#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:26:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179896 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/92/7019270.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_7019270
loop_
_publ_author_name
'Ibarra, Ilich A.'
'Hesterberg, Travis W.'
'Holliday, Bradley J.'
'Lynch, Vincent M.'
'Humphrey, Simon M.'
_publ_section_title
;
 Gas sorption and luminescence properties of a terbium(iii)-phosphine
 oxide coordination material with two-dimensional pore topology.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8003
_journal_page_last               8009
_journal_paper_doi               10.1039/c2dt30138e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C21 H14 O7 P Tb, C3 H7 N O, 2(H2 O)'
_chemical_formula_sum            'C24 H25 N O10 P Tb'
_chemical_formula_weight         671.29
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.185(5)
_cell_length_b                   12.100(2)
_cell_length_c                   20.605(4)
_cell_measurement_reflns_used    15879
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.5
_cell_volume                     6778(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1849
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60180
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS: Area-Detector Absorption Correction. (1996)
Siemens Industrial Automation, Inc.: Madison, WI.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5944
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0795
_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)+(0.0730P)²+21.9981P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1894
_reflns_number_gt                3576
_reflns_number_total             5944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30138e.txt
_cod_data_source_block           sh11018
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               7019270
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
P1 P 0.89206(12) 0.1218(2) 0.09595(14) 0.0286(7) Uani 1 1 d .
Tb1 Tb 0.57143(2) 0.11089(4) 0.02225(3) 0.0295(2) Uani 1 1 d .
O1P O 0.9202(3) 0.2079(5) 0.0592(4) 0.0306(19) Uani 1 1 d .
O1 O 0.9176(3) -0.4205(6) 0.0360(4) 0.047(3) Uani 1 1 d .
O2 O 0.9904(3) -0.3655(6) 0.0024(4) 0.042(2) Uani 1 1 d .
O3 O 0.9348(3) 0.0368(6) 0.4135(3) 0.042(2) Uani 1 1 d .
O4 O 0.9210(3) 0.2173(6) 0.4195(4) 0.036(2) Uani 1 1 d .
O5 O 0.6410(3) 0.0982(6) 0.0980(4) 0.036(2) Uani 1 1 d .
O6 O 0.6566(3) 0.1020(7) -0.0078(3) 0.037(2) Uani 1 1 d .
O7 O 0.5251(4) 0.0754(7) 0.1191(4) 0.049(3) Uani 1 1 d .
C1 C 0.9085(4) -0.0156(9) 0.0709(5) 0.027(3) Uani 1 1 d .
C2 C 0.8734(5) -0.0969(9) 0.0657(7) 0.053(4) Uani 1 1 d .
H2A H 0.8396 -0.0795 0.0714 0.064 Uiso 1 1 calc R
C3 C 0.8877(5) -0.2059(10) 0.0519(8) 0.057(4) Uani 1 1 d .
H3A H 0.8638 -0.2630 0.0505 0.069 Uiso 1 1 calc R
C4 C 0.9350(4) -0.2298(9) 0.0408(5) 0.029(3) Uiso 1 1 d .
C5 C 0.9708(5) -0.1480(9) 0.0442(6) 0.044(3) Uani 1 1 d .
H5A H 1.0044 -0.1651 0.0371 0.053 Uiso 1 1 calc R
C6 C 0.9565(5) -0.0426(9) 0.0580(6) 0.038(3) Uani 1 1 d .
H6A H 0.9807 0.0141 0.0586 0.045 Uiso 1 1 calc R
C7 C 0.9492(4) -0.3471(9) 0.0254(6) 0.032(3) Uani 1 1 d .
C8 C 0.9039(5) 0.1252(8) 0.1820(5) 0.032(3) Uani 1 1 d .
C9 C 0.9105(6) 0.0262(11) 0.2156(6) 0.058(4) Uani 1 1 d .
H9A H 0.9103 -0.0423 0.1930 0.070 Uiso 1 1 calc R
C10 C 0.9173(6) 0.0287(10) 0.2824(6) 0.051(4) Uani 1 1 d .
H10H H 0.9210 -0.0386 0.3057 0.062 Uiso 1 1 calc R
C11 C 0.9189(5) 0.1293(9) 0.3155(5) 0.036(3) Uani 1 1 d .
C12 C 0.9152(6) 0.2261(10) 0.2807(7) 0.060(5) Uani 1 1 d .
H12A H 0.9168 0.2954 0.3023 0.072 Uiso 1 1 calc R
C13 C 0.9090(6) 0.2216(9) 0.2129(6) 0.048(4) Uani 1 1 d .
H13A H 0.9084 0.2883 0.1886 0.058 Uiso 1 1 calc R
C14 C 0.9257(5) 0.1309(9) 0.3869(5) 0.033(3) Uani 1 1 d .
C15 C 0.8275(5) 0.1265(8) 0.0856(5) 0.033(3) Uani 1 1 d .
C16 C 0.7930(5) 0.1179(10) 0.1374(6) 0.040(3) Uani 1 1 d .
H16A H 0.8048 0.1171 0.1808 0.048 Uiso 1 1 calc R
C17 C 0.7430(5) 0.1106(11) 0.1265(6) 0.045(3) Uani 1 1 d .
H17A H 0.7205 0.1073 0.1618 0.053 Uiso 1 1 calc R
C18 C 0.7264(4) 0.1082(9) 0.0630(5) 0.033(3) Uani 1 1 d .
C19 C 0.7589(5) 0.1151(11) 0.0114(6) 0.045(3) Uani 1 1 d .
H19A H 0.7470 0.1125 -0.0319 0.054 Uiso 1 1 calc R
C20 C 0.8094(4) 0.1259(9) 0.0235(6) 0.037(3) Uani 1 1 d .
H20A H 0.8315 0.1329 -0.0120 0.044 Uiso 1 1 calc R
C21 C 0.6719(4) 0.1013(9) 0.0508(6) 0.032(3) Uani 1 1 d .
O100 O 0.5536(8) 0.016(2) 0.2425(11) 0.210(9) Uiso 1 1 d D
N100 N 0.5589(10) -0.103(2) 0.3345(13) 0.35(3) Uiso 1 1 d D
C102 C 0.5451(10) -0.204(2) 0.3593(11) 0.137(9) Uiso 1 1 d D
H10A H 0.5255 -0.2439 0.3269 0.205 Uiso 1 1 calc R
H10B H 0.5253 -0.1928 0.3986 0.205 Uiso 1 1 calc R
H10C H 0.5745 -0.2470 0.3700 0.205 Uiso 1 1 calc R
C101 C 0.5850(15) -0.027(3) 0.3719(18) 0.30(2) Uiso 1 1 d D
H10D H 0.5917 0.0390 0.3461 0.453 Uiso 1 1 calc R
H10E H 0.6161 -0.0606 0.3858 0.453 Uiso 1 1 calc R
H10F H 0.5655 -0.0072 0.4101 0.453 Uiso 1 1 calc R
C100 C 0.5448(11) -0.081(3) 0.2720(13) 0.31(3) Uiso 1 1 d D
H10G H 0.5280 -0.1368 0.2485 0.374 Uiso 1 1 calc R
O50 O 0.3307(14) 0.119(3) 0.0903(16) 0.148(12) Uiso 0.50 1 d P
O51 O 0.6620(17) 0.896(3) 0.187(2) 0.193(17) Uiso 0.50 1 d P
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
O1P P1 C15 115.0(5) . .
O1P P1 C1 111.8(5) . .
C15 P1 C1 104.0(5) . .
O1P P1 C8 113.0(5) . .
C15 P1 C8 107.2(6) . .
C1 P1 C8 105.0(5) . .
O2 Tb1 O1P 92.8(3) 6_565 2_655
O2 Tb1 O1 105.9(3) 6_565 2_645
O1P Tb1 O1 150.9(3) 2_655 2_645
O2 Tb1 O7 72.6(3) 6_565 .
O1P Tb1 O7 87.0(3) 2_655 .
O1 Tb1 O7 77.9(3) 2_645 .
O2 Tb1 O6 151.8(3) 6_565 .
O1P Tb1 O6 91.8(3) 2_655 .
O1 Tb1 O6 82.2(3) 2_645 .
O7 Tb1 O6 135.5(3) . .
O2 Tb1 O3 76.8(3) 6_565 8_755
O1P Tb1 O3 131.1(2) 2_655 8_755
O1 Tb1 O3 75.9(3) 2_645 8_755
O7 Tb1 O3 131.9(3) . 8_755
O6 Tb1 O3 79.2(3) . 8_755
O2 Tb1 O5 153.3(3) 6_565 .
O1P Tb1 O5 77.1(3) 2_655 .
O1 Tb1 O5 76.3(3) 2_645 .
O7 Tb1 O5 82.2(3) . .
O6 Tb1 O5 54.4(2) . .
O3 Tb1 O5 128.3(3) 8_755 .
O2 Tb1 O4 80.0(3) 6_565 8_755
O1P Tb1 O4 77.5(2) 2_655 8_755
O1 Tb1 O4 127.0(3) 2_645 8_755
O7 Tb1 O4 147.6(3) . 8_755
O6 Tb1 O4 74.0(3) . 8_755
O3 Tb1 O4 53.8(3) 8_755 8_755
O5 Tb1 O4 120.6(3) . 8_755
O2 Tb1 C21 175.1(3) 6_565 .
O1P Tb1 C21 82.8(3) 2_655 .
O1 Tb1 C21 79.0(3) 2_645 .
O7 Tb1 C21 109.3(3) . .
O6 Tb1 C21 27.1(3) . .
O3 Tb1 C21 104.4(3) 8_755 .
O5 Tb1 C21 27.4(3) . .
O4 Tb1 C21 96.9(3) 8_755 .
O2 Tb1 C14 78.1(3) 6_565 8_755
O1P Tb1 C14 104.0(3) 2_655 8_755
O1 Tb1 C14 101.7(3) 2_645 8_755
O7 Tb1 C14 149.2(3) . 8_755
O6 Tb1 C14 73.7(3) . 8_755
O3 Tb1 C14 27.4(3) 8_755 8_755
O5 Tb1 C14 128.1(3) . 8_755
O4 Tb1 C14 26.5(3) 8_755 8_755
C21 Tb1 C14 100.7(4) . 8_755
P1 O1P Tb1 150.3(5) . 2_655
C7 O1 Tb1 126.1(8) . 2_645
C7 O2 Tb1 169.7(8) . 6_655
C14 O3 Tb1 93.0(7) . 8_756
C14 O4 Tb1 90.9(6) . 8_756
C21 O5 Tb1 91.2(7) . .
C21 O6 Tb1 94.1(7) . .
C6 C1 C2 118.3(11) . .
C6 C1 P1 120.9(8) . .
C2 C1 P1 120.8(9) . .
C1 C2 C3 119.7(12) . .
C1 C2 H2A 120.2 . .
C3 C2 H2A 120.2 . .
C4 C3 C2 120.3(12) . .
C4 C3 H3A 119.9 . .
C2 C3 H3A 119.9 . .
C3 C4 C5 120.7(11) . .
C3 C4 C7 119.0(10) . .
C5 C4 C7 120.3(11) . .
C6 C5 C4 118.6(12) . .
C6 C5 H5A 120.7 . .
C4 C5 H5A 120.7 . .
C5 C6 C1 122.3(11) . .
C5 C6 H6A 118.9 . .
C1 C6 H6A 118.9 . .
O2 C7 O1 123.9(10) . .
O2 C7 C4 118.9(10) . .
O1 C7 C4 117.2(10) . .
C13 C8 C9 120.0(11) . .
C13 C8 P1 120.5(8) . .
C9 C8 P1 119.5(8) . .
C10 C9 C8 119.4(11) . .
C10 C9 H9A 120.3 . .
C8 C9 H9A 120.3 . .
C9 C10 C11 120.5(11) . .
C9 C10 H10H 119.7 . .
C11 C10 H10H 119.7 . .
C12 C11 C10 119.0(11) . .
C12 C11 C14 120.9(10) . .
C10 C11 C14 120.1(10) . .
C11 C12 C13 119.5(11) . .
C11 C12 H12A 120.3 . .
C13 C12 H12A 120.3 . .
C8 C13 C12 121.3(11) . .
C8 C13 H13A 119.4 . .
C12 C13 H13A 119.4 . .
O4 C14 O3 122.1(10) . .
O4 C14 C11 122.2(9) . .
O3 C14 C11 115.7(10) . .
O4 C14 Tb1 62.6(6) . 8_756
O3 C14 Tb1 59.6(5) . 8_756
C11 C14 Tb1 172.1(9) . 8_756
C20 C15 C16 117.7(12) . .
C20 C15 P1 117.9(10) . .
C16 C15 P1 124.0(9) . .
C17 C16 C15 122.0(12) . .
C17 C16 H16A 119.0 . .
C15 C16 H16A 119.0 . .
C16 C17 C18 118.4(12) . .
C16 C17 H17A 120.8 . .
C18 C17 H17A 120.8 . .
C17 C18 C19 121.2(12) . .
C17 C18 C21 118.6(11) . .
C19 C18 C21 120.2(11) . .
C18 C19 C20 119.6(11) . .
C18 C19 H19A 120.2 . .
C20 C19 H19A 120.2 . .
C15 C20 C19 121.1(12) . .
C15 C20 H20A 119.5 . .
C19 C20 H20A 119.5 . .
O6 C21 O5 120.1(11) . .
O6 C21 C18 118.6(11) . .
O5 C21 C18 121.3(11) . .
O6 C21 Tb1 58.8(6) . .
O5 C21 Tb1 61.4(6) . .
C18 C21 Tb1 173.9(8) . .
C100 N100 C102 116.4(17) . .
C100 N100 C101 122.4(17) . .
C102 N100 C101 121.1(17) . .
N100 C102 H10A 109.5 . .
N100 C102 H10B 109.5 . .
H10A C102 H10B 109.5 . .
N100 C102 H10C 109.5 . .
H10A C102 H10C 109.5 . .
H10B C102 H10C 109.5 . .
N100 C101 H10D 109.5 . .
N100 C101 H10E 109.5 . .
H10D C101 H10E 109.5 . .
N100 C101 H10F 109.5 . .
H10D C101 H10F 109.5 . .
H10E C101 H10F 109.5 . .
O100 C100 N100 123(2) . .
O100 C100 H10G 118.4 . .
N100 C100 H10G 118.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O1P 1.497(8) .
P1 C15 1.770(13) .
P1 C1 1.797(11) .
P1 C8 1.802(11) .
Tb1 O2 2.278(9) 6_565
Tb1 O1P 2.333(7) 2_655
Tb1 O1 2.340(7) 2_645
Tb1 O7 2.398(8) .
Tb1 O6 2.399(8) .
Tb1 O3 2.420(7) 8_755
Tb1 O5 2.457(8) .
Tb1 O4 2.486(7) 8_755
Tb1 C21 2.797(12) .
Tb1 C14 2.800(11) 8_755
O1P Tb1 2.333(7) 2_655
O1 C7 1.255(14) .
O1 Tb1 2.340(7) 2_645
O2 C7 1.238(13) .
O2 Tb1 2.278(9) 6_655
O3 C14 1.289(12) .
O3 Tb1 2.420(7) 8_756
O4 C14 1.249(12) .
O4 Tb1 2.486(7) 8_756
O5 C21 1.287(14) .
O6 C21 1.277(13) .
C1 C6 1.372(16) .
C1 C2 1.375(15) .
C2 C3 1.405(15) .
C2 H2A 0.9500 .
C3 C4 1.337(17) .
C3 H3A 0.9500 .
C4 C5 1.388(15) .
C4 C7 1.504(15) .
C5 C6 1.362(16) .
C5 H5A 0.9500 .
C6 H6A 0.9500 .
C8 C13 1.336(15) .
C8 C9 1.395(16) .
C9 C10 1.388(17) .
C9 H9A 0.9500 .
C10 C11 1.397(16) .
C10 H10H 0.9500 .
C11 C12 1.378(16) .
C11 C14 1.482(15) .
C12 C13 1.409(17) .
C12 H12A 0.9500 .
C13 H13A 0.9500 .
C14 Tb1 2.800(11) 8_756
C15 C20 1.371(15) .
C15 C16 1.425(17) .
C16 C17 1.381(17) .
C16 H16A 0.9500 .
C17 C18 1.385(16) .
C17 H17A 0.9500 .
C18 C19 1.384(17) .
C18 C21 1.504(16) .
C19 C20 1.403(17) .
C19 H19A 0.9500 .
C20 H20A 0.9500 .
O100 C100 1.34(2) .
N100 C100 1.37(2) .
N100 C102 1.378(19) .
N100 C101 1.39(2) .
C102 H10A 0.9800 .
C102 H10B 0.9800 .
C102 H10C 0.9800 .
C101 H10D 0.9800 .
C101 H10E 0.9800 .
C101 H10F 0.9800 .
C100 H10G 0.9500 .
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
_platon_squeeze_void_content
1 0.250 0.147 0.133 1070 308 ' '
2 0.750 -0.156 0.370 1070 306 ' '
