#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:15:17 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180471 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/40/7214024.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_7214024
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Metal--organic frameworks built from alkali metal ions (Li+--Cs+) and
 1,2,3,4-cyclobutanetetracarboxylic acid
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1724
_journal_paper_doi               10.1039/c3ce41565a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C8 H7 O8 Rb'
_chemical_formula_weight         316.61
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1309(4)
_cell_length_b                   9.6620(5)
_cell_length_c                   12.7399(5)
_cell_measurement_reflns_used    56474
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      3.20
_cell_volume                     1000.86(8)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and thirteen ω scans with 2° steps (741 frames)'
_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  0.0105
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56474
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         3.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.978
_exptl_absorpt_correction_T_max  0.408
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0232
_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)+(0.0430P)²+0.1721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                1331
_reflns_number_total             1527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41565a.txt
_cod_data_source_block           6
_cod_database_code               7214024
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, 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
Rb Rb 0.7500 0.7500 0.445681(16) 0.02820(9) Uani 1 2 d S
O1 O 1.06921(12) 0.60330(10) 0.46183(7) 0.0241(2) Uani 1 1 d .
H1 H 1.0517 0.5335 0.4961 0.029 Uiso 0.50 1 d PR
O2 O 1.20957(13) 0.44061(10) 0.37659(8) 0.0251(2) Uani 1 1 d .
O3 O 0.96937(12) 0.64409(10) 0.21947(8) 0.0273(2) Uani 1 1 d .
H3 H 0.8810 0.6068 0.1888 0.033 Uiso 1 1 d R
O4 O 1.11130(13) 0.50637(11) 0.11118(8) 0.0337(2) Uani 1 1 d .
C1 C 1.18006(15) 0.56451(13) 0.39633(9) 0.0205(2) Uani 1 1 d .
C2 C 1.27662(15) 0.67380(13) 0.33856(11) 0.0194(2) Uani 1 1 d .
H2 H 1.3930 0.6672 0.3579 0.023 Uiso 1 1 calc R
C3 C 1.25943(14) 0.66948(16) 0.21590(11) 0.0205(3) Uani 1 1 d .
H3A H 1.3599 0.6381 0.1807 0.025 Uiso 1 1 calc R
C4 C 1.10703(17) 0.59756(14) 0.17626(10) 0.0228(2) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rb 0.02922(13) 0.02228(12) 0.03309(13) 0.000 0.000 0.00330(6)
O1 0.0259(5) 0.0218(5) 0.0245(4) 0.0031(3) 0.0055(3) 0.0022(4)
O2 0.0277(5) 0.0198(4) 0.0277(5) 0.0002(4) 0.0061(4) -0.0005(4)
O3 0.0245(5) 0.0269(5) 0.0306(5) -0.0062(4) -0.0036(4) -0.0032(4)
O4 0.0346(6) 0.0330(6) 0.0337(5) -0.0128(4) 0.0025(4) -0.0077(4)
C1 0.0207(6) 0.0214(6) 0.0192(5) 0.0015(4) -0.0007(4) -0.0005(4)
C2 0.0197(5) 0.0185(6) 0.0199(6) 0.0002(5) -0.0006(4) -0.0006(4)
C3 0.0219(6) 0.0194(6) 0.0201(5) -0.0006(5) 0.0020(4) -0.0021(4)
C4 0.0267(6) 0.0214(6) 0.0203(5) 0.0013(5) -0.0012(5) -0.0038(5)
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O4 Rb O4 150.19(4) 4_465 3_755
O4 Rb O2 72.04(3) 4_465 5_766
O4 Rb O2 134.83(3) 3_755 5_766
O4 Rb O2 134.83(3) 4_465 6_566
O4 Rb O2 72.04(3) 3_755 6_566
O2 Rb O2 79.13(4) 5_766 6_566
O4 Rb O1 87.01(3) 4_465 .
O4 Rb O1 95.04(3) 3_755 .
O2 Rb O1 63.17(3) 5_766 .
O2 Rb O1 110.14(3) 6_566 .
O4 Rb O1 95.04(3) 4_465 2_665
O4 Rb O1 87.01(3) 3_755 2_665
O2 Rb O1 110.14(3) 5_766 2_665
O2 Rb O1 63.17(3) 6_566 2_665
O1 Rb O1 172.04(4) . 2_665
O4 Rb O3 80.97(3) 4_465 2_665
O4 Rb O3 74.82(3) 3_755 2_665
O2 Rb O3 149.90(3) 5_766 2_665
O2 Rb O3 112.95(3) 6_566 2_665
O1 Rb O3 129.48(3) . 2_665
O1 Rb O3 58.48(2) 2_665 2_665
O4 Rb O3 74.82(3) 4_465 .
O4 Rb O3 80.97(3) 3_755 .
O2 Rb O3 112.95(3) 5_766 .
O2 Rb O3 149.90(3) 6_566 .
O1 Rb O3 58.48(2) . .
O1 Rb O3 129.48(3) 2_665 .
O3 Rb O3 71.02(3) 2_665 .
C1 O1 Rb 135.15(8) . .
C1 O1 H1 103.3 . .
Rb O1 H1 106.2 . .
C1 O2 Rb 117.92(8) . 5_766
C4 O3 Rb 149.46(8) . .
C4 O3 H3 111.1 . .
Rb O3 H3 93.9 . .
C4 O4 Rb 145.89(10) . 3_745
O2 C1 O1 123.12(12) . .
O2 C1 C2 118.29(11) . .
O1 C1 C2 118.58(11) . .
C1 C2 C2 121.67(11) . 2_765
C1 C2 C3 114.90(11) . .
C2 C2 C3 90.02(7) 2_765 .
C1 C2 H2 109.6 . .
C2 C2 H2 109.6 2_765 .
C3 C2 H2 109.6 . .
C4 C3 C3 112.21(12) . 2_765
C4 C3 C2 114.77(10) . .
C3 C3 C2 88.98(7) 2_765 .
C4 C3 H3A 112.9 . .
C3 C3 H3A 112.9 2_765 .
C2 C3 H3A 112.9 . .
O4 C4 O3 123.74(12) . .
O4 C4 C3 122.77(13) . .
O3 C4 C3 113.48(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rb O4 2.8164(11) 4_465
Rb O4 2.8164(11) 3_755
Rb O2 2.9371(10) 5_766
Rb O2 2.9371(10) 6_566
Rb O1 2.9645(10) .
Rb O1 2.9645(10) 2_665
Rb O3 3.5403(10) 2_665
Rb O3 3.5403(10) .
O1 C1 1.2842(15) .
O1 H1 0.8159 .
O2 C1 1.2466(16) .
O2 Rb 2.9371(10) 5_766
O3 C4 1.3259(17) .
O3 H3 0.8939 .
O4 C4 1.2103(16) .
O4 Rb 2.8164(11) 3_745
C1 C2 1.5076(17) .
C2 C2 1.535(3) 2_765
C2 C3 1.5695(18) .
C2 H2 0.9800 .
C3 C4 1.5078(18) .
C3 C3 1.564(3) 2_765
C3 H3A 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O1 0.82 1.73 2.4894(19) 153.6 5_766
O3 H3 O2 0.89 1.69 2.5748(14) 171.6 4_465
