H18A 108.4 . .
C18 C18 H18A 108.4 2 .
C17 C18 H18B 108.4 . .
C18 C18 H18B 108.4 2 .
H18A C18 H18B 107.5 . .
N2 C19 C21 125.7(6) . .
N2 C19 H19 117.2 . .
C21 C19 H19 117.2 . .
N2 C20 C22 124.7(7) . .
N2 C20 H20 117.7 . .
C22 C20 H20 117.7 . .
C19 C21 C23 118.4(7) . .
C19 C21 H21 120.8 . .
C23 C21 H21 120.8 . .
C20 C22 C23 119.8(6) . .
C20 C22 H22 120.1 . .
C23 C22 H22 120.1 . .
C22 C23 C21 117.0(6) . .
C22 C23 C24 121.4(7) . .
C21 C23 C24 121.6(7) . .
C30 C24 C23 117.5(8) 1_444 .
C30 C24 H24A 107.9 1_444 .
C23 C24 H24A 107.9 . .
C30 C24 H24B 107.9 1_444 .
C23 C24 H24B 107.9 . .
H24A C24 H24B 107.2 . .
N3 C25 C27 126.0(8) . .
N3 C25 H25 117.0 . .
C27 C25 H25 117.0 . .
N3 C26 C28 124.1(8) . .
N3 C26 H26 117.9 . .
C28 C26 H26 117.9 . .
C25 C27 C29 120.0(9) . .
C25 C27 H27 120.0 . .
C29 C27 H27 120.0 . .
C29 C28 C26 120.3(8) . .
C29 C28 H28 119.9 . .
C26 C28 H28 119.9 . .
C28 C29 C27 115.0(7) . .
C28 C29 C30 120.3(11) . .
C27 C29 C30 124.6(12) . .
C24 C30 C29 121.6(9) 1_666 .
C24 C30 H30A 106.9 1_666 .
C29 C30 H30A 106.9 . .
C24 C30 H30B 106.9 1_666 .
C29 C30 H30B 106.9 . .
H30A C30 H30B 106.7 . .
C14 N1 C13 116.3(5) . .
C14 N1 Zn1 119.7(4) . .
C13 N1 Zn1 124.1(4) . .
C19 N2 C20 114.4(6) . .
C19 N2 Zn2 123.5(4) . .
C20 N2 Zn2 122.0(5) . .
C25 N3 C26 114.6(6) . .
C25 N3 Zn2 118.8(5) . .
C26 N3 Zn2 126.5(5) . .
C1 O1 Zn1 150.7(4) . .
C1 O2 Zn2 129.6(4) . .
C8 O3 Zn1 152.0(4) . 1_455
C8 O4 Zn2 128.5(4) . 1_455
C9 O5 Zn2 118.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.099(4) .
Zn1 O1 2.099(4) 2_666
Zn1 N1 2.106(5) .
Zn1 N1 2.106(5) 2_666
Zn1 O3 2.129(4) 1_655
Zn1 O3 2.129(4) 2_566
Zn2 O5 2.007(4) .
Zn2 O2 2.042(4) .
Zn2 O4 2.048(4) 1_655
Zn2 N2 2.142(5) .
Zn2 N3 2.167(5) .
C1 O1 1.223(7) .
C1 O2 1.246(7) .
C1 C2 1.525(8) .
C2 C4 1.371(8) .
C2 C3 1.377(8) .
C3 F1 1.337(7) .
C3 C5 1.375(8) .
C4 F2 1.347(7) .
C4 C6 1.382(9) .
C5 F3 1.353(6) .
C5 C7 1.371(8) .
C6 F4 1.349(7) .
C6 C7 1.379(8) .
C7 C8 1.515(8) .
C8 O3 1.230(7) .
C8 O4 1.243(7) .
C9 O6 1.226(8) .
C9 O5 1.250(8) .
C9 C10 1.519(8) .
C10 C11 1.381(9) .
C10 C12 1.392(8) .
C11 F5 1.349(6) .
C11 C12 1.366(9) 2_675
C12 F6 1.336(7) .
C12 C11 1.366(9) 2_675
C13 N1 1.337(8) .
C13 C15 1.364(9) .
C13 H13 0.9300 .
C14 N1 1.336(7) .
C14 C16 1.351(9) .
C14 H14 0.9300 .
C15 C17 1.385(8) .
C15 H15 0.9300 .
C16 C17 1.396(9) .
C16 H16 0.9300 .
C17 C18 1.497(9) .
C18 C18 1.550(12) 2
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 N2 1.322(8) .
C19 C21 1.366(9) .
C19 H19 0.9300 .
C20 N2 1.335(7) .
C20 C22 1.355(9) .
C20 H20 0.9300 .
C21 C23 1.382(9) .
C21 H21 0.9300 .
C22 C23 1.369(9) .
C22 H22 0.9300 .
C23 C24 1.524(10) .
C24 C30 1.338(12) 1_444
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C25 N3 1.296(8) .
C25 C27 1.346(10) .
C25 H25 0.9300 .
C26 N3 1.310(9) .
C26 C28 1.371(11) .
C26 H26 0.9300 .
C27 C29 1.369(13) .
C27 H27 0.9300 .
C28 C29 1.365(12) .
C28 H28 0.9300 .
C29 C30 1.483(11) .
C30 C24 1.338(12) 1_666
C30 H30A 0.9700 .
C30 H30B 0.9700 .
O3 Zn1 2.129(4) 1_455
O4 Zn2 2.048(4) 1_455
