#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:13:32 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179051 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/13/4301316.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_4301316
loop_
_publ_author_name
'Cory A. Black'
'José Sánchez Costa'
'Wen Tian Fu'
'Chiara Massera'
'Olivier Roubeau'
'Simon J. Teat'
'Guillem Aromí'
'Patrick Gamez'
'Jan Reedijk'
_publ_contact_author             'Reedijk, J.'
_publ_contact_author_email       reedijk@chem.leidenuniv.nl
_publ_section_title
;
3-D Lanthanide Metal-Organic Frameworks: Structure, Photoluminescence, and
Magnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1062
_journal_page_last               1068
_journal_paper_doi               10.1021/ic8017826
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C42 H57 N9 O18 Tb2'
_chemical_formula_sum            'C42 H57 N9 O18 Tb2'
_chemical_formula_weight         1293.81
_chemical_name_common            'compound 4'
_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                101.4720(10)
_cell_angle_beta                 110.5000(10)
_cell_angle_gamma                99.2570(10)
_cell_formula_units_Z            1
_cell_length_a                   10.5390(9)
_cell_length_b                   11.2180(9)
_cell_length_c                   12.8420(11)
_cell_measurement_reflns_used    12617
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      1.26
_cell_volume                     1349.0(2)
_computing_data_collection       SMART
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'BRUKER AXS SMART 1000'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15867
_diffrn_reflns_theta_full        28.94
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.674
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.741671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.361
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6447
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0691P)²+1.0232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                5755
_reflns_number_total             6447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8017826_si_002_5.cif
_cod_data_source_block           4
_cod_database_code               4301316
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.606205(15) 0.049907(13) 0.175613(13) 0.02501(7) Uani 1 1 d . . .
O1 O 0.3440(3) -0.0031(3) -0.0118(3) 0.0393(6) Uani 1 1 d . . .
O2 O 0.3803(3) 0.0624(3) 0.1724(3) 0.0433(7) Uani 1 1 d . . .
O3 O 0.5688(3) 0.2203(3) 0.0970(2) 0.0422(7) Uani 1 1 d . . .
O4 O 0.5004(3) 0.1692(2) -0.0963(2) 0.0415(7) Uani 1 1 d . . .
O5 O 0.8320(3) 0.2067(3) 0.2637(3) 0.0601(10) Uani 1 1 d . . .
O6 O 0.6825(3) 0.2369(3) 0.3417(2) 0.0433(7) Uani 1 1 d . . .
O7 O 0.5825(4) -0.0274(3) 0.3342(3) 0.0539(8) Uani 1 1 d . . .
O8 O 0.7957(4) -0.0456(4) 0.2525(4) 0.0684(11) Uani 1 1 d D . .
C1 C 0.2981(4) 0.0259(4) 0.0664(4) 0.0355(8) Uani 1 1 d . . .
C2 C 0.1444(4) 0.0142(4) 0.0334(3) 0.0352(8) Uani 1 1 d . . .
C3 C 0.0925(4) 0.0585(5) 0.1161(4) 0.0443(10) Uani 1 1 d . . .
C4 C 0.0531(5) -0.0434(5) -0.0804(4) 0.0452(10) Uani 1 1 d . . .
H4 H 0.0887 -0.0728 -0.1346 0.19(3) Uiso 1 1 calc R . .
C5 C 0.5297(5) 0.2455(3) 0.0008(4) 0.0376(9) Uani 1 1 d . . .
C6 C 0.5177(5) 0.3783(3) 0.0017(4) 0.0417(10) Uani 1 1 d . . .
C7 C 0.5132(6) 0.4600(4) 0.1000(4) 0.0507(12) Uani 1 1 d . . .
C8 C 0.5032(6) 0.4190(4) -0.0958(4) 0.0503(12) Uani 1 1 d . . .
H8 H 0.5044 0.3647 -0.1603 0.19(3) Uiso 1 1 calc R . .
C9 C 0.8003(4) 0.2705(4) 0.3355(3) 0.0376(9) Uani 1 1 d . . .
C10 C 0.9024(5) 0.3902(4) 0.4199(3) 0.0408(9) Uani 1 1 d . . .
C11 C 0.8649(5) 0.4692(5) 0.4963(4) 0.0554(13) Uani 1 1 d . . .
C12 C 1.0389(6) 0.4212(5) 0.4239(5) 0.0588(14) Uani 1 1 d . . .
C13 C 0.4833(8) -0.1042(7) 0.3318(6) 0.078(2) Uani 1 1 d . . .
H13 H 0.3997 -0.1213 0.2677 0.19(3) Uiso 1 1 calc R . .
C14 C 0.6090(16) -0.1410(15) 0.5131(10) 0.185(7) Uani 1 1 d . . .
H14A H 0.6798 -0.1707 0.4924 0.278 Uiso 1 1 calc R . .
H14B H 0.5875 -0.1849 0.5642 0.278 Uiso 1 1 calc R . .
H14C H 0.6424 -0.0526 0.5512 0.278 Uiso 1 1 calc R . .
C15 C 0.3627(15) -0.2532(13) 0.4023(12) 0.184(7) Uani 1 1 d . . .
H15A H 0.3559 -0.3347 0.3566 0.277 Uiso 1 1 calc R . .
H15B H 0.2789 -0.2273 0.3677 0.277 Uiso 1 1 calc R . .
H15C H 0.3744 -0.2568 0.4791 0.277 Uiso 1 1 calc R . .
C16 C 0.8007(11) -0.1483(8) 0.2553(9) 0.105(3) Uiso 1 1 d D . .
H16 H 0.7236 -0.2127 0.2037 0.19(3) Uiso 1 1 calc R . .
C17 C 0.8964(15) -0.3201(13) 0.3043(12) 0.155 Uiso 1 1 d . . .
H17A H 0.8468 -0.3598 0.2229 0.233 Uiso 1 1 calc R . .
H17B H 0.8462 -0.3542 0.3457 0.233 Uiso 1 1 calc R . .
H17C H 0.9881 -0.3349 0.3295 0.233 Uiso 1 1 calc R . .
C18 C 1.0429(12) -0.0983(12) 0.3854(12) 0.154 Uiso 1 1 d D . .
H18A H 1.0357 -0.0143 0.3841 0.231 Uiso 1 1 calc R . .
H18B H 1.1028 -0.1219 0.3476 0.231 Uiso 1 1 calc R . .
H18C H 1.0816 -0.1018 0.4641 0.231 Uiso 1 1 calc R . .
N1 N 0.1723(9) 0.1149(12) 0.2271(7) 0.072(3) Uani 0.50 1 d P . .
N2 N 0.5203(15) 0.4242(10) 0.2031(9) 0.080(3) Uani 0.50 1 d P . .
N3 N 0.724(2) 0.468(2) 0.4842(19) 0.068(5) Uiso 0.25 1 d P . .
N3' N 1.097(3) 0.342(2) 0.362(2) 0.076(6) Uiso 0.25 1 d P . .
N4 N 0.4815(9) -0.1640(8) 0.4076(6) 0.112(3) Uani 1 1 d . . .
N5 N 0.9088(10) -0.1819(9) 0.3272(8) 0.122(3) Uiso 1 1 d 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'
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
_geom_angle_publ_flag
O1 Tb1 O1 75.49(9) 2_655 . ?
O1 Tb1 O2 124.38(10) 2_655 . ?
O1 Tb1 O3 76.17(11) 2_655 . ?
O1 Tb1 O4 77.66(11) 2_655 2_655 ?
O1 Tb1 O5 85.99(12) 2_655 . ?
O1 Tb1 O6 133.97(10) 2_655 . ?
O1 Tb1 O7 144.54(12) 2_655 . ?
O1 Tb1 O8 82.45(14) 2_655 . ?
O1 Tb1 C1 24.95(10) . . ?
O1 Tb1 C1 100.40(11) 2_655 . ?
O1 Tb1 C9 109.66(12) 2_655 . ?
O2 Tb1 O1 49.05(9) . . ?
O2 Tb1 O5 131.46(12) . . ?
O2 Tb1 O6 81.97(11) . . ?
O2 Tb1 O7 73.14(12) . . ?
O2 Tb1 O8 142.43(14) . . ?
O2 Tb1 C1 24.11(11) . . ?
O2 Tb1 C9 107.28(13) . . ?
O3 Tb1 O1 66.34(10) . . ?
O3 Tb1 O2 77.90(12) . . ?
O3 Tb1 O4 131.04(10) . 2_655 ?
O3 Tb1 O5 74.11(13) . . ?
O3 Tb1 O6 73.89(10) . . ?
O3 Tb1 O7 139.13(12) . . ?
O3 Tb1 O8 138.41(14) . . ?
O3 Tb1 C1 70.99(11) . . ?
O3 Tb1 C9 71.56(11) . . ?
O4 Tb1 O1 67.42(10) 2_655 . ?
O4 Tb1 O2 83.95(12) 2_655 . ?
O4 Tb1 O5 143.49(12) 2_655 . ?
O4 Tb1 O6 147.46(10) 2_655 . ?
O4 Tb1 O7 73.84(11) 2_655 . ?
O4 Tb1 O8 76.44(14) 2_655 . ?
O4 Tb1 C1 74.05(11) 2_655 . ?
O4 Tb1 C9 157.16(11) 2_655 . ?
O5 Tb1 O1 139.19(13) . . ?
O5 Tb1 O6 52.60(11) . . ?
O5 Tb1 C9 25.76(13) . . ?
O6 Tb1 O1 121.00(10) . . ?
O6 Tb1 C9 26.85(12) . . ?
O7 Tb1 O1 111.38(11) . . ?
O7 Tb1 O5 104.82(14) . . ?
O7 Tb1 O6 74.04(11) . . ?
O7 Tb1 C9 90.14(12) . . ?
O8 Tb1 O5 69.13(15) . . ?
O8 Tb1 O6 97.71(14) . . ?
O8 Tb1 O7 70.77(15) . . ?
O8 Tb1 C9 83.02(14) . . ?
O8 Tb1 O1 140.73(13) . . ?
O5 Tb1 C1 141.68(12) . . ?
O6 Tb1 C1 101.88(11) . . ?
O7 Tb1 C1 91.69(12) . . ?
O8 Tb1 C1 148.93(14) . . ?
C9 Tb1 O1 134.90(11) . . ?
C9 Tb1 C1 123.62(12) . . ?
Tb1 O1 Tb1 104.51(9) 2_655 . ?
C1 O1 Tb1 170.3(3) . 2_655 ?
C1 O1 Tb1 84.6(2) . . ?
C1 O2 Tb1 105.5(2) . . ?
C5 O3 Tb1 140.7(3) . . ?
C5 O4 Tb1 133.2(3) . 2_655 ?
C9 O5 Tb1 94.0(3) . . ?
C9 O6 Tb1 92.2(2) . . ?
C13 O7 Tb1 128.1(4) . . ?
C16 O8 Tb1 133.5(6) . . ?
O1 C1 Tb1 70.4(2) . . ?
O1 C1 O2 120.8(4) . . ?
O1 C1 C2 119.6(4) . . ?
O2 C1 C2 119.5(3) . . ?
O2 C1 Tb1 50.43(19) . . ?
C2 C1 Tb1 169.4(3) . . ?
C3 C2 C1 121.0(4) . . ?
C4 C2 C1 119.1(4) . . ?
C4 C2 C3 119.9(4) . . ?
C2 C3 C4 118.5(4) . 2 ?
N1 C3 C2 124.1(5) . . ?
N1 C3 C4 117.5(5) . 2 ?
C2 C4 C3 121.6(4) . 2 ?
O3 C5 O4 125.5(3) . . ?
O3 C5 C6 117.3(4) . . ?
O4 C5 C6 117.2(4) . . ?
C7 C6 C5 120.5(4) . . ?
C8 C6 C5 119.9(4) . . ?
C8 C6 C7 119.4(4) . . ?
C6 C7 N2 123.6(5) . . ?
C8 C7 C6 118.8(4) 2_665 . ?
C8 C7 N2 117.6(6) 2_665 . ?
C6 C8 C7 121.8(4) . 2_665 ?
O5 C9 Tb1 60.3(2) . . ?
O5 C9 O6 121.2(4) . . ?
O6 C9 Tb1 61.0(2) . . ?
O5 C9 C10 120.1(4) . . ?
O6 C9 C10 118.7(4) . . ?
C10 C9 Tb1 178.8(3) . . ?
C11 C10 C9 121.1(4) . . ?
C11 C10 C12 119.3(4) . . ?
C12 C10 C9 119.6(4) . . ?
C10 C11 C12 120.9(5) . 2_766 ?
C10 C11 N3' 125.2(10) . . ?
C12 C11 N3' 112.1(10) 2_766 . ?
C10 C12 N3 125.3(11) . . ?
C11 C12 C10 119.9(5) 2_766 . ?
C11 C12 N3 114.4(11) 2_766 . ?
O7 C13 N4 127.7(8) . . ?
O8 C16 N5 125.7(10) . . ?
C13 N4 C14 119.9(8) . . ?
C13 N4 C15 126.2(9) . . ?
C15 N4 C14 113.9(8) . . ?
C16 N5 C17 115.2(10) . . ?
C16 N5 C18 121.2(10) . . ?
C18 N5 C17 119.0(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.833(3) . ?
Tb1 O1 2.323(3) 2_655 ?
Tb1 O2 2.394(3) . ?
Tb1 O3 2.358(3) . ?
Tb1 O4 2.378(3) 2_655 ?
Tb1 O5 2.452(3) . ?
Tb1 O6 2.464(3) . ?
Tb1 O7 2.439(3) . ?
Tb1 O8 2.417(3) . ?
Tb1 C1 2.993(4) . ?
Tb1 C9 2.816(4) . ?
O1 Tb1 2.323(3) 2_655 ?
O1 C1 1.268(5) . ?
O2 C1 1.269(5) . ?
O3 C5 1.263(5) . ?
O4 C5 1.267(5) . ?
O4 Tb1 2.378(3) 2_655 ?
O5 C9 1.227(6) . ?
O6 C9 1.273(5) . ?
O7 C13 1.230(7) . ?
O8 C16 1.169(7) . ?
C1 C2 1.500(5) . ?
C2 C3 1.400(5) . ?
C2 C4 1.385(6) . ?
C3 N1 1.330(9) . ?
C3 C4 1.410(6) 2 ?
C4 C3 1.410(6) 2 ?
C5 C6 1.514(5) . ?
C6 C7 1.425(6) . ?
C6 C8 1.384(6) . ?
C7 C8 1.405(6) 2_665 ?
C7 N2 1.438(11) . ?
C8 C7 1.405(6) 2_665 ?
C9 C10 1.509(5) . ?
C10 C11 1.394(7) . ?
C10 C12 1.405(7) . ?
C11 C12 1.400(6) 2_766 ?
C11 N3' 1.43(2) . ?
C12 C11 1.400(6) 2_766 ?
C12 N3 1.42(2) . ?
C13 N4 1.290(8) . ?
N4 C14 1.477(14) . ?
N4 C15 1.444(12) . ?
N5 C16 1.353(12) . ?
N5 C17 1.494(15) . ?
N5 C18 1.411(8) . ?
