#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:10:02 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179616 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/80/4508081.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_4508081
loop_
_publ_author_name
'Senthil Raja, Duraisamy'
'Luo, Jheng-Hong'
'Wu, Cheng-You'
'Cheng, Yu-Jung'
'Yeh, Chun-Ting'
'Chen, Ya-Ting'
'Lo, Sheng-Han'
'Lai, Yu-Lun'
'Lin, Chia-Her'
_publ_section_title
;
 Solvothermal Synthesis, Structural Diversity, and Properties of Alkali
 Metal--Organic Frameworks Based on V-shaped Ligand
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3785
_journal_paper_doi               10.1021/cg400801s
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C14 H8 O6 Rb S'
_chemical_formula_weight         389.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 109.222(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1526(4)
_cell_length_b                   4.8183(2)
_cell_length_c                   12.3055(4)
_cell_measurement_reflns_used    2584
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2834
_cell_measurement_theta_min      3.3689
_cell_volume                     680.38(4)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6399
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    3.819
_exptl_absorpt_correction_T_max  0.8940
_exptl_absorpt_correction_T_min  0.3937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lamellar
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0626P)²+0.6080P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                1279
_reflns_number_total             1693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400801s_si_002.cif
_cod_data_source_block           3
_cod_database_code               4508081
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -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
Rb1 Rb 0.5000 0.18937(12) 0.2500 0.0452(2) Uani 1 2 d S
S1 S 0.0000 1.1074(3) 0.2500 0.0272(3) Uani 1 2 d S
O1 O 0.4346(2) 0.1919(6) 0.4519(2) 0.0313(6) Uani 1 1 d .
O2 O 0.3988(3) 0.2786(6) 0.6149(2) 0.0390(7) Uani 1 1 d .
O3 O -0.0394(2) 1.2551(6) 0.3313(3) 0.0392(7) Uani 1 1 d .
C1 C 0.3804(3) 0.3184(8) 0.5115(3) 0.0259(8) Uani 1 1 d .
C2 C 0.2885(3) 0.5221(7) 0.4466(3) 0.0237(7) Uani 1 1 d .
C3 C 0.2048(3) 0.6081(9) 0.4936(3) 0.0301(8) Uani 1 1 d .
H3A H 0.2079 0.5445 0.5659 0.036 Uiso 1 1 calc R
C4 C 0.1175(3) 0.7858(8) 0.4345(4) 0.0323(9) Uani 1 1 d .
H4A H 0.0609 0.8400 0.4658 0.039 Uiso 1 1 calc R
C5 C 0.1141(3) 0.8838(7) 0.3281(3) 0.0243(7) Uani 1 1 d .
C6 C 0.1978(4) 0.8061(8) 0.2800(3) 0.0310(8) Uani 1 1 d .
H6A H 0.1961 0.8752 0.2089 0.037 Uiso 1 1 calc R
C7 C 0.2840(3) 0.6234(8) 0.3403(3) 0.0290(8) Uani 1 1 d .
H7A H 0.3402 0.5676 0.3086 0.035 Uiso 1 1 calc R
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'
S S 0.1246 0.1234 '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
O2 Rb1 O2 74.42(13) 4 3_656
O2 Rb1 O1 71.52(8) 4 2_655
O2 Rb1 O1 108.88(8) 3_656 2_655
O2 Rb1 O1 108.88(8) 4 .
O2 Rb1 O1 71.52(8) 3_656 .
O1 Rb1 O1 179.52(11) 2_655 .
O2 Rb1 O2 176.52(7) 4 3_666
O2 Rb1 O2 109.06(9) 3_656 3_666
O1 Rb1 O2 106.90(8) 2_655 3_666
O1 Rb1 O2 72.68(8) . 3_666
O2 Rb1 O2 109.06(9) 4 4_565
O2 Rb1 O2 176.52(7) 3_656 4_565
O1 Rb1 O2 72.68(8) 2_655 4_565
O1 Rb1 O2 106.90(8) . 4_565
O2 Rb1 O2 67.47(10) 3_666 4_565
O2 Rb1 C1 164.33(8) 4 3_666
O2 Rb1 C1 93.66(9) 3_656 3_666
O1 Rb1 C1 122.88(8) 2_655 3_666
O1 Rb1 C1 56.75(8) . 3_666
O2 Rb1 C1 18.42(8) 3_666 3_666
O2 Rb1 C1 82.93(8) 4_565 3_666
O2 Rb1 C1 93.66(9) 4 4_565
O2 Rb1 C1 164.33(8) 3_656 4_565
O1 Rb1 C1 56.75(8) 2_655 4_565
O1 Rb1 C1 122.88(8) . 4_565
O2 Rb1 C1 82.93(8) 3_666 4_565
O2 Rb1 C1 18.42(8) 4_565 4_565
C1 Rb1 C1 99.74(11) 3_666 4_565
O2 Rb1 C1 14.93(8) 4 4
O2 Rb1 C1 85.48(8) 3_656 4
O1 Rb1 C1 57.60(8) 2_655 4
O1 Rb1 C1 122.77(8) . 4
O2 Rb1 C1 162.38(8) 3_666 4
O2 Rb1 C1 97.94(8) 4_565 4
C1 Rb1 C1 179.12(9) 3_666 4
C1 Rb1 C1 81.13(7) 4_565 4
O2 Rb1 C1 85.48(8) 4 3_656
O2 Rb1 C1 14.93(8) 3_656 3_656
O1 Rb1 C1 122.77(8) 2_655 3_656
O1 Rb1 C1 57.60(8) . 3_656
O2 Rb1 C1 97.94(8) 3_666 3_656
O2 Rb1 C1 162.38(8) 4_565 3_656
C1 Rb1 C1 81.13(7) 3_666 3_656
C1 Rb1 C1 179.12(9) 4_565 3_656
C1 Rb1 C1 97.99(11) 4 3_656
O2 Rb1 Rb1 142.79(6) 4 1_565
O2 Rb1 Rb1 142.79(6) 3_656 1_565
O1 Rb1 Rb1 89.76(6) 2_655 1_565
O1 Rb1 Rb1 89.76(6) . 1_565
O2 Rb1 Rb1 33.73(5) 3_666 1_565
O2 Rb1 Rb1 33.73(5) 4_565 1_565
C1 Rb1 Rb1 49.87(6) 3_666 1_565
C1 Rb1 Rb1 49.87(6) 4_565 1_565
C1 Rb1 Rb1 131.00(6) 4 1_565
C1 Rb1 Rb1 131.00(6) 3_656 1_565
O2 Rb1 Rb1 37.21(6) 4 1_545
O2 Rb1 Rb1 37.21(6) 3_656 1_545
O1 Rb1 Rb1 90.24(6) 2_655 1_545
O1 Rb1 Rb1 90.24(6) . 1_545
O2 Rb1 Rb1 146.27(5) 3_666 1_545
O2 Rb1 Rb1 146.27(5) 4_565 1_545
C1 Rb1 Rb1 130.13(6) 3_666 1_545
C1 Rb1 Rb1 130.13(6) 4_565 1_545
C1 Rb1 Rb1 49.00(6) 4 1_545
C1 Rb1 Rb1 49.00(6) 3_656 1_545
Rb1 Rb1 Rb1 180.0 1_565 1_545
O3 S1 O3 120.4(3) . 2
O3 S1 C5 107.39(17) . 2
O3 S1 C5 107.81(17) 2 2
O3 S1 C5 107.81(17) . .
O3 S1 C5 107.39(17) 2 .
C5 S1 C5 105.0(2) 2 .
C1 O1 Rb1 147.2(2) . .
C1 O2 Rb1 128.8(3) . 3_656
C1 O2 Rb1 109.4(3) . 3_666
Rb1 O2 Rb1 109.06(9) 3_656 3_666
O2 C1 O1 124.1(3) . .
O2 C1 C2 120.0(3) . .
O1 C1 C2 115.9(3) . .
O2 C1 Rb1 52.2(2) . 3_666
O1 C1 Rb1 128.1(2) . 3_666
C2 C1 Rb1 91.8(2) . 3_666
O2 C1 Rb1 36.29(19) . 3_656
O1 C1 Rb1 89.9(2) . 3_656
C2 C1 Rb1 151.0(2) . 3_656
Rb1 C1 Rb1 81.13(7) 3_666 3_656
C7 C2 C3 118.9(3) . .
C7 C2 C1 121.6(3) . .
C3 C2 C1 119.5(3) . .
C4 C3 C2 120.7(4) . .
C4 C3 H3A 119.7 . .
C2 C3 H3A 119.7 . .
C3 C4 C5 119.6(4) . .
C3 C4 H4A 120.2 . .
C5 C4 H4A 120.2 . .
C4 C5 C6 121.1(3) . .
C4 C5 S1 119.8(3) . .
C6 C5 S1 119.1(3) . .
C7 C6 C5 118.4(4) . .
C7 C6 H6A 120.8 . .
C5 C6 H6A 120.8 . .
C2 C7 C6 121.3(4) . .
C2 C7 H7A 119.3 . .
C6 C7 H7A 119.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rb1 O2 2.831(3) 4
Rb1 O2 2.831(3) 3_656
Rb1 O1 2.847(3) 2_655
Rb1 O1 2.847(3) .
Rb1 O2 3.083(3) 3_666
Rb1 O2 3.083(3) 4_565
Rb1 C1 3.680(4) 3_666
Rb1 C1 3.680(4) 4_565
Rb1 C1 3.729(4) 4
Rb1 C1 3.729(4) 3_656
Rb1 Rb1 4.8183(2) 1_565
Rb1 Rb1 4.8183(2) 1_545
S1 O3 1.433(3) .
S1 O3 1.433(3) 2
S1 C5 1.769(4) 2
S1 C5 1.769(4) .
O1 C1 1.288(5) .
O2 C1 1.232(5) .
O2 Rb1 2.831(3) 3_656
O2 Rb1 3.083(3) 3_666
C1 C2 1.504(5) .
C1 Rb1 3.680(4) 3_666
C1 Rb1 3.729(4) 3_656
C2 C7 1.381(5) .
C2 C3 1.389(5) .
C3 C4 1.371(6) .
C3 H3A 0.9300 .
C4 C5 1.379(6) .
C4 H4A 0.9300 .
C5 C6 1.386(6) .
C6 C7 1.382(5) .
C6 H6A 0.9300 .
C7 H7A 0.9300 .
