#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:36:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179385 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/82/4328226.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_4328226
loop_
_publ_author_name
'Zu-Jin Lin'
'Zhen Yang'
'Tian-Fu Liu'
'Yuan-Biao Huang'
'Rong Cao'
_publ_contact_author_address
;
State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China
;
_publ_contact_author_email       linzujin@fjirsm.ac.cn
_publ_contact_author_fax         +86-0591-83796710
_publ_contact_author_name        'Zujin Lin'
_publ_contact_author_phone       +86-0591-83725186
_publ_section_title
;
 Microwave-Assisted Synthesis of a Series of Lanthanide Metal-Organic
 Frameworks and Gas Sorption Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1813
_journal_page_last               1820
_journal_paper_doi               10.1021/ic202082w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C43 H25 O16 P2 Tb2'
_chemical_formula_weight         1177.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 107.787(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.617(4)
_cell_length_b                   10.572(3)
_cell_length_c                   23.548(7)
_cell_measurement_reflns_used    9502
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.1296
_cell_volume                     3465.0(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Mercury2 (1x1 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26623
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    2.115
_exptl_absorpt_correction_T_max  0.7854
_exptl_absorpt_correction_T_min  0.7020
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1142
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.935
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0670P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                6965
_reflns_number_total             7909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202082w_si_003_05.cif
_cod_data_source_block           Tb
_cod_original_cell_volume        3465.0(16)
_cod_database_code               4328226
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Tb1 Tb 0.153943(11) 0.568541(16) 0.227971(7) 0.02639(8) Uani 1 1 d .
C1 C 0.2165(3) 0.1994(3) 0.14093(16) 0.0311(7) Uani 1 1 d .
C2 C 0.2000(4) 0.1727(4) 0.19461(19) 0.0472(11) Uani 1 1 d .
H2 H 0.1965 0.2384 0.2201 0.057 Uiso 1 1 calc R
C3 C 0.1887(4) 0.0495(4) 0.2104(2) 0.0519(13) Uani 1 1 d .
H3 H 0.1780 0.0324 0.2466 0.062 Uiso 1 1 calc R
C4 C 0.1933(3) -0.0491(4) 0.17254(19) 0.0365(9) Uani 1 1 d .
C5 C 0.2114(5) -0.0224(4) 0.1196(2) 0.0613(15) Uani 1 1 d .
H5 H 0.2165 -0.0885 0.0947 0.074 Uiso 1 1 calc R
C6 C 0.2220(4) 0.0999(4) 0.1030(2) 0.0547(13) Uani 1 1 d .
H6 H 0.2328 0.1164 0.0668 0.066 Uiso 1 1 calc R
C7 C 0.1792(3) -0.1835(4) 0.18988(18) 0.0365(8) Uani 1 1 d .
C8 C 0.3560(3) 0.4001(3) 0.14651(16) 0.0301(7) Uani 1 1 d .
C9 C 0.4277(3) 0.3099(4) 0.1597(2) 0.0432(10) Uani 1 1 d .
H9 H 0.4110 0.2248 0.1551 0.052 Uiso 1 1 calc R
C10 C 0.5229(3) 0.3427(4) 0.1793(2) 0.0452(10) Uani 1 1 d .
H10 H 0.5698 0.2801 0.1878 0.054 Uiso 1 1 calc R
C11 C 0.5493(3) 0.4687(4) 0.18643(17) 0.0350(8) Uani 1 1 d .
C12 C 0.4776(3) 0.5605(4) 0.1732(3) 0.0455(11) Uani 1 1 d .
H12 H 0.4946 0.6455 0.1780 0.055 Uiso 1 1 calc R
C13 C 0.3826(3) 0.5275(4) 0.1533(2) 0.0408(9) Uani 1 1 d .
H13 H 0.3357 0.5901 0.1442 0.049 Uiso 1 1 calc R
C14 C 0.6532(3) 0.5055(4) 0.21188(18) 0.0352(8) Uani 1 1 d .
C15 C 0.1903(3) 0.3716(4) 0.04207(15) 0.0300(7) Uani 1 1 d .
C16 C 0.2540(3) 0.3751(6) 0.00923(19) 0.0570(13) Uani 1 1 d .
H16 H 0.3199 0.3736 0.0283 0.068 Uiso 1 1 calc R
C17 C 0.2189(3) 0.3810(6) -0.05225(19) 0.0612(14) Uani 1 1 d .
H17 H 0.2622 0.3846 -0.0741 0.073 Uiso 1 1 calc R
C18 C 0.1229(3) 0.3818(4) -0.08193(15) 0.0313(7) Uani 1 1 d .
C19 C 0.0588(3) 0.3772(6) -0.04943(19) 0.0563(13) Uani 1 1 d .
H19 H -0.0070 0.3774 -0.0688 0.068 Uiso 1 1 calc R
C20 C 0.0930(3) 0.3724(6) 0.01211(18) 0.0561(13) Uani 1 1 d .
H20 H 0.0495 0.3697 0.0338 0.067 Uiso 1 1 calc R
C21 C 0.0875(3) 0.3856(4) -0.14894(15) 0.0318(7) Uani 1 1 d .
C22 C 0.0000 0.3426(7) 0.2500 0.079(3) Uani 1 2 d S
H22 H 0.0000 0.2546 0.2500 0.095 Uiso 1 2 calc SR
O1 O 0.1723(2) 0.4490(2) 0.14847(12) 0.0331(6) Uani 1 1 d .
O2 O 0.1563(2) -0.2021(3) 0.23703(13) 0.0428(7) Uani 1 1 d .
O3 O 0.1897(2) -0.2738(3) 0.15782(14) 0.0450(7) Uani 1 1 d .
O4 O 0.7172(2) 0.4218(3) 0.22001(15) 0.0430(7) Uani 1 1 d .
O5 O 0.6757(2) 0.6181(3) 0.22689(14) 0.0469(8) Uani 1 1 d .
O6 O 0.1492(2) 0.3957(3) -0.17573(12) 0.0449(7) Uani 1 1 d .
O7 O -0.0014(2) 0.3773(3) -0.17385(13) 0.0472(7) Uani 1 1 d .
O8 O 0.0703(2) 0.3884(3) 0.24082(16) 0.0509(8) Uani 1 1 d .
P1 P 0.22991(6) 0.36158(9) 0.12210(4) 0.02670(19) 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'
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'
P P 0.1023 0.0942 '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
O7 Tb1 O6 100.93(11) 3_565 4_566
O7 Tb1 O8 79.36(12) 3_565 .
O6 Tb1 O8 80.38(12) 4_566 .
O7 Tb1 O1 91.16(11) 3_565 .
O6 Tb1 O1 156.09(11) 4_566 .
O8 Tb1 O1 81.71(10) . .
O7 Tb1 O2 77.50(11) 3_565 1_565
O6 Tb1 O2 75.87(11) 4_566 1_565
O8 Tb1 O2 142.75(10) . 1_565
O1 Tb1 O2 127.30(9) . 1_565
O7 Tb1 O5 151.84(13) 3_565 2_655
O6 Tb1 O5 82.56(11) 4_566 2_655
O8 Tb1 O5 128.52(12) . 2_655
O1 Tb1 O5 96.47(11) . 2_655
O2 Tb1 O5 76.32(11) 1_565 2_655
O7 Tb1 O4 155.14(12) 3_565 2_655
O6 Tb1 O4 82.11(11) 4_566 2_655
O8 Tb1 O4 76.83(11) . 2_655
O1 Tb1 O4 78.47(10) . 2_655
O2 Tb1 O4 126.66(10) 1_565 2_655
O5 Tb1 O4 52.83(10) 2_655 2_655
O7 Tb1 O3 80.22(11) 3_565 1_565
O6 Tb1 O3 127.51(10) 4_566 1_565
O8 Tb1 O3 148.21(11) . 1_565
O1 Tb1 O3 74.60(9) . 1_565
O2 Tb1 O3 52.86(9) 1_565 1_565
O5 Tb1 O3 75.82(11) 2_655 1_565
O4 Tb1 O3 117.70(10) 2_655 1_565
O7 Tb1 C14 176.10(11) 3_565 2_655
O6 Tb1 C14 82.59(11) 4_566 2_655
O8 Tb1 C14 103.01(12) . 2_655
O1 Tb1 C14 86.14(11) . 2_655
O2 Tb1 C14 101.90(11) 1_565 2_655
O5 Tb1 C14 26.39(13) 2_655 2_655
O4 Tb1 C14 26.49(11) 2_655 2_655
O3 Tb1 C14 96.32(12) 1_565 2_655
O7 Tb1 C7 77.87(12) 3_565 1_565
O6 Tb1 C7 101.79(12) 4_566 1_565
O8 Tb1 C7 157.13(12) . 1_565
O1 Tb1 C7 100.87(11) . 1_565
O2 Tb1 C7 26.54(10) 1_565 1_565
O5 Tb1 C7 74.08(11) 2_655 1_565
O4 Tb1 C7 126.03(11) 2_655 1_565
O3 Tb1 C7 26.32(10) 1_565 1_565
C14 Tb1 C7 99.84(12) 2_655 1_565
C2 C1 C6 119.3(4) . .
C2 C1 P1 118.8(3) . .
C6 C1 P1 121.9(3) . .
C3 C2 C1 120.4(4) . .
C2 C3 C4 120.3(4) . .
C5 C4 C3 119.2(4) . .
C5 C4 C7 121.1(4) . .
C3 C4 C7 119.7(4) . .
C6 C5 C4 121.3(4) . .
C5 C6 C1 119.6(4) . .
O3 C7 O2 121.5(4) . .
O3 C7 C4 120.1(4) . .
O2 C7 C4 118.5(3) . .
O3 C7 Tb1 62.5(2) . 1_545
O2 C7 Tb1 59.0(2) . 1_545
C4 C7 Tb1 177.3(3) . 1_545
C9 C8 C13 118.3(4) . .
C9 C8 P1 123.3(3) . .
C13 C8 P1 118.5(3) . .
C10 C9 C8 121.6(4) . .
C9 C10 C11 120.1(4) . .
C10 C11 C12 118.8(4) . .
C10 C11 C14 120.5(4) . .
C12 C11 C14 120.6(4) . .
C13 C12 C11 121.0(4) . .
C12 C13 C8 120.2(4) . .
O5 C14 O4 120.3(3) . .
O5 C14 C11 120.2(4) . .
O4 C14 C11 119.5(4) . .
O5 C14 Tb1 60.0(2) . 2_655
O4 C14 Tb1 60.5(2) . 2_655
C11 C14 Tb1 173.7(3) . 2_655
C20 C15 C16 118.6(3) . .
C20 C15 P1 119.2(3) . .
C16 C15 P1 122.1(3) . .
C15 C16 C17 119.3(4) . .
C18 C17 C16 122.1(4) . .
C17 C18 C19 118.8(4) . .
C17 C18 C21 120.6(3) . .
C19 C18 C21 120.6(3) . .
C18 C19 C20 119.6(4) . .
C15 C20 C19 121.5(4) . .
O6 C21 O7 124.9(3) . .
O6 C21 C18 117.4(3) . .
O7 C21 C18 117.7(3) . .
O8 C22 O8 133.0(7) . 2
P1 O1 Tb1 151.20(17) . .
C7 O2 Tb1 94.5(2) . 1_545
C7 O3 Tb1 91.2(2) . 1_545
C14 O4 Tb1 93.0(2) . 2_655
C14 O5 Tb1 93.7(2) . 2_655
C21 O6 Tb1 138.3(3) . 4_565
C21 O7 Tb1 160.2(3) . 3_565
C22 O8 Tb1 148.8(4) . .
O1 P1 C1 111.53(16) . .
O1 P1 C15 110.75(16) . .
C1 P1 C15 106.89(17) . .
O1 P1 C8 112.08(17) . .
C1 P1 C8 108.36(17) . .
C15 P1 C8 106.98(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O7 2.278(3) 3_565
Tb1 O6 2.321(3) 4_566
Tb1 O8 2.333(3) .
Tb1 O1 2.342(3) .
Tb1 O2 2.434(3) 1_565
Tb1 O5 2.446(3) 2_655
Tb1 O4 2.459(3) 2_655
Tb1 O3 2.512(3) 1_565
Tb1 C14 2.820(4) 2_655
Tb1 C7 2.831(4) 1_565
C1 C2 1.386(5) .
C1 C6 1.398(5) .
C1 P1 1.797(4) .
C2 C3 1.378(6) .
C3 C4 1.386(6) .
C4 C5 1.380(6) .
C4 C7 1.510(5) .
C5 C6 1.373(6) .
C7 O3 1.256(5) .
C7 O2 1.269(5) .
C7 Tb1 2.831(4) 1_545
C8 C9 1.380(5) .
C8 C13 1.398(5) .
C8 P1 1.801(4) .
C9 C10 1.370(5) .
C10 C11 1.383(6) .
C11 C12 1.391(6) .
C11 C14 1.505(5) .
C12 C13 1.368(6) .
C14 O5 1.256(6) .
C14 O4 1.260(5) .
C14 Tb1 2.820(4) 2_655
C15 C20 1.381(5) .
C15 C16 1.381(5) .
C15 P1 1.798(4) .
C16 C17 1.382(6) .
C17 C18 1.364(6) .
C18 C19 1.379(5) .
C18 C21 1.504(5) .
C19 C20 1.382(6) .
C21 O6 1.254(5) .
C21 O7 1.255(5) .
C22 O8 1.213(4) .
C22 O8 1.213(4) 2
O1 P1 1.505(3) .
O2 Tb1 2.434(3) 1_545
O3 Tb1 2.512(3) 1_545
O4 Tb1 2.459(3) 2_655
O5 Tb1 2.446(3) 2_655
O6 Tb1 2.321(3) 4_565
O7 Tb1 2.278(3) 3_565
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 0.406 -0.086 0.418 1844.7 246.5
