#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/62/4506278.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_4506278
loop_
_publ_author_name
'Wang, Hao'
'Liu, Sui-Jun'
'Tian, Dan'
'Jia, Ji-Min'
'Hu, Tong-Liang'
_publ_section_title
;
 Temperature-Dependent Structures of Lanthanide Metal--Organic Frameworks
 Based on Furan-2,5-Dicarboxylate and Oxalate
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3263
_journal_paper_doi               10.1021/cg3004036
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C7 H6 O9 Pr,H2 O'
_chemical_formula_sum            'C7 H8 O10 Pr'
_chemical_formula_weight         393.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4786(15)
_cell_length_b                   9.832(2)
_cell_length_c                   15.487(5)
_cell_measurement_reflns_used    10209
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.30
_cell_volume                     1081.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       ω
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9264
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         3.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.555
_exptl_absorpt_correction_T_max  0.4627
_exptl_absorpt_correction_T_min  0.3727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Higashi,1995
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         1938
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0274
_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)+(0.0263P)²+2.3268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                1705
_reflns_number_total             1938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3004036_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4506278
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
O7 O 0.7232(4) 0.5717(3) 0.5187(2) 0.0180(7) Uani 1 1 d .
Pr1 Pr 0.27505(3) 0.44453(2) 0.643662(16) 0.01234(9) Uani 1 1 d D
O1 O 0.1593(5) 0.6650(3) 0.5784(2) 0.0211(7) Uani 1 1 d .
O1W O 0.0039(5) 0.5285(3) 0.6939(2) 0.0209(8) Uani 1 1 d D
O2 O -0.0033(5) 0.6906(3) 0.4309(2) 0.0233(8) Uani 1 1 d .
O2W O 0.2367(5) 0.2744(4) 0.7618(3) 0.0309(9) Uani 1 1 d D
O3 O 0.3024(4) 0.9160(3) 0.5859(2) 0.0165(7) Uani 1 1 d .
O4 O 0.4798(4) 1.2510(3) 0.6410(2) 0.0196(7) Uani 1 1 d .
O5 O 0.5478(5) 1.0590(3) 0.7211(2) 0.0228(8) Uani 1 1 d .
O6 O 0.5541(4) 0.5490(3) 0.6141(2) 0.0222(8) Uani 1 1 d .
C1 C 0.1108(6) 0.7298(5) 0.5046(3) 0.0140(10) Uani 1 1 d .
C2 C 0.1901(6) 0.8678(5) 0.5042(3) 0.0140(10) Uani 1 1 d .
C3 C 0.1668(7) 0.9627(5) 0.4387(3) 0.0230(11) Uani 1 1 d .
H3 H 0.0988 0.9532 0.3774 0.028 Uiso 1 1 calc R
C4 C 0.2671(7) 1.0802(5) 0.4820(3) 0.0212(11) Uani 1 1 d .
H4 H 0.2763 1.1630 0.4547 0.025 Uiso 1 1 calc R
C5 C 0.3465(6) 1.0470(4) 0.5711(3) 0.0143(9) Uani 1 1 d .
C6 C 0.4663(6) 1.1234(5) 0.6503(3) 0.0148(10) Uani 1 1 d .
C7 C 0.5801(6) 0.5348(4) 0.5384(3) 0.0133(10) Uani 1 1 d .
O3W O 0.1503(5) 0.8209(4) 0.7426(3) 0.0303(9) Uani 1 1 d D
H1WA H -0.044(6) 0.468(4) 0.718(4) 0.046 Uiso 1 1 d D
H1WB H -0.086(5) 0.560(5) 0.649(2) 0.046 Uiso 1 1 d D
H2WB H 0.315(5) 0.216(4) 0.790(3) 0.046 Uiso 1 1 d D
H2WA H 0.128(4) 0.250(5) 0.766(3) 0.046 Uiso 1 1 d D
H3WA H 0.146(8) 0.797(6) 0.6905(18) 0.046 Uiso 1 1 d D
H3WB H 0.251(5) 0.798(6) 0.782(3) 0.046 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 '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
C7 O7 Pr1 119.7(3) . 3_666
O5 Pr1 O2 146.99(12) 2_646 3_566
O5 Pr1 O1 88.34(11) 2_646 .
O2 Pr1 O1 99.00(11) 3_566 .
O5 Pr1 O4 101.78(11) 2_646 1_545
O2 Pr1 O4 90.07(11) 3_566 1_545
O1 Pr1 O4 145.84(11) . 1_545
O5 Pr1 O6 72.57(11) 2_646 .
O2 Pr1 O6 140.44(11) 3_566 .
O1 Pr1 O6 76.45(11) . .
O4 Pr1 O6 75.73(11) 1_545 .
O5 Pr1 O7 136.97(11) 2_646 3_666
O2 Pr1 O7 75.77(11) 3_566 3_666
O1 Pr1 O7 75.82(11) . 3_666
O4 Pr1 O7 74.67(11) 1_545 3_666
O6 Pr1 O7 64.94(10) . 3_666
O5 Pr1 O1W 81.55(12) 2_646 .
O2 Pr1 O1W 71.87(11) 3_566 .
O1 Pr1 O1W 67.77(11) . .
O4 Pr1 O1W 145.54(11) 1_545 .
O6 Pr1 O1W 136.08(11) . .
O7 Pr1 O1W 125.67(11) 3_666 .
O5 Pr1 O2W 80.58(13) 2_646 .
O2 Pr1 O2W 73.39(12) 3_566 .
O1 Pr1 O2W 140.68(11) . .
O4 Pr1 O2W 73.47(11) 1_545 .
O6 Pr1 O2W 133.49(11) . .
O7 Pr1 O2W 135.03(12) 3_666 .
O1W Pr1 O2W 73.30(11) . .
C1 O1 Pr1 142.3(3) . .
Pr1 O1W H1WA 114(3) . .
Pr1 O1W H1WB 111(3) . .
H1WA O1W H1WB 106(4) . .
C1 O2 Pr1 147.2(3) . 3_566
Pr1 O2W H2WB 127(3) . .
Pr1 O2W H2WA 123(2) . .
H2WB O2W H2WA 107(4) . .
C2 O3 C5 106.4(3) . .
C6 O4 Pr1 133.8(3) . 1_565
C6 O5 Pr1 175.7(3) . 2_656
C7 O6 Pr1 120.7(3) . .
O2 C1 O1 126.3(4) . .
O2 C1 C2 115.9(4) . .
O1 C1 C2 117.8(4) . .
C3 C2 O3 110.7(4) . .
C3 C2 C1 132.8(4) . .
O3 C2 C1 116.4(4) . .
C2 C3 C4 106.4(4) . .
C2 C3 H3 126.8 . .
C4 C3 H3 126.8 . .
C5 C4 C3 106.3(4) . .
C5 C4 H4 126.8 . .
C3 C4 H4 126.8 . .
C4 C5 O3 110.2(4) . .
C4 C5 C6 132.8(4) . .
O3 C5 C6 117.1(4) . .
O5 C6 O4 124.5(5) . .
O5 C6 C5 118.3(4) . .
O4 C6 C5 117.2(4) . .
O6 C7 O7 126.1(4) . .
O6 C7 C7 117.0(5) . 3_666
O7 C7 C7 116.8(5) . 3_666
H3WA O3W H3WB 113(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O7 C7 1.255(5) .
O7 Pr1 2.523(3) 3_666
Pr1 O5 2.381(3) 2_646
Pr1 O2 2.399(3) 3_566
Pr1 O1 2.433(3) .
Pr1 O4 2.451(3) 1_545
Pr1 O6 2.494(3) .
Pr1 O7 2.523(3) 3_666
Pr1 O1W 2.528(3) .
Pr1 O2W 2.562(4) .
O1 C1 1.258(5) .
O1W H1WA 0.838(19) .
O1W H1WB 0.859(19) .
O2 C1 1.252(6) .
O2 Pr1 2.399(3) 3_566
O2W H2WB 0.836(19) .
O2W H2WA 0.864(19) .
O3 C2 1.365(5) .
O3 C5 1.367(5) .
O4 C6 1.270(6) .
O4 Pr1 2.451(3) 1_565
O5 C6 1.246(5) .
O5 Pr1 2.381(3) 2_656
O6 C7 1.255(5) .
C1 C2 1.482(6) .
C2 C3 1.348(7) .
C3 C4 1.425(7) .
C3 H3 0.9300 .
C4 C5 1.359(7) .
C4 H4 0.9300 .
C5 C6 1.477(6) .
C7 C7 1.557(8) 3_666
O3W H3WA 0.833(19) .
O3W H3WB 0.84(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O5 Pr1 O1 C1 145.8(5) 2_646 .
O2 Pr1 O1 C1 -66.6(5) 3_566 .
O4 Pr1 O1 C1 37.0(6) 1_545 .
O6 Pr1 O1 C1 73.3(5) . .
O7 Pr1 O1 C1 6.2(5) 3_666 .
O1W Pr1 O1 C1 -132.7(5) . .
O2W Pr1 O1 C1 -141.3(5) . .
O5 Pr1 O6 C7 179.5(4) 2_646 .
O2 Pr1 O6 C7 -0.2(4) 3_566 .
O1 Pr1 O6 C7 -88.0(3) . .
O4 Pr1 O6 C7 72.0(3) 1_545 .
O7 Pr1 O6 C7 -7.5(3) 3_666 .
O1W Pr1 O6 C7 -123.8(3) . .
O2W Pr1 O6 C7 121.8(3) . .
Pr1 O2 C1 O1 28.9(9) 3_566 .
Pr1 O2 C1 C2 -149.1(4) 3_566 .
Pr1 O1 C1 O2 50.6(7) . .
Pr1 O1 C1 C2 -131.5(4) . .
C5 O3 C2 C3 1.6(5) . .
C5 O3 C2 C1 -175.2(4) . .
O2 C1 C2 C3 -1.1(8) . .
O1 C1 C2 C3 -179.3(5) . .
O2 C1 C2 O3 174.8(4) . .
O1 C1 C2 O3 -3.4(6) . .
O3 C2 C3 C4 -1.5(6) . .
C1 C2 C3 C4 174.6(5) . .
C2 C3 C4 C5 0.8(6) . .
C3 C4 C5 O3 0.2(5) . .
C3 C4 C5 C6 179.9(5) . .
C2 O3 C5 C4 -1.1(5) . .
C2 O3 C5 C6 179.2(4) . .
Pr1 O5 C6 O4 -49(5) 2_656 .
Pr1 O5 C6 C5 130(4) 2_656 .
Pr1 O4 C6 O5 -101.9(5) 1_565 .
Pr1 O4 C6 C5 78.6(5) 1_565 .
C4 C5 C6 O5 -166.8(5) . .
O3 C5 C6 O5 12.9(6) . .
C4 C5 C6 O4 12.7(8) . .
O3 C5 C6 O4 -167.6(4) . .
Pr1 O6 C7 O7 -173.0(3) . .
Pr1 O6 C7 C7 7.2(6) . 3_666
Pr1 O7 C7 O6 -173.0(3) 3_666 .
Pr1 O7 C7 C7 6.8(6) 3_666 3_666
