#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:15:17 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180471 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/40/7214025.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_7214025
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 Cs O8'
_chemical_formula_weight         364.05
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                   9.8276(3)
_cell_length_b                   9.8276(3)
_cell_length_c                   10.2207(5)
_cell_measurement_reflns_used    34426
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      3.55
_cell_volume                     987.13(6)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and eight ω scans with 2° steps (578 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  0.0190
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34426
_diffrn_reflns_theta_full        30.49
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         3.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.783
_exptl_absorpt_correction_T_max  0.612
_exptl_absorpt_correction_T_min  0.429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0231
_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)+(0.0344P)²+0.5252P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                1412
_reflns_number_total             1497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41565a.txt
_cod_data_source_block           7
_cod_original_cell_volume        987.13(8)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7214025
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
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
Cs1 Cs 0.2500 0.2500 0.79058(2) 0.02263(8) Uani 1 4 d S
Cs2 Cs 0.2500 0.2500 0.35535(2) 0.01825(8) Uani 1 4 d S
O1 O 0.13331(17) 0.06122(16) 0.56824(13) 0.0221(3) Uani 1 1 d .
O2 O 0.05248(16) -0.11429(15) 0.68343(16) 0.0237(3) Uani 1 1 d .
O3 O 0.42195(17) -0.05108(18) 0.83394(18) 0.0321(4) Uani 1 1 d .
O4A O 0.5612(3) -0.2158(3) 0.8868(3) 0.0209(8) Uani 0.500(5) 1 d P
O4B O 0.5727(3) -0.1591(4) 0.9713(4) 0.0285(9) Uani 0.500(5) 1 d P
C1 C 0.1195(2) -0.0605(2) 0.58349(18) 0.0189(3) Uani 1 1 d .
C2 C 0.18306(17) -0.16148(17) 0.4906(2) 0.0185(3) Uani 1 1 d .
H2 H 0.1636 -0.1357 0.3999 0.022 Uiso 1 1 calc R
C3 C 0.4502(3) -0.1391(3) 0.9150(3) 0.0467(8) Uani 1 1 d .
C4 C 0.34590(19) -0.19559(18) 1.0088(2) 0.0197(3) Uani 1 1 d .
H4 H 0.3747 -0.1793 1.0993 0.024 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'
Cs Cs -0.3680 2.1192 '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
O4B Cs1 O4B 52.64(8) 7_667 6_567
O4B Cs1 O4B 52.64(8) 7_667 5_657
O4B Cs1 O4B 77.66(13) 6_567 5_657
O4B Cs1 O4B 77.66(13) 7_667 8_557
O4B Cs1 O4B 52.64(8) 6_567 8_557
O4B Cs1 O4B 52.64(8) 5_657 8_557
O4B Cs1 O1 97.43(7) 7_667 2
O4B Cs1 O1 126.63(7) 6_567 2
O4B Cs1 O1 121.83(6) 5_657 2
O4B Cs1 O1 174.16(7) 8_557 2
O4B Cs1 O1 121.83(6) 7_667 4
O4B Cs1 O1 97.43(7) 6_567 4
O4B Cs1 O1 174.16(7) 5_657 4
O4B Cs1 O1 126.63(7) 8_557 4
O1 Cs1 O1 58.63(3) 2 4
O4B Cs1 O1 126.63(7) 7_667 3
O4B Cs1 O1 174.16(7) 6_567 3
O4B Cs1 O1 97.43(7) 5_657 3
O4B Cs1 O1 121.83(6) 8_557 3
O1 Cs1 O1 58.63(3) 2 3
O1 Cs1 O1 87.65(5) 4 3
O4B Cs1 O1 174.16(7) 7_667 .
O4B Cs1 O1 121.83(6) 6_567 .
O4B Cs1 O1 126.63(7) 5_657 .
O4B Cs1 O1 97.43(7) 8_557 .
O1 Cs1 O1 87.65(5) 2 .
O1 Cs1 O1 58.63(3) 4 .
O1 Cs1 O1 58.63(3) 3 .
O4B Cs1 O3 51.60(8) 7_667 3
O4B Cs1 O3 103.84(7) 6_567 3
O4B Cs1 O3 63.88(7) 5_657 3
O4B Cs1 O3 114.85(8) 8_557 3
O1 Cs1 O3 59.33(4) 2 3
O1 Cs1 O3 114.91(4) 4 3
O1 Cs1 O3 76.40(4) 3 3
O1 Cs1 O3 134.13(4) . 3
O4B Cs1 O3 63.88(7) 7_667 2
O4B Cs1 O3 51.60(8) 6_567 2
O4B Cs1 O3 114.85(7) 5_657 2
O4B Cs1 O3 103.85(7) 8_557 2
O1 Cs1 O3 76.40(4) 2 2
O1 Cs1 O3 59.33(4) 4 2
O1 Cs1 O3 134.13(4) 3 2
O1 Cs1 O3 114.91(4) . 2
O3 Cs1 O3 89.045(8) 3 2
O4B Cs1 O3 103.84(7) 7_667 .
O4B Cs1 O3 114.85(7) 6_567 .
O4B Cs1 O3 51.60(8) 5_657 .
O4B Cs1 O3 63.88(7) 8_557 .
O1 Cs1 O3 114.91(4) 2 .
O1 Cs1 O3 134.13(4) 4 .
O1 Cs1 O3 59.33(4) 3 .
O1 Cs1 O3 76.40(4) . .
O3 Cs1 O3 89.047(8) 3 .
O3 Cs1 O3 165.18(6) 2 .
O4B Cs1 O3 114.85(8) 7_667 4
O4B Cs1 O3 63.88(7) 6_567 4
O4B Cs1 O3 103.85(7) 5_657 4
O4B Cs1 O3 51.60(8) 8_557 4
O1 Cs1 O3 134.13(4) 2 4
O1 Cs1 O3 76.40(4) 4 4
O1 Cs1 O3 114.91(4) 3 4
O1 Cs1 O3 59.33(4) . 4
O3 Cs1 O3 165.18(6) 3 4
O3 Cs1 O3 89.047(8) 2 4
O3 Cs1 O3 89.047(8) . 4
O1 Cs2 O1 90.14(6) . 2
O1 Cs2 O1 60.08(3) . 4
O1 Cs2 O1 60.08(3) 2 4
O1 Cs2 O1 60.08(3) . 3
O1 Cs2 O1 60.08(3) 2 3
O1 Cs2 O1 90.14(6) 4 3
O1 Cs2 O4A 163.97(6) . 7_666
O1 Cs2 O4A 99.36(6) 2 7_666
O1 Cs2 O4A 113.89(6) 4 7_666
O1 Cs2 O4A 135.95(6) 3 7_666
O1 Cs2 O4A 113.89(6) . 6_566
O1 Cs2 O4A 135.95(6) 2 6_566
O1 Cs2 O4A 99.35(6) 4 6_566
O1 Cs2 O4A 163.97(6) 3 6_566
O4A Cs2 O4A 50.74(7) 7_666 6_566
O1 Cs2 O4A 135.95(6) . 5_656
O1 Cs2 O4A 113.89(6) 2 5_656
O1 Cs2 O4A 163.97(6) 4 5_656
O1 Cs2 O4A 99.35(6) 3 5_656
O4A Cs2 O4A 50.74(7) 7_666 5_656
O4A Cs2 O4A 74.60(11) 6_566 5_656
O1 Cs2 O4A 99.35(6) . 8_556
O1 Cs2 O4A 163.97(6) 2 8_556
O1 Cs2 O4A 135.94(6) 4 8_556
O1 Cs2 O4A 113.89(6) 3 8_556
O4A Cs2 O4A 74.60(11) 7_666 8_556
O4A Cs2 O4A 50.74(7) 6_566 8_556
O4A Cs2 O4A 50.74(7) 5_656 8_556
O1 Cs2 O2 60.23(4) . 5_556
O1 Cs2 O2 131.85(4) 2 5_556
O1 Cs2 O2 72.01(4) 4 5_556
O1 Cs2 O2 118.65(4) 3 5_556
O4A Cs2 O2 104.13(6) 7_666 5_556
O4A Cs2 O2 53.69(6) 6_566 5_556
O4A Cs2 O2 113.58(6) 5_656 5_556
O4A Cs2 O2 64.13(6) 8_556 5_556
O1 Cs2 O2 131.85(4) . 6_666
O1 Cs2 O2 60.23(4) 2 6_666
O1 Cs2 O2 118.65(4) 4 6_666
O1 Cs2 O2 72.01(4) 3 6_666
O4A Cs2 O2 64.14(6) 7_666 6_666
O4A Cs2 O2 113.58(6) 6_566 6_666
O4A Cs2 O2 53.69(6) 5_656 6_666
O4A Cs2 O2 104.13(6) 8_556 6_666
O2 Cs2 O2 166.13(6) 5_556 6_666
O1 Cs2 O2 72.01(4) . 7_656
O1 Cs2 O2 118.65(4) 2 7_656
O1 Cs2 O2 131.85(4) 4 7_656
O1 Cs2 O2 60.23(4) 3 7_656
O4A Cs2 O2 113.58(6) 7_666 7_656
O4A Cs2 O2 104.13(6) 6_566 7_656
O4A Cs2 O2 64.13(6) 5_656 7_656
O4A Cs2 O2 53.69(6) 8_556 7_656
O2 Cs2 O2 89.164(7) 5_556 7_656
O2 Cs2 O2 89.164(7) 6_666 7_656
O1 Cs2 O2 118.65(4) . 8_566
O1 Cs2 O2 72.01(4) 2 8_566
O1 Cs2 O2 60.23(4) 4 8_566
O1 Cs2 O2 131.85(4) 3 8_566
O4A Cs2 O2 53.69(6) 7_666 8_566
O4A Cs2 O2 64.13(6) 6_566 8_566
O4A Cs2 O2 104.13(6) 5_656 8_566
O4A Cs2 O2 113.58(6) 8_556 8_566
O2 Cs2 O2 89.166(7) 5_556 8_566
O2 Cs2 O2 89.164(7) 6_666 8_566
O2 Cs2 O2 166.13(6) 7_656 8_566
C1 O1 Cs2 136.52(13) . .
C1 O1 Cs1 121.90(13) . .
Cs2 O1 Cs1 91.11(4) . .
C1 O2 Cs2 121.27(12) . 5_556
C3 O3 Cs1 143.5(2) . .
C3 O4A Cs2 135.1(2) . 5_656
C3 O4A Cs1 104.9(2) . 5_657
Cs2 O4A Cs1 112.94(8) 5_656 5_657
C3 O4B Cs1 150.7(2) . 5_657
O1 C1 O2 123.18(19) . .
O1 C1 C2 121.41(18) . .
O2 C1 C2 115.38(17) . .
C1 C2 C2 114.8(2) . 7_656
C1 C2 C2 120.8(2) . 8_556
C2 C2 C2 89.13(4) 7_656 8_556
C1 C2 H2 110.1 . .
C2 C2 H2 110.1 7_656 .
C2 C2 H2 110.1 8_556 .
O3 C3 O4B 126.3(3) . .
O3 C3 O4A 115.4(3) . .
O3 C3 C4 122.3(2) . .
O4B C3 C4 106.3(2) . .
O4A C3 C4 118.5(2) . .
C3 C4 C4 117.2(2) . 7_657
C3 C4 C4 118.6(2) . 8_557
C4 C4 C4 89.22(4) 7_657 8_557
C3 C4 H4 110.1 . .
C4 C4 H4 110.1 7_657 .
C4 C4 H4 110.1 8_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cs1 O4B 3.124(3) 7_667
Cs1 O4B 3.124(3) 6_567
Cs1 O4B 3.124(3) 5_657
Cs1 O4B 3.124(3) 8_557
Cs1 O1 3.1497(15) 2
Cs1 O1 3.1498(15) 4
Cs1 O1 3.1498(15) 3
Cs1 O1 3.1498(15) .
Cs1 O3 3.4362(16) 3
Cs1 O3 3.4362(16) 2
Cs1 O3 3.4362(16) .
Cs1 O3 3.4362(16) 4
Cs2 O1 3.0808(15) .
Cs2 O1 3.0808(15) 2
Cs2 O1 3.0809(15) 4
Cs2 O1 3.0809(15) 3
Cs2 O4A 3.111(3) 7_666
Cs2 O4A 3.111(3) 6_566
Cs2 O4A 3.111(3) 5_656
Cs2 O4A 3.111(3) 8_556
Cs2 O2 3.2822(16) 5_556
Cs2 O2 3.2822(16) 6_666
Cs2 O2 3.2822(16) 7_656
Cs2 O2 3.2822(16) 8_566
O1 C1 1.214(3) .
O2 C1 1.325(2) .
O2 Cs2 3.2822(16) 5_556
O3 C3 1.230(3) .
O4A C3 1.358(4) .
O4A Cs2 3.111(3) 5_656
O4A Cs1 3.798(3) 5_657
O4B C3 1.349(4) .
O4B Cs1 3.124(3) 5_657
C1 C2 1.508(3) .
C2 C2 1.554(2) 7_656
C2 C2 1.554(2) 8_556
C2 H2 0.9800 .
C3 C4 1.509(3) .
C4 C4 1.543(3) 7_657
C4 C4 1.543(3) 8_557
C4 H4 0.9800 .
