#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:52:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180402 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/71/7207157.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_7207157
loop_
_publ_author_name
'Gao, Ming-Juan'
'Yang, Ping'
'Cai, Bin'
'Dai, Jing-Wei'
'Wu, Jian-Zhong'
'Yu, Ying'
_publ_section_title
;
 Spontaneous resolution of lanthanide coordination polymers with
 2-hydroxypyrimidine-4,6-dicarboxylic acid
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              1264
_journal_paper_doi               10.1039/c1ce06090b
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C6 H5 N2 O7 Tb, 1.13(H2 O), 0.4(O), 0.8(H)'
_chemical_formula_sum            'C6 H8.06 N2 O8.53 Tb'
_chemical_formula_weight         403.65
_chemical_name_systematic
;
?
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_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                120.00
_cell_formula_units_Z            9
_cell_length_a                   12.4040(10)
_cell_length_b                   12.4040(10)
_cell_length_c                   19.6075(16)
_cell_measurement_reflns_used    4623
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.81
_cell_volume                     2612.6(4)
_computing_cell_refinement       'APEX2 (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'APEX2 (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4781
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    6.129
_exptl_absorpt_correction_T_max  0.7916
_exptl_absorpt_correction_T_min  0.2987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1722
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.019(12)
_refine_ls_extinction_coef       0.00163(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0123
_refine_ls_R_factor_gt           0.0122
_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)+(0.0120P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0303
_refine_ls_wR_factor_ref         0.0303
_reflns_number_gt                1151
_reflns_number_total             1154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce06090b.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               7207157
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
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
C1 C 0.1103(3) 0.2235(3) 0.22083(12) 0.0200(6) Uani 1 1 d .
C2 C 0.0817(3) 0.2812(3) 0.28095(18) 0.0190(9) Uani 1 1 d .
C3 C 0.1670(4) 0.3333 0.3333 0.0253(12) Uani 1 2 d S
H3 H 0.2420 0.3333 0.3333 0.030 Uiso 1 2 calc SR
C4 C -0.0539(4) 0.3333 0.3333 0.0158(9) Uani 1 2 d S
N1 N -0.0264(2) 0.2800(2) 0.27951(12) 0.0153(5) Uani 1 1 d .
O1 O 0.2030(2) 0.2105(3) 0.22569(11) 0.0326(6) Uani 1 1 d .
O2 O 0.0402(2) 0.1961(2) 0.16979(11) 0.0277(6) Uani 1 1 d .
O3 O -0.1547(3) 0.3333 0.3333 0.0224(7) Uani 1 2 d S
O1W O 0.20622(19) 0.1759(2) 0.08388(11) 0.0209(5) Uani 1 1 d .
H1W H 0.1339 0.1619 0.0892 0.031 Uiso 1 1 d R
H2W H 0.2019 0.1426 0.0468 0.031 Uiso 1 1 d R
O2W O 0.2591(9) 0.4569(8) 0.1014(6) 0.169(7) Uani 0.567(16) 1 d P
H3W H 0.2177 0.3799 0.1113 0.253 Uiso 0.567(16) 1 d PR
H4W H 0.2566 0.4975 0.1336 0.253 Uiso 0.567(16) 1 d PR
O3W O 0.3333 0.6667 0.0193(7) 0.116(6) Uani 0.597(18) 3 d SP
H5W H 0.3509 0.6155 0.0402 0.174 Uiso 0.199(6) 1 d PR
H6W H 0.3939 0.7395 0.0131 0.174 Uiso 0.199(6) 1 d PR
Tb1 Tb 0.3333 0.156561(19) 0.1667 0.00943(7) Uani 1 2 d S
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
O1 C1 O2 125.9(3) . .
O1 C1 C2 117.0(3) . .
O2 C1 C2 117.1(3) . .
N1 C2 C3 123.5(3) . .
N1 C2 C1 116.8(3) . .
C3 C2 C1 119.7(3) . .
C2 C3 C2 115.7(5) 17 .
C2 C3 H3 122.1 17 .
C2 C3 H3 122.1 . .
O3 C4 N1 119.2(2) . .
O3 C4 N1 119.2(2) . 17
N1 C4 N1 121.5(4) . 17
C2 N1 C4 117.9(3) . .
C2 N1 Tb1 112.81(19) . 2
C4 N1 Tb1 129.2(2) . 2
C1 O1 Tb1 144.63(19) . .
C1 O2 Tb1 126.6(2) . 2
Tb1 O1W H1W 126.9 . .
Tb1 O1W H2W 115.9 . .
H1W O1W H2W 102.2 . .
H3W O2W H4W 109.1 . .
H5W O3W H6W 115.7 . .
O2 Tb1 O2 109.79(13) 11 3
O2 Tb1 O1 82.02(10) 11 12
O2 Tb1 O1 149.86(7) 3 12
O2 Tb1 O1 149.85(7) 11 .
O2 Tb1 O1 82.02(10) 3 .
O1 Tb1 O1 101.74(15) 12 .
O2 Tb1 O1W 134.95(7) 11 .
O2 Tb1 O1W 78.19(8) 3 .
O1 Tb1 O1W 74.37(8) 12 .
O1 Tb1 O1W 73.67(7) . .
O2 Tb1 O1W 78.19(8) 11 12
O2 Tb1 O1W 134.94(7) 3 12
O1 Tb1 O1W 73.66(8) 12 12
O1 Tb1 O1W 74.37(8) . 12
O1W Tb1 O1W 128.27(11) . 12
O2 Tb1 N1 64.94(7) 11 11
O2 Tb1 N1 78.33(8) 3 11
O1 Tb1 N1 82.38(9) 12 11
O1 Tb1 N1 145.04(7) . 11
O1W Tb1 N1 74.19(7) . 11
O1W Tb1 N1 138.36(8) 12 11
O2 Tb1 N1 78.33(8) 11 3
O2 Tb1 N1 64.93(7) 3 3
O1 Tb1 N1 145.04(7) 12 3
O1 Tb1 N1 82.37(9) . 3
O1W Tb1 N1 138.36(8) . 3
O1W Tb1 N1 74.19(7) 12 3
N1 Tb1 N1 114.06(11) 11 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.242(5) .
C1 O2 1.256(4) .
C1 C2 1.510(4) .
C2 N1 1.334(4) .
C2 C3 1.382(4) .
C3 C2 1.382(4) 17
C3 H3 0.9300 .
C4 O3 1.250(6) .
C4 N1 1.376(3) .
C4 N1 1.376(3) 17
N1 Tb1 2.660(2) 2
O1 Tb1 2.341(2) .
O2 Tb1 2.330(2) 2
O1W Tb1 2.357(2) .
O1W H1W 0.8310 .
O1W H2W 0.8247 .
O2W H3W 0.8500 .
O2W H4W 0.8181 .
O3W H5W 0.8696 .
O3W H6W 0.8467 .
Tb1 O2 2.330(2) 11
Tb1 O2 2.330(2) 3
Tb1 O1 2.341(2) 12
Tb1 O1W 2.357(2) 12
Tb1 N1 2.660(2) 11
Tb1 N1 2.660(2) 3
