#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:53:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178828 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/82/4108273.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_4108273
loop_
_publ_author_name
'Hiroyasu Furukawa'
'Jaheon Kim'
'Nathan W. Ockwig'
'Michael O'Keeffe'
'Omar M. Yaghi'
_publ_contact_author_address
; 
Department of Chemistry and Biochemistry
University of Caligornia-Los Angeles 
Los Angeles, CA 90095 
USA 
;
_publ_contact_author_email       yaghi@chem.ucla.edu
_publ_contact_author_name        'Professor Omar M. Yaghi'
_publ_section_title
;
 Control of Vertex Geometry, Structure Dimensionality, Functionality, and
 Pore Metrics in the Reticular Synthesis of Crystalline Metal-Organic
 Frameworks and Polyhedra
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11650
_journal_page_last               11661
_journal_paper_doi               10.1021/ja803783c
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C50 H60 Cu2 N4 O14'
_chemical_formula_weight         1068.10
_chemical_name_common            MOF-117
_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                 104.786(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0679(14)
_cell_length_b                   18.449(3)
_cell_length_c                   14.567(2)
_cell_measurement_reflns_used    2337
_cell_measurement_temperature    258(2)
_cell_measurement_theta_max      19.47
_cell_measurement_theta_min      2.20
_cell_volume                     2616.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      258(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'phi and 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  0.0920
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25770
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
ratio of minimum to maximum apparent transmission:  0.774590 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6180
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1205P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.2115
_reflns_number_gt                3395
_reflns_number_total             6180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja803783c_si_011.cif
_cod_data_source_block           MOF-117
_cod_original_cell_volume        2616.1(6)
_cod_database_code               4108273
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
Cu1 Cu 0.95210(5) -0.04930(3) 1.04954(4) 0.0332(2) Uani 1 1 d .
O1 O 0.2793(5) 0.2709(2) 1.0529(3) 0.0708(13) Uani 1 1 d .
O2 O 0.7927(3) 0.01331(18) 1.0433(2) 0.0452(8) Uani 1 1 d .
O3 O 0.8777(3) 0.09632(19) 0.9619(2) 0.0487(9) Uani 1 1 d .
O4 O 0.0550(4) 0.4926(2) 0.6586(2) 0.0491(9) Uani 1 1 d .
O5 O 0.1387(3) 0.41103(19) 0.5752(2) 0.0465(9) Uani 1 1 d .
C1 C 0.3347(5) 0.2670(3) 0.9883(4) 0.0460(12) Uani 1 1 d .
C2 C 0.4529(5) 0.2167(3) 0.9940(3) 0.0400(11) Uani 1 1 d .
C3 C 0.4467(5) 0.1459(3) 1.0255(3) 0.0411(11) Uani 1 1 d .
H3A H 0.3695 0.1297 1.0434 0.049 Uiso 1 1 calc R
C4 C 0.5572(5) 0.0996(3) 1.0298(3) 0.0412(11) Uani 1 1 d .
H4A H 0.5541 0.0523 1.0509 0.049 Uiso 1 1 calc R
C5 C 0.6724(5) 0.1238(3) 1.0026(3) 0.0404(11) Uani 1 1 d .
C6 C 0.6790(5) 0.1952(3) 0.9750(4) 0.0472(13) Uani 1 1 d .
H6A H 0.7575 0.2120 0.9594 0.057 Uiso 1 1 calc R
C7 C 0.5701(5) 0.2413(3) 0.9704(4) 0.0482(13) Uani 1 1 d .
H7A H 0.5752 0.2892 0.9515 0.058 Uiso 1 1 calc R
C8 C 0.7901(5) 0.0732(3) 1.0029(3) 0.0367(11) Uani 1 1 d .
C9 C 0.2869(5) 0.3120(3) 0.9017(3) 0.0402(11) Uani 1 1 d .
C10 C 0.3062(5) 0.2906(3) 0.8150(3) 0.0445(12) Uani 1 1 d .
H10A H 0.3558 0.2488 0.8109 0.053 Uiso 1 1 calc R
C11 C 0.2522(5) 0.3311(3) 0.7345(3) 0.0435(12) Uani 1 1 d .
H11A H 0.2625 0.3153 0.6761 0.052 Uiso 1 1 calc R
C12 C 0.1833(5) 0.3945(3) 0.7401(3) 0.0372(11) Uani 1 1 d .
C13 C 0.1649(6) 0.4173(3) 0.8268(4) 0.0505(14) Uani 1 1 d .
H13A H 0.1186 0.4603 0.8308 0.061 Uiso 1 1 calc R
C14 C 0.2153(6) 0.3760(3) 0.9068(3) 0.0520(14) Uani 1 1 d .
H14A H 0.2016 0.3909 0.9647 0.062 Uiso 1 1 calc R
C15 C 0.1209(5) 0.4364(3) 0.6512(3) 0.0383(11) Uani 1 1 d .
O1S O 0.9164(4) -0.1373(2) 1.1386(3) 0.0561(10) Uani 1 1 d D
N1S N 1.0600(6) -0.2188(4) 1.2281(5) 0.0901(19) Uani 1 1 d D
C1S C 0.9862(6) -0.1926(4) 1.1494(4) 0.0611(16) Uani 1 1 d DU
H1SA H 0.9859 -0.2187 1.0947 0.073 Uiso 1 1 calc R
C2S C 1.0978(13) -0.1636(8) 1.3210(8) 0.179(7) Uani 1 1 d DU
H2SA H 1.1912 -0.1700 1.3592 0.215 Uiso 1 1 calc R
H2SB H 1.0818 -0.1131 1.3029 0.215 Uiso 1 1 calc R
C3S C 1.0110(15) -0.1878(9) 1.3608(14) 0.251(10) Uani 1 1 d DU
H3SA H 1.0148 -0.1605 1.4175 0.377 Uiso 1 1 calc R
H3SB H 1.0304 -0.2378 1.3769 0.377 Uiso 1 1 calc R
H3SC H 0.9209 -0.1836 1.3186 0.377 Uiso 1 1 calc R
C4S C 1.1349(8) -0.2880(5) 1.2314(7) 0.112(3) Uani 1 1 d DU
H4SA H 1.1093 -0.3197 1.2772 0.134 Uiso 1 1 calc R
H4SB H 1.1058 -0.3112 1.1697 0.134 Uiso 1 1 calc R
C5S C 1.2839(9) -0.2809(5) 1.2565(6) 0.122(3) Uani 1 1 d DU
H5SA H 1.3249 -0.3279 1.2564 0.183 Uiso 1 1 calc R
H5SB H 1.3143 -0.2597 1.3185 0.183 Uiso 1 1 calc R
H5SC H 1.3107 -0.2503 1.2109 0.183 Uiso 1 1 calc R
O2S O 1.3221(16) -0.4121(7) 1.0617(14) 0.316(9) Uani 1 1 d DU
N2S N 1.3837(16) -0.4989(7) 1.1569(11) 0.226(8) Uani 1 1 d DU
C6S C 1.4154(19) -0.4544(10) 1.1020(17) 0.288(13) Uani 1 1 d DU
H6SA H 1.5028 -0.4528 1.0918 0.346 Uiso 1 1 calc R
C7S C 1.230(3) -0.5293(14) 1.1434(16) 0.43(2) Uani 1 1 d DU
H7SA H 1.1636 -0.5085 1.0896 0.521 Uiso 1 1 calc R
H7SB H 1.2240 -0.5818 1.1423 0.521 Uiso 1 1 calc R
C8S C 1.226(2) -0.5027(11) 1.2196(15) 0.293(12) Uani 1 1 d DU
H8SA H 1.1406 -0.5147 1.2333 0.440 Uiso 1 1 calc R
H8SB H 1.2347 -0.4510 1.2165 0.440 Uiso 1 1 calc R
H8SC H 1.3008 -0.5216 1.2687 0.440 Uiso 1 1 calc R
C9S C 1.495(3) -0.5229(12) 1.2456(17) 0.43(2) Uani 1 1 d DU
H9SA H 1.5718 -0.4893 1.2603 0.518 Uiso 1 1 calc R
H9SB H 1.4582 -0.5280 1.3006 0.518 Uiso 1 1 calc R
C10S C 1.533(3) -0.5896(11) 1.216(2) 0.40(2) Uani 1 1 d DU
H10B H 1.6060 -0.6100 1.2649 0.604 Uiso 1 1 calc R
H10C H 1.5647 -0.5830 1.1594 0.604 Uiso 1 1 calc R
H10D H 1.4557 -0.6217 1.2026 0.604 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'
Cu Cu 0.3201 1.2651 '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
O5 Cu1 O3 88.09(15) 2_646 3_757
O5 Cu1 O2 89.69(15) 2_646 .
O3 Cu1 O2 167.76(14) 3_757 .
O5 Cu1 O4 167.56(14) 2_646 4_666
O3 Cu1 O4 90.72(15) 3_757 4_666
O2 Cu1 O4 88.86(15) . 4_666
O5 Cu1 O1S 99.60(15) 2_646 .
O3 Cu1 O1S 90.09(14) 3_757 .
O2 Cu1 O1S 102.14(15) . .
O4 Cu1 O1S 92.78(15) 4_666 .
O5 Cu1 Cu1 84.24(10) 2_646 3_757
O3 Cu1 Cu1 79.07(10) 3_757 3_757
O2 Cu1 Cu1 88.74(10) . 3_757
O4 Cu1 Cu1 83.38(11) 4_666 3_757
O1S Cu1 Cu1 168.42(11) . 3_757
C8 O2 Cu1 117.5(3) . .
C8 O3 Cu1 128.5(3) . 3_757
C15 O4 Cu1 123.6(3) . 4_465
C15 O5 Cu1 122.8(3) . 2_656
O1 C1 C9 120.9(5) . .
O1 C1 C2 120.7(4) . .
C9 C1 C2 118.4(4) . .
C3 C2 C7 120.1(4) . .
C3 C2 C1 120.0(4) . .
C7 C2 C1 119.8(4) . .
C2 C3 C4 119.2(4) . .
C2 C3 H3A 120.4 . .
C4 C3 H3A 120.4 . .
C5 C4 C3 120.4(5) . .
C5 C4 H4A 119.8 . .
C3 C4 H4A 119.8 . .
C6 C5 C4 119.6(5) . .
C6 C5 C8 119.6(4) . .
C4 C5 C8 120.8(4) . .
C7 C6 C5 120.4(5) . .
C7 C6 H6A 119.8 . .
C5 C6 H6A 119.8 . .
C6 C7 C2 120.2(5) . .
C6 C7 H7A 119.9 . .
C2 C7 H7A 119.9 . .
O2 C8 O3 126.2(4) . .
O2 C8 C5 118.1(4) . .
O3 C8 C5 115.8(4) . .
C10 C9 C14 118.9(4) . .
C10 C9 C1 121.8(4) . .
C14 C9 C1 119.2(4) . .
C11 C10 C9 120.4(5) . .
C11 C10 H10A 119.8 . .
C9 C10 H10A 119.8 . .
C12 C11 C10 120.4(4) . .
C12 C11 H11A 119.8 . .
C10 C11 H11A 119.8 . .
C11 C12 C13 119.9(4) . .
C11 C12 C15 119.6(4) . .
C13 C12 C15 120.4(4) . .
C14 C13 C12 119.9(5) . .
C14 C13 H13A 120.1 . .
C12 C13 H13A 120.1 . .
C13 C14 C9 120.4(5) . .
C13 C14 H14A 119.8 . .
C9 C14 H14A 119.8 . .
O5 C15 O4 125.7(4) . .
O5 C15 C12 116.5(4) . .
O4 C15 C12 117.8(4) . .
C1S O1S Cu1 121.6(4) . .
C1S N1S C4S 121.7(7) . .
C1S N1S C2S 117.1(7) . .
C4S N1S C2S 119.7(6) . .
O1S C1S N1S 127.3(7) . .
O1S C1S H1SA 116.3 . .
N1S C1S H1SA 116.3 . .
C3S C2S N1S 96.7(15) . .
C3S C2S H2SA 112.4 . .
N1S C2S H2SA 112.4 . .
C3S C2S H2SB 112.4 . .
N1S C2S H2SB 112.4 . .
H2SA C2S H2SB 110.0 . .
C2S C3S H3SA 109.5 . .
C2S C3S H3SB 109.5 . .
H3SA C3S H3SB 109.5 . .
C2S C3S H3SC 109.5 . .
H3SA C3S H3SC 109.5 . .
H3SB C3S H3SC 109.5 . .
C5S C4S N1S 114.4(8) . .
C5S C4S H4SA 108.7 . .
N1S C4S H4SA 108.7 . .
C5S C4S H4SB 108.6 . .
N1S C4S H4SB 108.6 . .
H4SA C4S H4SB 107.6 . .
C4S C5S H5SA 109.5 . .
C4S C5S H5SB 109.5 . .
H5SA C5S H5SB 109.5 . .
C4S C5S H5SC 109.5 . .
H5SA C5S H5SC 109.5 . .
H5SB C5S H5SC 109.5 . .
C6S N2S C9S 118.4(17) . .
C6S N2S C7S 123.3(16) . .
C9S N2S C7S 118.2(16) . .
N2S C6S O2S 115.5(18) . .
N2S C6S H6SA 122.3 . .
O2S C6S H6SA 122.3 . .
C8S C7S N2S 90.0(15) . .
C8S C7S H7SA 113.6 . .
N2S C7S H7SA 113.7 . .
C8S C7S H7SB 113.7 . .
N2S C7S H7SB 113.6 . .
H7SA C7S H7SB 110.9 . .
C7S C8S H8SA 109.5 . .
C7S C8S H8SB 109.5 . .
H8SA C8S H8SB 109.5 . .
C7S C8S H8SC 109.5 . .
H8SA C8S H8SC 109.5 . .
H8SB C8S H8SC 109.5 . .
C10S C9S N2S 101.0(18) . .
C10S C9S H9SA 111.4 . .
N2S C9S H9SA 111.5 . .
C10S C9S H9SB 111.7 . .
N2S C9S H9SB 111.6 . .
H9SA C9S H9SB 109.4 . .
C9S C10S H10B 109.5 . .
C9S C10S H10C 109.6 . .
H10B C10S H10C 109.5 . .
C9S C10S H10D 109.3 . .
H10B C10S H10D 109.5 . .
H10C C10S H10D 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O5 1.956(3) 2_646
Cu1 O3 1.965(3) 3_757
Cu1 O2 1.961(3) .
Cu1 O4 1.963(3) 4_666
Cu1 O1S 2.165(4) .
Cu1 Cu1 2.6520(11) 3_757
O1 C1 1.213(6) .
O2 C8 1.249(6) .
O3 C8 1.259(5) .
O3 Cu1 1.965(3) 3_757
O4 C15 1.251(6) .
O4 Cu1 1.963(3) 4_465
O5 C15 1.255(6) .
O5 Cu1 1.956(3) 2_656
C1 C9 1.483(7) .
C1 C2 1.495(7) .
C2 C3 1.390(7) .
C2 C7 1.388(7) .
C3 C4 1.392(7) .
C3 H3A 0.9300 .
C4 C5 1.390(7) .
C4 H4A 0.9300 .
C5 C6 1.383(7) .
C5 C8 1.508(7) .
C6 C7 1.377(7) .
C6 H6A 0.9300 .
C7 H7A 0.9300 .
C9 C10 1.384(7) .
C9 C14 1.396(7) .
C10 C11 1.378(6) .
C10 H10A 0.9300 .
C11 C12 1.373(7) .
C11 H11A 0.9300 .
C12 C13 1.387(7) .
C12 C15 1.502(6) .
C13 C14 1.376(7) .
C13 H13A 0.9300 .
C14 H14A 0.9300 .
O1S C1S 1.226(7) .
N1S C1S 1.291(7) .
N1S C4S 1.478(10) .
N1S C2S 1.658(14) .
C1S H1SA 0.9300 .
C2S C3S 1.248(13) .
C2S H2SA 0.9700 .
C2S H2SB 0.9700 .
C3S H3SA 0.9600 .
C3S H3SB 0.9600 .
C3S H3SC 0.9600 .
C4S C5S 1.457(10) .
C4S H4SA 0.9700 .
C4S H4SB 0.9700 .
C5S H5SA 0.9600 .
C5S H5SB 0.9600 .
C5S H5SC 0.9600 .
O2S C6S 1.248(14) .
N2S C6S 1.243(15) .
N2S C9S 1.545(18) .
N2S C7S 1.612(18) .
C6S H6SA 0.9300 .
C7S C8S 1.222(16) .
C7S H7SA 0.9700 .
C7S H7SB 0.9700 .
C8S H8SA 0.9600 .
C8S H8SB 0.9600 .
C8S H8SC 0.9600 .
C9S C10S 1.390(17) .
C9S H9SA 0.9700 .
C9S H9SB 0.9700 .
C10S H10B 0.9600 .
C10S H10C 0.9600 .
C10S H10D 0.9600 .
