#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/03/2210338.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_2210338
loop_
_publ_author_name
'Stein, Irena'
'Ruschewitz, Uwe'
_publ_section_title
;
 Poly[di-μ₃-aqua-μ₄-terephthalato-dirubidium]
;
_journal_coeditor_code           NG2059
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2116
_journal_page_last               m2118
_journal_paper_doi               10.1107/S160053680602928X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Rb2 (C8 H4 O4) (H2 O)2]'
_chemical_formula_moiety         'C8 H8 O6 Rb2'
_chemical_formula_sum            'C8 H8 O6 Rb2'
_chemical_formula_weight         371.08
_chemical_name_common            'Dirubidium terephthalate dihydrate'
_chemical_name_systematic
;
Poly[di-μ₃-aqua-μ₄-terephthalato-dirubidium]
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.663(3)
_cell_length_b                   3.9531(5)
_cell_length_c                   11.873(3)
_cell_measurement_reflns_used    1243
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.95
_cell_volume                     551.6(2)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Stoe IPDS IP'
_diffrn_measurement_method       φ
_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  0.0911
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5609
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         3.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.881
_exptl_absorpt_correction_T_max  0.3325
_exptl_absorpt_correction_T_min  0.2475
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED32 (Stoe & Cie, 2001); crystal shape optimized by X-SHAPE (Stoe &
Cie,
1999)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.872
_refine_diff_density_min         -1.482
_refine_ls_extinction_coef       0.015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1243
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0420
_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)+(0.0625P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                874
_reflns_number_total             1243
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2059.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2210338
_cod_database_fobs_code          2210338
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_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
Rb Rb1 0.65483(4) 0.79622(13) 0.18263(4) 0.0335(2) Uani d . 1
O O2 0.7052(3) 0.3109(10) 0.3821(3) 0.0335(8) Uani d . 1
O O1 0.7521(3) 0.2016(11) 0.5772(3) 0.0369(9) Uani d . 1
O O3 0.4564(3) 0.2658(11) 0.1041(4) 0.0393(9) Uani d D 1
C C1 0.7751(4) 0.2159(12) 0.4845(4) 0.0229(9) Uani d . 1
C C2 0.8917(4) 0.1065(12) 0.4916(4) 0.0203(9) Uani d . 1
C C3 0.9264(4) 0.1514(13) 0.3939(4) 0.0255(10) Uani d . 1
H H3 0.8775 0.2528 0.3230 0.029(14) Uiso calc R 1
C C4 0.9664(4) -0.0449(14) 0.5975(4) 0.0253(10) Uani d . 1
H H4 0.9442 -0.0748 0.6632 0.036(16) Uiso calc R 1
H H1 0.402(4) 0.095(12) 0.095(5) 0.039(16) Uiso d D 1
H H2 0.409(5) 0.459(12) 0.085(6) 0.06(2) Uiso d D 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'
Rb Rb -0.9393 2.9676 '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
O1 Rb1 O1 4_565 4_575 87.71(9)
O1 Rb1 O2 4_565 . 84.44(11)
O1 Rb1 O2 4_575 . 144.07(11)
O1 Rb1 O3 4_565 1_565 138.19(12)
O1 Rb1 O3 4_575 1_565 83.16(11)
O2 Rb1 O3 . 1_565 124.43(11)
O1 Rb1 O2 4_565 1_565 144.59(10)
O1 Rb1 O2 4_575 1_565 82.84(11)
O2 Rb1 O2 . 1_565 83.56(9)
O3 Rb1 O2 1_565 1_565 74.42(11)
O1 Rb1 O3 4_565 . 80.62(10)
O1 Rb1 O3 4_575 . 139.66(11)
O2 Rb1 O3 . . 73.22(11)
O3 Rb1 O3 1_565 . 80.49(9)
O2 Rb1 O3 1_565 . 126.75(10)
O1 Rb1 O3 4_565 3_665 64.31(11)
O1 Rb1 O3 4_575 3_665 71.05(11)
O2 Rb1 O3 . 3_665 133.89(11)
O3 Rb1 O3 1_565 3_665 74.15(13)
O2 Rb1 O3 1_565 3_665 141.01(10)
O3 Rb1 O3 . 3_665 69.08(13)
O1 Rb1 O3 4_565 2_655 133.23(11)
O1 Rb1 O3 4_575 2_655 137.05(11)
O2 Rb1 O3 . 2_655 52.20(10)
O3 Rb1 O3 1_565 2_655 73.37(11)
O2 Rb1 O3 1_565 2_655 56.66(10)
O3 Rb1 O3 . 2_655 71.49(11)
O3 Rb1 O3 3_665 2_655 132.01(12)
O1 Rb1 C3 4_565 1_565 96.64(11)
O1 Rb1 C3 4_575 1_565 65.79(11)
O2 Rb1 C3 . 1_565 80.36(11)
O3 Rb1 C3 1_565 1_565 116.00(12)
O2 Rb1 C3 1_565 1_565 48.48(10)
O3 Rb1 C3 . 1_565 153.57(11)
O3 Rb1 C3 3_665 1_565 133.38(10)
O3 Rb1 C3 2_655 1_565 92.74(10)
O1 Rb1 C1 4_565 1_565 130.00(11)
O1 Rb1 C1 4_575 1_565 91.36(10)
O2 Rb1 C1 . 1_565 68.00(11)
O3 Rb1 C1 1_565 1_565 91.05(11)
O2 Rb1 C1 1_565 1_565 17.94(10)
O3 Rb1 C1 . 1_565 125.41(10)
O3 Rb1 C1 3_665 1_565 157.95(11)
O3 Rb1 C1 2_655 1_565 54.59(10)
C3 Rb1 C1 1_565 1_565 39.96(10)
O1 Rb1 Rb1 4_565 1_565 133.73(7)
O1 Rb1 Rb1 4_575 1_565 46.02(8)
O2 Rb1 Rb1 . 1_565 130.95(8)
O3 Rb1 Rb1 1_565 1_565 51.47(8)
O2 Rb1 Rb1 1_565 1_565 47.38(7)
O3 Rb1 Rb1 . 1_565 131.97(8)
O3 Rb1 Rb1 3_665 1_565 94.43(8)
O3 Rb1 Rb1 2_655 1_565 92.07(8)
C3 Rb1 Rb1 1_565 1_565 67.68(8)
C1 Rb1 Rb1 1_565 1_565 63.53(7)
O1 Rb1 Rb1 4_565 1_545 46.27(7)
O1 Rb1 Rb1 4_575 1_545 133.98(8)
O2 Rb1 Rb1 . 1_545 49.05(7)
O3 Rb1 Rb1 1_565 1_545 128.53(8)
O2 Rb1 Rb1 1_565 1_545 132.62(7)
O3 Rb1 Rb1 . 1_545 48.03(8)
O3 Rb1 Rb1 3_665 1_545 85.57(8)
O3 Rb1 Rb1 2_655 1_545 87.93(8)
C3 Rb1 Rb1 1_565 1_545 112.32(8)
C1 Rb1 Rb1 1_565 1_545 116.47(7)
Rb1 Rb1 Rb1 1_565 1_545 180.0
O1 Rb1 H2 4_565 . 94.3(8)
O1 Rb1 H2 4_575 . 130.9(10)
O2 Rb1 H2 . . 84.7(9)
O3 Rb1 H2 1_565 . 63.3(5)
O2 Rb1 H2 1_565 . 117.5(10)
O3 Rb1 H2 . . 17.2(4)
O3 Rb1 H2 3_665 . 66.0(12)
O3 Rb1 H2 2_655 . 68.1(12)
C3 Rb1 H2 1_565 . 160.5(12)
C1 Rb1 H2 1_565 . 122.1(11)
Rb1 Rb1 H2 1_565 . 114.8(5)
Rb1 Rb1 H2 1_545 . 65.2(5)
C1 O2 Rb1 . . 146.7(3)
C1 O2 Rb1 . 1_545 115.1(3)
Rb1 O2 Rb1 . 1_545 83.56(9)
C1 O1 Rb1 . 4_566 134.8(3)
C1 O1 Rb1 . 4_576 129.7(3)
Rb1 O1 Rb1 4_566 4_576 87.71(9)
Rb1 O3 Rb1 1_545 . 80.49(9)
Rb1 O3 Rb1 1_545 3_665 105.85(13)
Rb1 O3 Rb1 . 3_665 110.92(12)
Rb1 O3 Rb1 1_545 2_645 109.34(13)
Rb1 O3 Rb1 . 2_645 105.62(12)
Rb1 O3 Rb1 3_665 2_645 132.45(12)
Rb1 O3 H1 1_545 . 95(4)
Rb1 O3 H1 . . 170(4)
Rb1 O3 H1 3_665 . 79(3)
Rb1 O3 H1 2_645 . 67(4)
Rb1 O3 H2 1_545 . 165(5)
Rb1 O3 H2 . . 84(5)
Rb1 O3 H2 3_665 . 79(4)
Rb1 O3 H2 2_645 . 75(4)
H1 O3 H2 . . 100(6)
O1 C1 O2 . . 123.7(4)
O1 C1 C2 . . 119.0(4)
O2 C1 C2 . . 117.2(4)
O1 C1 Rb1 . 1_545 133.4(3)
O2 C1 Rb1 . 1_545 47.0(2)
C2 C1 Rb1 . 1_545 88.1(2)
C3 C2 C4 . . 119.0(4)
C3 C2 C1 . . 121.4(4)
C4 C2 C1 . . 119.6(4)
C4 C3 C2 3_756 . 120.2(4)
C4 C3 Rb1 3_756 1_545 124.8(3)
C2 C3 Rb1 . 1_545 90.8(3)
C4 C3 H3 3_756 . 119.9
C2 C3 H3 . . 119.9
Rb1 C3 H3 1_545 . 54.0
C3 C4 C2 3_756 . 120.8(4)
C3 C4 H4 3_756 . 119.6
C2 C4 H4 . . 119.6
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
Rb1 O1 4_565 2.847(4) y
Rb1 O1 4_575 2.859(4) y
Rb1 O2 . 2.927(4) y
Rb1 O3 1_565 2.980(4) y
Rb1 O2 1_565 3.005(4) y
Rb1 O3 . 3.136(4) y
Rb1 O3 3_665 3.172(4) y
Rb1 O3 2_655 3.327(4) y
Rb1 Rb1 1_565 3.9531(5) ?
Rb1 Rb1 1_545 3.9531(5) ?
O2 C1 . 1.265(6) y
O1 C1 . 1.240(5) y
O3 H1 . 0.94(2) ?
O3 H2 . 0.94(2) ?
C1 C2 . 1.511(6) y
C2 C3 . 1.395(6) y
C2 C4 . 1.396(7) y
C3 C4 3_756 1.389(6) y
C3 H3 . 0.9300 ?
C4 H4 . 0.9300 ?
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
O3 H1 O2 2_645 0.94(2) 1.86(3) 2.775(5) 164(5)
O3 H2 O2 2_655 0.94(2) 2.15(4) 3.018(6) 153(6)
O3 H2 O1 2_655 0.94(2) 2.42(5) 3.215(6) 141(6)
