#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:17:09 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143498 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/52/7035251.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_7035251
loop_
_publ_author_name
'Bag, Partha Pratim'
'Wang, Xu-Sheng'
'Cao, Rong'
_publ_section_title
;
 Microwave-assisted large scale synthesis of lanthanide metal-organic
 frameworks (Ln-MOFs), having a preferred conformation and
 photoluminescence properties.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11954
_journal_page_last               11962
_journal_paper_doi               10.1039/c5dt01598g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C30 H27 Cl N5 O14 Tb'
_chemical_formula_weight         875.94
_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
_audit_update_record
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                106.349(2)
_cell_angle_beta                 98.6290(10)
_cell_angle_gamma                100.060(2)
_cell_formula_units_Z            2
_cell_length_a                   9.53070(10)
_cell_length_b                   12.7016(3)
_cell_length_c                   18.8199(3)
_cell_measurement_reflns_used    7009
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.4400
_cell_measurement_theta_min      4.8050
_cell_volume                     2104.13(7)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20569
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    1.806
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.0825
_exptl_crystal_size_mid          0.0545
_exptl_crystal_size_min          0.0350
_platon_squeeze_details
;
;
_refine_diff_density_max         6.070
_refine_diff_density_min         -4.504
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         8882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0622
_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)+(0.1185P)²+10.0078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.1828
_reflns_number_gt                7977
_reflns_number_total             8879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01598g2.cif
_cod_data_source_block           tb_final
_cod_depositor_comments
'Adding full bibliography for 7035246--7035254.cif.'
_cod_original_cell_volume        2104.13(6)
_cod_database_code               7035251
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
Tb1 Tb -0.23336(3) 0.98367(2) -0.003313(13) 0.01807(12) Uani 1 1 d .
N2 N 0.0003(5) 0.1482(4) -0.3202(3) 0.0169(9) Uani 1 1 d .
O6 O -0.3136(4) 0.0240(4) -0.8828(2) 0.0244(10) Uani 1 1 d .
O4 O -0.1391(4) 0.0653(4) -0.0960(2) 0.0234(9) Uani 1 1 d .
O2 O 0.0087(4) 0.8907(4) -0.0738(2) 0.0207(8) Uani 1 1 d .
N1 N -0.0418(6) 0.6074(4) -0.3252(3) 0.0193(10) Uani 1 1 d .
O1 O -0.2302(5) 0.8227(4) -0.1122(2) 0.0248(9) Uani 1 1 d .
O3 O 0.1053(4) 0.1200(4) -0.0634(2) 0.0222(9) Uani 1 1 d .
N3 N -0.4334(6) 0.1668(5) -0.6321(3) 0.0281(7) Uani 1 1 d .
C10 C -0.0800(6) 0.2310(5) -0.4223(3) 0.0159(11) Uani 1 1 d .
C30 C -0.4333(6) 0.0418(5) -0.8672(3) 0.0145(10) Uani 1 1 d .
C27 C -0.4354(6) 0.0820(5) -0.7840(3) 0.0158(10) Uani 1 1 d .
C8 C -0.0945(6) 0.4184(5) -0.4257(3) 0.0164(11) Uani 1 1 d .
C28 C -0.5621(6) 0.1022(5) -0.7596(3) 0.0197(12) Uani 1 1 d .
H28 H -0.6505 0.0870 -0.7956 0.024 Uiso 1 1 calc R
O9 O 0.4007(6) -0.3680(5) -0.2890(3) 0.0406(13) Uani 1 1 d .
O8 O -0.4162(5) 0.8095(4) -0.0063(3) 0.0364(12) Uani 1 1 d .
C25 C -0.3108(6) 0.1461(6) -0.6540(3) 0.0212(12) Uani 1 1 d .
H25 H -0.2241 0.1615 -0.6169 0.025 Uiso 1 1 calc R
C13 C -0.2282(7) 0.3750(6) -0.4767(3) 0.0222(12) Uani 1 1 d .
C9 C -0.0207(6) 0.3471(5) -0.3974(3) 0.0146(10) Uani 1 1 d .
C12 C -0.2909(6) 0.2586(6) -0.4979(3) 0.0233(13) Uani 1 1 d .
C11 C -0.2182(6) 0.1861(5) -0.4717(3) 0.0209(12) Uani 1 1 d .
C1 C -0.1021(6) 0.8232(5) -0.1202(3) 0.0193(11) Uani 1 1 d .
C20 C -0.0115(6) 0.1189(5) -0.1831(3) 0.0203(12) Uani 1 1 d .
O7 O -0.2801(6) 1.1747(4) 0.0252(3) 0.0389(13) Uani 1 1 d .
C26 C -0.3089(6) 0.1029(5) -0.7294(3) 0.0184(11) Uani 1 1 d .
H26 H -0.2218 0.0874 -0.7443 0.022 Uiso 1 1 calc R
C3 C 0.0593(7) 0.7374(5) -0.2028(4) 0.0257(13) Uani 1 1 d .
H3 H 0.1424 0.7807 -0.1645 0.031 Uiso 1 1 calc R
C23 C -0.0167(6) 0.1004(5) -0.1070(3) 0.0209(12) Uani 1 1 d .
C6 C -0.1981(7) 0.6758(5) -0.2467(3) 0.0237(13) Uani 1 1 d .
H6 H -0.2940 0.6765 -0.2386 0.028 Uiso 1 1 calc R
C15 C 0.1230(7) 0.3963(5) -0.3405(4) 0.0254(13) Uani 1 1 d .
H15A H 0.1603 0.3354 -0.3275 0.038 Uiso 1 1 calc R
H15B H 0.1081 0.4493 -0.2947 0.038 Uiso 1 1 calc R
H15C H 0.1935 0.4359 -0.3626 0.038 Uiso 1 1 calc R
C17 C 0.0066(7) 0.1540(5) -0.3996(3) 0.0213(12) Uani 1 1 d .
H17A H 0.1095 0.1801 -0.4019 0.026 Uiso 1 1 calc R
H17B H -0.0304 0.0774 -0.4365 0.026 Uiso 1 1 calc R
C18 C -0.1262(6) 0.1439(5) -0.2968(4) 0.0221(12) Uani 1 1 d .
H18 H -0.2101 0.1510 -0.3279 0.027 Uiso 1 1 calc R
C2 C -0.0795(6) 0.7424(5) -0.1912(3) 0.0197(11) Uani 1 1 d .
C29 C -0.5590(6) 0.1441(6) -0.6836(3) 0.0244(13) Uani 1 1 d .
H29 H -0.6456 0.1573 -0.6671 0.029 Uiso 1 1 calc R
C21 C 0.1178(7) 0.1251(6) -0.2087(4) 0.0279(14) Uani 1 1 d .
H21 H 0.2037 0.1203 -0.1780 0.033 Uiso 1 1 calc R
C19 C -0.1339(6) 0.1295(5) -0.2282(3) 0.0206(12) Uani 1 1 d .
H19 H -0.2232 0.1267 -0.2114 0.025 Uiso 1 1 calc R
C4 C 0.0756(7) 0.6688(5) -0.2707(4) 0.0252(13) Uani 1 1 d .
H4 H 0.1706 0.6648 -0.2792 0.030 Uiso 1 1 calc R
C5 C -0.1778(7) 0.6082(5) -0.3139(3) 0.0236(12) Uani 1 1 d .
H5 H -0.2596 0.5622 -0.3522 0.028 Uiso 1 1 calc R
C7 C -0.0210(7) 0.5430(5) -0.4013(3) 0.0227(12) Uani 1 1 d .
H7A H 0.0846 0.5510 -0.3999 0.027 Uiso 1 1 calc R
H7B H -0.0610 0.5761 -0.4394 0.027 Uiso 1 1 calc R
C24 C -0.4407(7) 0.2107(7) -0.5497(3) 0.0338(17) Uani 1 1 d .
H24A H -0.4933 0.1486 -0.5348 0.041 Uiso 1 1 calc R
H24B H -0.4968 0.2702 -0.5430 0.041 Uiso 1 1 calc R
C14 C -0.3119(8) 0.4481(7) -0.5099(4) 0.0371(18) Uani 1 1 d .
H14A H -0.3882 0.4653 -0.4818 0.056 Uiso 1 1 calc R
H14B H -0.3566 0.4075 -0.5633 0.056 Uiso 1 1 calc R
H14C H -0.2449 0.5184 -0.5058 0.056 Uiso 1 1 calc R
C22 C 0.1218(7) 0.1382(6) -0.2784(4) 0.0258(13) Uani 1 1 d .
H22 H 0.2094 0.1403 -0.2968 0.031 Uiso 1 1 calc R
C16 C -0.2824(9) 0.0608(7) -0.4969(4) 0.043(2) Uani 1 1 d .
H16A H -0.2821 0.0352 -0.4524 0.064 Uiso 1 1 calc R
H16B H -0.2240 0.0212 -0.5293 0.064 Uiso 1 1 calc R
H16C H -0.3828 0.0447 -0.5254 0.064 Uiso 1 1 calc R
Cl1 Cl -0.5021(3) 0.1333(3) -0.3196(2) 0.0805(9) Uani 1 1 d .
N5 N -0.0983(6) -0.1627(5) -0.3999(3) 0.0281(7) Uani 1 1 d .
O10 O 0.3830(7) -0.3133(8) -0.1716(4) 0.068(2) Uani 1 1 d .
N4 N 0.4238(6) -0.3728(5) -0.2246(3) 0.0281(7) Uani 1 1 d .
O11 O 0.4900(7) -0.4466(6) -0.2142(4) 0.0537(9) Uani 1 1 d .
O5 O -0.5460(7) 0.0302(6) -0.9131(4) 0.0537(9) Uani 1 1 d .
O12 O -0.0090(7) -0.1093(6) -0.4261(4) 0.0537(9) Uani 1 1 d .
O14 O -0.2127(11) -0.2507(11) -0.4269(5) 0.098(3) Uani 1 1 d .
O13 O -0.0349(15) -0.1551(15) -0.3473(12) 0.237(13) 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'
Cl Cl 0.1484 0.1585 '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'
Tb Tb -0.1723 4.1537 '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'
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 Tb1 O2 144.7(2) 2_464 2_575
O5 Tb1 O3 143.1(2) 2_464 2_565
O2 Tb1 O3 72.07(15) 2_575 2_565
O5 Tb1 O6 99.99(18) 2_464 1_566
O2 Tb1 O6 83.16(14) 2_575 1_566
O3 Tb1 O6 76.86(15) 2_565 1_566
O5 Tb1 O1 78.91(19) 2_464 .
O2 Tb1 O1 120.48(14) 2_575 .
O3 Tb1 O1 81.01(15) 2_565 .
O6 Tb1 O1 140.31(16) 1_566 .
O5 Tb1 O7 73.1(2) 2_464 .
O2 Tb1 O7 74.34(15) 2_575 .
O3 Tb1 O7 136.98(16) 2_565 .
O6 Tb1 O7 73.15(18) 1_566 .
O1 Tb1 O7 140.31(17) . .
O5 Tb1 O4 79.05(19) 2_464 1_565
O2 Tb1 O4 79.03(15) 2_575 1_565
O3 Tb1 O4 124.06(14) 2_565 1_565
O6 Tb1 O4 145.37(16) 1_566 1_565
O1 Tb1 O4 73.98(16) . 1_565
O7 Tb1 O4 73.54(18) . 1_565
O5 Tb1 O8 72.0(2) 2_464 .
O2 Tb1 O8 140.02(16) 2_575 .
O3 Tb1 O8 72.15(15) 2_565 .
O6 Tb1 O8 71.88(18) 1_566 .
O1 Tb1 O8 70.14(17) . .
O7 Tb1 O8 124.34(18) . .
O4 Tb1 O8 137.26(17) 1_565 .
C18 N2 C22 122.3(5) . .
C18 N2 C17 120.0(5) . .
C22 N2 C17 117.5(5) . .
C30 O6 Tb1 130.9(3) . 1_544
C23 O4 Tb1 135.9(4) . 1_545
C1 O2 Tb1 173.8(4) . 2_575
C5 N1 C4 121.0(5) . .
C5 N1 C7 119.4(5) . .
C4 N1 C7 119.5(5) . .
C1 O1 Tb1 110.1(3) . .
C23 O3 Tb1 135.9(4) . 2_565
C25 N3 C29 120.9(6) . .
C25 N3 C24 122.2(5) . .
C29 N3 C24 116.8(5) . .
C9 C10 C11 120.2(5) . .
C9 C10 C17 119.7(5) . .
C11 C10 C17 120.0(5) . .
O5 C30 O6 126.1(5) . .
O5 C30 C27 118.1(5) . .
O6 C30 C27 115.8(4) . .
C26 C27 C28 118.2(5) . .
C26 C27 C30 120.6(5) . .
C28 C27 C30 121.2(5) . .
C13 C8 C9 120.7(5) . .
C13 C8 C7 121.2(5) . .
C9 C8 C7 118.0(5) . .
C29 C28 C27 119.9(5) . .
N3 C25 C26 120.8(5) . .
C8 C13 C12 118.8(6) . .
C8 C13 C14 123.0(6) . .
C12 C13 C14 118.2(6) . .
C10 C9 C8 119.8(5) . .
C10 C9 C15 120.3(5) . .
C8 C9 C15 120.0(5) . .
C11 C12 C13 121.3(5) . .
C11 C12 C24 119.0(6) . .
C13 C12 C24 119.7(6) . .
C12 C11 C10 119.0(5) . .
C12 C11 C16 121.3(6) . .
C10 C11 C16 119.7(6) . .
O1 C1 O2 123.7(5) . .
O1 C1 C2 118.0(5) . .
O2 C1 C2 118.3(5) . .
C21 C20 C19 118.5(5) . .
C21 C20 C23 119.9(5) . .
C19 C20 C23 121.5(5) . .
C25 C26 C27 119.7(5) . .
C4 C3 C2 119.1(6) . .
O4 C23 O3 127.9(5) . .
O4 C23 C20 116.8(5) . .
O3 C23 C20 115.3(5) . .
C5 C6 C2 120.1(6) . .
C10 C17 N2 113.3(5) . .
N2 C18 C19 119.7(5) . .
C6 C2 C3 119.2(5) . .
C6 C2 C1 119.9(5) . .
C3 C2 C1 120.8(5) . .
N3 C29 C28 120.4(5) . .
C22 C21 C20 120.1(6) . .
C18 C19 C20 120.1(5) . .
N1 C4 C3 120.6(5) . .
N1 C5 C6 119.8(6) . .
N1 C7 C8 113.0(5) . .
N3 C24 C12 112.6(5) . .
N2 C22 C21 119.3(5) . .
O13 N5 O12 101.2(10) . .
O13 N5 O14 115.3(9) . .
O12 N5 O14 137.1(7) . .
O9 N4 O10 124.1(7) . .
O9 N4 O11 116.1(6) . .
O10 N4 O11 119.8(7) . .
C30 O5 Tb1 176.7(5) . 2_464
N5 O12 O13 35.5(4) . .
N5 O13 O12 43.3(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O5 2.377(7) 2_464
Tb1 O2 2.409(4) 2_575
Tb1 O3 2.414(4) 2_565
Tb1 O6 2.448(4) 1_566
Tb1 O1 2.462(4) .
Tb1 O7 2.467(5) .
Tb1 O4 2.468(4) 1_565
Tb1 O8 2.547(5) .
N2 C18 1.342(7) .
N2 C22 1.346(8) .
N2 C17 1.526(7) .
O6 C30 1.262(7) .
O6 Tb1 2.448(4) 1_544
O4 C23 1.242(7) .
O4 Tb1 2.468(4) 1_545
O2 C1 1.265(7) .
O2 Tb1 2.409(4) 2_575
N1 C5 1.346(8) .
N1 C4 1.347(8) .
N1 C7 1.497(7) .
O1 C1 1.252(7) .
O3 C23 1.259(7) .
O3 Tb1 2.415(4) 2_565
N3 C25 1.339(8) .
N3 C29 1.353(8) .
N3 C24 1.511(8) .
C10 C9 1.397(8) .
C10 C11 1.413(8) .
C10 C17 1.493(8) .
C30 O5 1.232(8) .
C30 C27 1.507(7) .
C27 C26 1.393(7) .
C27 C28 1.395(7) .
C8 C13 1.392(8) .
C8 C9 1.407(8) .
C8 C7 1.520(8) .
C28 C29 1.372(8) .
O9 N4 1.219(8) .
C25 C26 1.375(8) .
C13 C12 1.411(10) .
C13 C14 1.523(9) .
C9 C15 1.515(7) .
C12 C11 1.395(9) .
C12 C24 1.518(8) .
C11 C16 1.510(9) .
C1 C2 1.508(8) .
C20 C21 1.387(8) .
C20 C19 1.387(8) .
C20 C23 1.521(8) .
C3 C4 1.376(9) .
C3 C2 1.382(8) .
C6 C5 1.376(8) .
C6 C2 1.378(8) .
C18 C19 1.365(8) .
C21 C22 1.373(9) .
N5 O13 1.050(15) .
N5 O12 1.241(9) .
N5 O14 1.335(13) .
O10 N4 1.229(8) .
N4 O11 1.259(9) .
O5 Tb1 2.377(7) 2_464
O12 O13 1.774(19) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.006 0.500 0.000 589.8 28.8
