#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/08/2230863.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2230863
loop_
_publ_author_name
'Han, Li-Jun'
'Deng, Yuan-Fu'
'Ng, Seik Weng'
_publ_section_title
;
 Poly[[diaqua-μ₃-citrato-praseodymium(III)] monohydrate]
;
_journal_coeditor_code           SI2362
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m981
_journal_paper_doi               10.1107/S1600536811023804
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Pr (C6 H5 O7) (H2 O)2], H2 O'
_chemical_formula_moiety         'Pr (H2 O)2 (C6 H5 O7), H2 O'
_chemical_formula_sum            'C6 H11 O10 Pr'
_chemical_formula_weight         384.06
_chemical_name_systematic
;
Poly[[diaqua-μ₃-citrato-praseodymium(III)] monohydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.0672(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.2645(3)
_cell_length_b                   9.7356(7)
_cell_length_c                   17.0425(10)
_cell_measurement_reflns_used    8369
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.18
_cell_volume                     1039.22(11)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9596
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.735
_exptl_absorpt_correction_T_max  0.6489
_exptl_absorpt_correction_T_min  0.3308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    2.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.809
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2366
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+1.4664P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                2182
_reflns_number_total             2366
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            si2362.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2230863
_cod_database_fobs_code          2230863
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr Pr1 0.11415(2) 0.319324(16) 0.566983(9) 0.01012(6) Uani d . 1 1 . .
O O1 0.2224(4) 0.2466(3) 0.70094(14) 0.0212(5) Uani d . 1 1 . .
O O2 0.3108(4) 0.2315(3) 0.82649(14) 0.0245(5) Uani d . 1 1 . .
O O3 0.5035(3) 0.2913(2) 0.56851(14) 0.0195(5) Uani d . 1 1 . .
O O4 0.7923(3) 0.2852(2) 0.64591(13) 0.0150(4) Uani d . 1 1 . .
O O5 0.8717(3) 0.5316(2) 0.55742(13) 0.0166(4) Uani d . 1 1 . .
O O6 0.7309(4) 0.7354(2) 0.57242(13) 0.0185(5) Uani d . 1 1 . .
O O7 0.3381(3) 0.5013(2) 0.63152(13) 0.0138(4) Uani d D 1 1 . .
H H7 0.297(6) 0.574(2) 0.652(2) 0.021 Uiso d D 1 1 . .
O O1W -0.1683(3) 0.2119(3) 0.47949(14) 0.0192(5) Uani d D 1 1 . .
H H11 -0.172(5) 0.219(4) 0.4305(6) 0.029 Uiso d D 1 1 . .
H H12 -0.289(3) 0.230(4) 0.4971(18) 0.029 Uiso d D 1 1 . .
O O2W 0.1834(4) 0.0691(3) 0.56804(16) 0.0277(6) Uani d D 1 1 . .
H H21 0.147(6) -0.001(3) 0.543(2) 0.042 Uiso d D 1 1 . .
H H22 0.300(4) 0.054(4) 0.591(2) 0.042 Uiso d D 1 1 . .
O O3W 0.5632(6) -0.0132(4) 0.6318(2) 0.0564(10) Uani d D 1 1 . .
H H31 0.617(8) -0.092(2) 0.626(4) 0.085 Uiso d D 1 1 . .
H H32 0.635(8) 0.042(4) 0.605(3) 0.085 Uiso d D 1 1 . .
C C1 0.3229(5) 0.2872(3) 0.76032(18) 0.0146(6) Uani d . 1 1 . .
C C2 0.4742(5) 0.4089(3) 0.75574(17) 0.0141(6) Uani d . 1 1 . .
H H2A 0.6066 0.3849 0.7829 0.017 Uiso calc R 1 1 . .
H H2B 0.4118 0.4855 0.7836 0.017 Uiso calc R 1 1 . .
C C3 0.6141(5) 0.3355(3) 0.62538(18) 0.0125(6) Uani d . 1 1 . .
C C4 0.5269(4) 0.4564(3) 0.67268(17) 0.0109(6) Uani d . 1 1 . .
C C5 0.6919(5) 0.5734(3) 0.67823(17) 0.0130(6) Uani d . 1 1 . .
H H5A 0.6285 0.6513 0.7046 0.016 Uiso calc R 1 1 . .
H H5B 0.8134 0.5429 0.7097 0.016 Uiso calc R 1 1 . .
C C6 0.7682(4) 0.6185(3) 0.59874(17) 0.0120(6) Uani d . 1 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Pr1 O4 . 1_455 143.27(8) ?
O3 Pr1 O1 . . 72.72(8) ?
O4 Pr1 O1 1_455 . 70.79(7) ?
O3 Pr1 O2W . . 73.53(8) ?
O4 Pr1 O2W 1_455 . 90.48(8) ?
O1 Pr1 O2W . . 70.50(9) ?
O3 Pr1 O7 . . 61.63(7) ?
O4 Pr1 O7 1_455 . 108.24(7) ?
O1 Pr1 O7 . . 69.83(7) ?
O2W Pr1 O7 . . 126.67(8) ?
O3 Pr1 O1W . . 130.32(7) ?
O4 Pr1 O1W 1_455 . 72.22(7) ?
O1 Pr1 O1W . . 127.21(8) ?
O2W Pr1 O1W . . 73.54(8) ?
O7 Pr1 O1W . . 159.37(8) ?
O3 Pr1 O5 . 1_455 132.58(7) ?
O4 Pr1 O5 1_455 1_455 69.79(7) ?
O1 Pr1 O5 . 1_455 116.15(8) ?
O2W Pr1 O5 . 1_455 153.65(8) ?
O7 Pr1 O5 . 1_455 77.53(7) ?
O1W Pr1 O5 . 1_455 83.60(7) ?
O3 Pr1 O5 . 3_666 91.25(8) ?
O4 Pr1 O5 1_455 3_666 124.51(7) ?
O1 Pr1 O5 . 3_666 155.43(7) ?
O2W Pr1 O5 . 3_666 123.56(8) ?
O7 Pr1 O5 . 3_666 86.28(7) ?
O1W Pr1 O5 . 3_666 77.36(8) ?
O5 Pr1 O5 1_455 3_666 61.52(8) ?
O3 Pr1 O6 . 3_666 66.72(7) ?
O4 Pr1 O6 1_455 3_666 141.46(7) ?
O1 Pr1 O6 . 3_666 132.42(8) ?
O2W Pr1 O6 . 3_666 74.95(8) ?
O7 Pr1 O6 . 3_666 109.04(7) ?
O1W Pr1 O6 . 3_666 69.47(7) ?
O5 Pr1 O6 1_455 3_666 109.42(7) ?
O5 Pr1 O6 3_666 3_666 49.65(7) ?
C1 O1 Pr1 . . 141.7(2) ?
C3 O3 Pr1 . . 120.28(19) ?
C3 O4 Pr1 . 1_655 121.60(19) ?
C6 O5 Pr1 . 1_655 143.1(2) ?
C6 O5 Pr1 . 3_666 96.06(18) ?
Pr1 O5 Pr1 1_655 3_666 118.48(8) ?
C6 O6 Pr1 . 3_666 94.03(18) ?
C4 O7 Pr1 . . 116.75(17) ?
C4 O7 H7 . . 108(3) ?
Pr1 O7 H7 . . 128(3) ?
Pr1 O1W H11 . . 124(3) ?
Pr1 O1W H12 . . 109(3) ?
H11 O1W H12 . . 109(2) ?
Pr1 O2W H21 . . 139(3) ?
Pr1 O2W H22 . . 109(3) ?
H21 O2W H22 . . 110(2) ?
H31 O3W H32 . . 107(2) ?
O1 C1 O2 . . 123.7(3) ?
O1 C1 C2 . . 120.8(3) ?
O2 C1 C2 . . 115.5(3) ?
C1 C2 C4 . . 115.4(2) ?
C1 C2 H2A . . 108.4 ?
C4 C2 H2A . . 108.4 ?
C1 C2 H2B . . 108.4 ?
C4 C2 H2B . . 108.4 ?
H2A C2 H2B . . 107.5 ?
O3 C3 O4 . . 123.6(3) ?
O3 C3 C4 . . 118.1(3) ?
O4 C3 C4 . . 118.3(3) ?
O7 C4 C2 . . 110.8(2) ?
O7 C4 C3 . . 106.0(2) ?
C2 C4 C3 . . 109.8(2) ?
O7 C4 C5 . . 110.6(2) ?
C2 C4 C5 . . 108.8(2) ?
C3 C4 C5 . . 110.8(2) ?
C6 C5 C4 . . 112.5(2) ?
C6 C5 H5A . . 109.1 ?
C4 C5 H5A . . 109.1 ?
C6 C5 H5B . . 109.1 ?
C4 C5 H5B . . 109.1 ?
H5A C5 H5B . . 107.8 ?
O6 C6 O5 . . 119.9(3) ?
O6 C6 C5 . . 122.0(3) ?
O5 C6 C5 . . 118.1(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pr1 O1 . 2.473(2) ?
Pr1 O3 . 2.454(2) ?
Pr1 O4 1_455 2.467(2) ?
Pr1 O5 1_455 2.568(2) ?
Pr1 O5 3_666 2.572(2) ?
Pr1 O6 3_666 2.637(2) ?
Pr1 O7 . 2.502(2) ?
Pr1 O1W . 2.520(2) ?
Pr1 O2W . 2.474(3) ?
O1 C1 . 1.246(4) ?
O2 C1 . 1.255(4) ?
O3 C3 . 1.257(4) ?
O4 C3 . 1.262(4) ?
O4 Pr1 1_655 2.467(2) ?
O5 C6 . 1.284(4) ?
O5 Pr1 1_655 2.568(2) ?
O5 Pr1 3_666 2.572(2) ?
O6 C6 . 1.244(4) ?
O6 Pr1 3_666 2.637(2) ?
O7 C4 . 1.432(3) ?
O7 H7 . 0.834(10) ?
O1W H11 . 0.840(10) ?
O1W H12 . 0.840(10) ?
O2W H21 . 0.840(10) ?
O2W H22 . 0.840(10) ?
O3W H31 . 0.840(10) ?
O3W H32 . 0.850(10) ?
C1 C2 . 1.520(4) ?
C2 C4 . 1.531(4) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C4 . 1.533(4) ?
C4 C5 . 1.540(4) ?
C5 C6 . 1.510(4) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O7 H7 O2 2_556 0.830(10) 1.720(10) 2.536(3) 167(4) yes
O1w H11 O2 4_565 0.840(10) 1.840(10) 2.666(3) 169(4) yes
O1w H12 O3 1_455 0.840(10) 1.89(2) 2.692(3) 159(3) yes
O2w H21 O1w 3_556 0.840(10) 2.09(2) 2.854(4) 151(4) yes
O2w H22 O3w . 0.840(10) 1.890(10) 2.718(4) 168(4) yes
O3w H31 O6 1_545 0.840(10) 2.05(2) 2.856(4) 160(6) yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O3 Pr1 O1 C1 . . . . 67.4(4) ?
O4 Pr1 O1 C1 1_455 . . . -116.8(4) ?
O2W Pr1 O1 C1 . . . . 145.6(4) ?
O7 Pr1 O1 C1 . . . . 2.0(3) ?
O1W Pr1 O1 C1 . . . . -164.6(3) ?
O5 Pr1 O1 C1 1_455 . . . -62.1(4) ?
O5 Pr1 O1 C1 3_666 . . . 16.1(5) ?
O6 Pr1 O1 C1 3_666 . . . 99.8(4) ?
O4 Pr1 O3 C3 1_455 . . . -49.7(3) ?
O1 Pr1 O3 C3 . . . . -43.1(2) ?
O2W Pr1 O3 C3 . . . . -117.3(2) ?
O7 Pr1 O3 C3 . . . . 32.9(2) ?
O1W Pr1 O3 C3 . . . . -167.6(2) ?
O5 Pr1 O3 C3 1_455 . . . 66.8(3) ?
O5 Pr1 O3 C3 3_666 . . . 118.0(2) ?
O6 Pr1 O3 C3 3_666 . . . 162.4(3) ?
O3 Pr1 O7 C4 . . . . -35.86(18) ?
O4 Pr1 O7 C4 1_455 . . . 105.51(18) ?
O1 Pr1 O7 C4 . . . . 44.86(18) ?
O2W Pr1 O7 C4 . . . . 0.7(2) ?
O1W Pr1 O7 C4 . . . . -166.6(2) ?
O5 Pr1 O7 C4 1_455 . . . 169.07(19) ?
O5 Pr1 O7 C4 3_666 . . . -129.30(19) ?
O6 Pr1 O7 C4 3_666 . . . -84.44(19) ?
Pr1 O1 C1 O2 . . . . 164.9(2) ?
Pr1 O1 C1 C2 . . . . -16.3(5) ?
O1 C1 C2 C4 . . . . -11.9(4) ?
O2 C1 C2 C4 . . . . 167.0(3) ?
Pr1 O3 C3 O4 . . . . 152.9(2) ?
Pr1 O3 C3 C4 . . . . -26.6(4) ?
Pr1 O4 C3 O3 1_655 . . . 72.0(4) ?
Pr1 O4 C3 C4 1_655 . . . -108.5(3) ?
Pr1 O7 C4 C2 . . . . -83.4(2) ?
Pr1 O7 C4 C3 . . . . 35.7(3) ?
Pr1 O7 C4 C5 . . . . 155.86(18) ?
C1 C2 C4 O7 . . . . 61.8(3) ?
C1 C2 C4 C3 . . . . -55.0(3) ?
C1 C2 C4 C5 . . . . -176.4(3) ?
O3 C3 C4 O7 . . . . -6.7(4) ?
O4 C3 C4 O7 . . . . 173.7(2) ?
O3 C3 C4 C2 . . . . 113.0(3) ?
O4 C3 C4 C2 . . . . -66.5(3) ?
O3 C3 C4 C5 . . . . -126.7(3) ?
O4 C3 C4 C5 . . . . 53.7(4) ?
O7 C4 C5 C6 . . . . -63.2(3) ?
C2 C4 C5 C6 . . . . 175.0(2) ?
C3 C4 C5 C6 . . . . 54.1(3) ?
Pr1 O6 C6 O5 3_666 . . . 6.0(3) ?
Pr1 O6 C6 C5 3_666 . . . -173.0(2) ?
Pr1 O5 C6 O6 1_655 . . . 153.9(2) ?
Pr1 O5 C6 O6 3_666 . . . -6.2(3) ?
Pr1 O5 C6 C5 1_655 . . . -27.1(4) ?
Pr1 O5 C6 C5 3_666 . . . 172.8(2) ?
Pr1 O5 C6 Pr1 1_655 . . 3_666 160.0(3) ?
C4 C5 C6 O6 . . . . 114.9(3) ?
C4 C5 C6 O5 . . . . -64.0(3) ?
