#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:06:59 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178885 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/14/4111413.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_4111413
loop_
_publ_author_name
'Nathaniel L. Rosi'
'Jaheon Kim'
'Mohamed Eddaoudi'
'Banglin Chen'
'Michael O'Keeffe'
'Omar M. Yaghi'
_publ_contact_author_address
;
Department of Chemistry
930 N. University Ave.
Ann Arbor, MI 48109-1055
USA
;
_publ_contact_author_email       oyaghi@umich.edu
_publ_contact_author_fax         '+1 734 763 2307'
_publ_contact_author_name        'Professor Omar M. Yaghi'
_publ_contact_author_phone       '+1 734 615 2146'
_publ_section_title
;
 Rod Packings and Metal-Organic Frameworks Constructed from Rod-Shaped
 Secondary Building Units
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1504
_journal_page_last               1518
_journal_paper_doi               10.1021/ja045123o
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C30 H23 N O9 Tb, C3 H7 N O'
_chemical_formula_sum            'C33 H30 N2 O10 Tb'
_chemical_formula_weight         773.51
_chemical_name_common            MOF-80
_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                109.7500(10)
_cell_angle_beta                 103.6130(10)
_cell_angle_gamma                100.1400(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8294(4)
_cell_length_b                   12.1098(5)
_cell_length_c                   14.6279(6)
_cell_measurement_reflns_used    5972
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.27
_cell_volume                     1529.29(11)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELX-TL xp'
_computing_publication_material  'Siemens SHELX-TL xcif'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'omega and phi scan'
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19781
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.375
_exptl_absorpt_correction_T_max  .949
_exptl_absorpt_correction_T_min  .842
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       plate
_exptl_crystal_F_000             774
_exptl_crystal_size_max          .06
_exptl_crystal_size_mid          .04
_exptl_crystal_size_min          .02
_refine_diff_density_max         0.932
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       none
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6251
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0361P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                4794
_reflns_number_total             6251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja045123o_s12.cif
_cod_data_source_block           MOF-80
_cod_database_code               4111413
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
Tb Tb -0.23970(3) -0.97874(2) -1.004694(17) 0.01809(9) Uani 1 1 d .
O1W O -0.0476(4) -0.7924(3) -0.9482(3) 0.0274(8) Uani 1 1 d D
H1W H -0.049(6) -0.753(4) -0.986(3) 0.033 Uiso 1 1 d D
H2W H 0.035(3) -0.801(5) -0.929(4) 0.033 Uiso 1 1 d D
O2W O -0.3468(4) -1.1057(3) -0.9254(3) 0.0252(8) Uani 1 1 d D
H3W H -0.426(3) -1.092(4) -0.921(4) 0.030 Uiso 1 1 d D
H4W H -0.377(5) -1.178(2) -0.970(3) 0.030 Uiso 1 1 d D
O1 O -0.2876(3) -0.8460(3) -0.8631(2) 0.0256(8) Uani 1 1 d .
O2 O -0.5202(3) -0.9316(3) -0.8892(2) 0.0256(8) Uani 1 1 d .
O3 O -0.2306(3) -0.1821(3) -0.0901(2) 0.0250(8) Uani 1 1 d .
O4 O -0.4164(4) -0.3184(3) -0.0895(2) 0.0317(9) Uani 1 1 d .
O5 O -0.0356(3) -0.9838(3) -0.8925(2) 0.0241(8) Uani 1 1 d .
O6 O 0.1820(3) -1.0152(3) -0.8455(2) 0.0259(8) Uani 1 1 d .
C1 C -0.4867(5) -0.7995(4) -0.6832(3) 0.0213(11) Uani 1 1 d .
H1A H -0.5652 -0.8720 -0.7198 0.026 Uiso 1 1 calc R
C2 C -0.3862(5) -0.7677(4) -0.7297(3) 0.0200(10) Uani 1 1 d .
C3 C -0.2731(5) -0.6596(4) -0.6774(4) 0.0232(11) Uani 1 1 d .
H3A H -0.2039 -0.6398 -0.7092 0.028 Uiso 1 1 calc R
C4 C -0.1499(6) -0.4643(5) -0.5253(4) 0.0311(13) Uani 1 1 d .
H4A H -0.0843 -0.4397 -0.5578 0.037 Uiso 1 1 calc R
C5 C -0.1384(6) -0.3903(5) -0.4296(4) 0.0311(13) Uani 1 1 d .
H5A H -0.0626 -0.3158 -0.3955 0.037 Uiso 1 1 calc R
C6 C -0.2309(5) -0.3421(4) -0.2804(3) 0.0261(12) Uani 1 1 d .
H6A H -0.1577 -0.2660 -0.2460 0.031 Uiso 1 1 calc R
C7 C -0.3295(5) -0.3737(4) -0.2337(3) 0.0219(11) Uani 1 1 d .
C8 C -0.4388(5) -0.4851(4) -0.2840(3) 0.0243(11) Uani 1 1 d .
H8A H -0.5067 -0.5058 -0.2517 0.029 Uiso 1 1 calc R
C9 C -0.5607(6) -0.6808(5) -0.4357(4) 0.0346(13) Uani 1 1 d .
H9A H -0.6281 -0.7039 -0.4039 0.041 Uiso 1 1 calc R
C10 C -0.5718(5) -0.7559(5) -0.5310(4) 0.0308(13) Uani 1 1 d .
H10A H -0.6467 -0.8310 -0.5649 0.037 Uiso 1 1 calc R
C11 C -0.4721(5) -0.7244(4) -0.5825(4) 0.0252(11) Uani 1 1 d .
C12 C -0.3594(5) -0.6128(4) -0.5303(3) 0.0205(11) Uani 1 1 d .
C13 C -0.2602(5) -0.5803(4) -0.5794(4) 0.0233(11) Uani 1 1 d .
C14 C -0.2373(5) -0.4205(4) -0.3776(4) 0.0251(12) Uani 1 1 d .
C15 C -0.3477(5) -0.5347(4) -0.4294(3) 0.0217(11) Uani 1 1 d .
C16 C -0.4489(5) -0.5665(4) -0.3815(4) 0.0235(11) Uani 1 1 d .
C17 C -0.3993(5) -0.8536(4) -0.8354(4) 0.0229(11) Uani 1 1 d .
C18 C -0.3280(5) -0.2865(5) -0.1303(4) 0.0260(12) Uani 1 1 d .
C19 C 0.0438(5) -0.9995(4) -0.7320(3) 0.0194(10) Uani 1 1 d .
C20 C -0.0639(5) -0.9548(5) -0.6979(4) 0.0265(12) Uani 1 1 d .
H20A H -0.1263 -0.9251 -0.7380 0.032 Uiso 1 1 calc R
C21 C -0.0818(5) -0.9529(5) -0.6058(4) 0.0271(12) Uani 1 1 d .
C22 C 0.0092(5) -0.9996(4) -0.5473(3) 0.0218(11) Uani 1 1 d .
C23 C 0.1187(5) -1.0456(5) -0.5814(4) 0.0261(12) Uani 1 1 d .
C24 C 0.1348(5) -1.0438(4) -0.6736(4) 0.0258(12) Uani 1 1 d .
H24A H 0.2091 -1.0733 -0.6967 0.031 Uiso 1 1 calc R
C25 C 0.0640(5) -0.9995(4) -0.8306(4) 0.0243(11) Uani 1 1 d .
C26 C -0.1882(6) -0.9028(6) -0.5664(4) 0.0474(17) Uani 1 1 d .
H26A H -0.2453 -0.8660 -0.6027 0.057 Uiso 1 1 calc R
C27 C 0.2097(6) -1.0938(6) -0.5208(4) 0.0444(16) Uani 1 1 d .
H27A H 0.2852 -1.1232 -0.5422 0.053 Uiso 1 1 calc R
O1S O -0.3406(4) -0.8376(4) -1.0623(3) 0.0357(9) Uani 1 1 d .
C1S C -0.3284(7) -0.7314(8) -1.0294(6) 0.060(2) Uani 1 1 d .
H1SA H -0.2862 -0.6860 -0.9576 0.072 Uiso 1 1 calc R
N1S N -0.3718(7) -0.6710(6) -1.0893(5) 0.0690(17) Uani 1 1 d .
O2S O -0.0333(5) -0.6689(4) -1.0744(4) 0.0684(14) Uani 1 1 d .
C4S C 0.0508(8) -0.6870(7) -1.1228(6) 0.065(2) Uani 1 1 d .
H4SA H 0.1102 -0.7383 -1.1118 0.078 Uiso 1 1 calc R
C5S C 0.1630(10) -0.6701(9) -1.2505(7) 0.121(4) Uani 1 1 d .
H5SA H 0.2130 -0.7246 -1.2289 0.145 Uiso 1 1 calc R
H5SB H 0.2351 -0.5955 -1.2388 0.145 Uiso 1 1 calc R
H5SC H 0.1068 -0.7114 -1.3236 0.145 Uiso 1 1 calc R
C6S C -0.0243(10) -0.5595(8) -1.2143(8) 0.106(3) Uani 1 1 d .
H6SA H -0.0863 -0.5465 -1.1703 0.127 Uiso 1 1 calc R
H6SB H -0.0856 -0.5987 -1.2863 0.127 Uiso 1 1 calc R
H6SC H 0.0400 -0.4806 -1.2019 0.127 Uiso 1 1 calc R
N2S N 0.0641(7) -0.6382(6) -1.1910(5) 0.0761(19) Uani 1 1 d .
C2S C -0.3449(12) -0.5424(7) -1.0478(8) 0.117(4) Uani 1 1 d .
H2SA H -0.3153 -0.5116 -0.9729 0.141 Uiso 1 1 calc R
H2SB H -0.4339 -0.5211 -1.0733 0.141 Uiso 1 1 calc R
H2SC H -0.2670 -0.5054 -1.0686 0.141 Uiso 1 1 calc R
C3S C -0.4245(11) -0.7409(8) -1.1996(6) 0.106(3) Uani 1 1 d .
H3SA H -0.4423 -0.8283 -1.2140 0.127 Uiso 1 1 calc R
H3SB H -0.3512 -0.7166 -1.2296 0.127 Uiso 1 1 calc R
H3SC H -0.5155 -0.7250 -1.2294 0.127 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'
Tb Tb -0.1723 4.1537 '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 Tb O2 150.45(12) . 2_433
O5 Tb O1 88.54(11) . .
O2 Tb O1 97.22(11) 2_433 .
O5 Tb O6 107.19(11) . 2_533
O2 Tb O6 86.17(11) 2_433 2_533
O1 Tb O6 141.30(11) . 2_533
O5 Tb O3 79.01(11) . 1_544
O2 Tb O3 79.76(11) 2_433 1_544
O1 Tb O3 144.80(11) . 1_544
O6 Tb O3 73.83(11) 2_533 1_544
O5 Tb O1S 140.61(13) . .
O2 Tb O1S 68.26(12) 2_433 .
O1 Tb O1S 74.24(12) . .
O6 Tb O1S 71.37(12) 2_533 .
O3 Tb O1S 133.57(12) 1_544 .
O5 Tb O1W 70.25(12) . .
O2 Tb O1W 139.29(12) 2_433 .
O1 Tb O1W 77.38(11) . .
O6 Tb O1W 75.37(12) 2_533 .
O3 Tb O1W 126.88(11) 1_544 .
O1S Tb O1W 71.50(12) . .
O5 Tb O2W 78.21(11) . .
O2 Tb O2W 75.87(12) 2_433 .
O1 Tb O2W 73.09(11) . .
O6 Tb O2W 143.76(11) 2_533 .
O3 Tb O2W 72.17(11) 1_544 .
O1S Tb O2W 127.04(12) . .
O1W Tb O2W 136.89(12) . .
C17 O1 Tb 130.8(3) . .
C17 O2 Tb 161.7(3) . 2_433
C18 O3 Tb 132.4(3) . 1_566
C25 O5 Tb 171.7(3) . .
C25 O6 Tb 123.7(3) . 2_533
C2 C1 C11 120.1(4) . .
C1 C2 C3 120.3(4) . .
C1 C2 C17 119.0(4) . .
C3 C2 C17 120.8(4) . .
C13 C3 C2 120.9(4) . .
C5 C4 C13 121.2(5) . .
C4 C5 C14 122.1(5) . .
C7 C6 C14 120.9(4) . .
C6 C7 C8 120.2(4) . .
C6 C7 C18 121.3(4) . .
C8 C7 C18 118.5(4) . .
C16 C8 C7 120.8(4) . .
C10 C9 C16 121.3(5) . .
C9 C10 C11 121.3(5) . .
C1 C11 C12 119.6(4) . .
C1 C11 C10 121.6(4) . .
C12 C11 C10 118.8(4) . .
C13 C12 C11 119.7(4) . .
C13 C12 C15 120.8(4) . .
C11 C12 C15 119.6(4) . .
C3 C13 C12 119.4(4) . .
C3 C13 C4 122.5(4) . .
C12 C13 C4 118.1(4) . .
C6 C14 C15 119.4(4) . .
C6 C14 C5 122.7(5) . .
C15 C14 C5 117.8(4) . .
C16 C15 C12 120.5(4) . .
C16 C15 C14 119.5(4) . .
C12 C15 C14 119.9(4) . .
C8 C16 C15 119.3(4) . .
C8 C16 C9 122.2(4) . .
C15 C16 C9 118.6(4) . .
O1 C17 O2 124.0(4) . .
O1 C17 C2 118.0(4) . .
O2 C17 C2 117.9(4) . .
O4 C18 O3 124.4(4) . .
O4 C18 C7 119.7(4) . .
O3 C18 C7 115.9(4) . .
C20 C19 C24 119.6(4) . .
C20 C19 C25 120.8(4) . .
C24 C19 C25 119.6(4) . .
C19 C20 C21 121.1(4) . .
C20 C21 C22 119.3(4) . .
C20 C21 C26 122.4(5) . .
C22 C21 C26 118.3(4) . .
C23 C22 C21 120.1(4) . .
C23 C22 C22 119.8(5) . 2_534
C21 C22 C22 120.1(5) . 2_534
C24 C23 C22 118.7(4) . .
C24 C23 C27 122.1(4) . .
C22 C23 C27 119.1(4) . .
C19 C24 C23 121.2(4) . .
O5 C25 O6 124.2(4) . .
O5 C25 C19 118.8(4) . .
O6 C25 C19 117.0(4) . .
C27 C26 C21 122.2(5) 2_534 .
C26 C27 C23 120.4(5) 2_534 .
C1S O1S Tb 137.1(4) . .
O1S C1S N1S 123.3(7) . .
C1S N1S C2S 121.4(7) . .
C1S N1S C3S 117.0(7) . .
C2S N1S C3S 120.8(7) . .
O2S C4S N2S 123.1(8) . .
C4S N2S C5S 119.7(8) . .
C4S N2S C6S 122.5(7) . .
C5S N2S C6S 117.7(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb O5 2.298(3) .
Tb O2 2.322(3) 2_433
Tb O1 2.360(3) .
Tb O6 2.371(3) 2_533
Tb O3 2.385(3) 1_544
Tb O1S 2.407(4) .
Tb O1W 2.417(4) .
Tb O2W 2.455(3) .
O1 C17 1.256(5) .
O2 C17 1.260(6) .
O2 Tb 2.322(3) 2_433
O3 C18 1.291(6) .
O3 Tb 2.384(3) 1_566
O4 C18 1.241(6) .
O5 C25 1.257(6) .
O6 C25 1.264(5) .
O6 Tb 2.371(3) 2_533
C1 C2 1.395(6) .
C1 C11 1.402(6) .
C2 C3 1.395(6) .
C2 C17 1.504(6) .
C3 C13 1.390(6) .
C4 C5 1.348(7) .
C4 C13 1.443(7) .
C5 C14 1.438(6) .
C6 C7 1.383(6) .
C6 C14 1.396(6) .
C7 C8 1.401(6) .
C7 C18 1.519(6) .
C8 C16 1.401(6) .
C9 C10 1.348(6) .
C9 C16 1.437(7) .
C10 C11 1.444(6) .
C11 C12 1.419(6) .
C12 C13 1.416(6) .
C12 C15 1.423(6) .
C14 C15 1.429(6) .
C15 C16 1.416(6) .
C19 C20 1.390(6) .
C19 C24 1.391(6) .
C19 C25 1.501(6) .
C20 C21 1.391(6) .
C21 C22 1.414(7) .
C21 C26 1.437(7) .
C22 C23 1.412(6) .
C22 C22 1.441(8) 2_534
C23 C24 1.401(6) .
C23 C27 1.445(7) .
C26 C27 1.353(7) 2_534
C27 C26 1.353(7) 2_534
O1S C1S 1.183(8) .
C1S N1S 1.360(8) .
N1S C2S 1.416(9) .
N1S C3S 1.455(9) .
O2S C4S 1.211(8) .
C4S N2S 1.340(9) .
C5S N2S 1.468(9) .
C6S N2S 1.467(10) .
