#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:15:17 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180471 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/40/7214020.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_7214020
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 H16 Li4 O13'
_chemical_formula_weight         347.97
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 98.514(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.6635(16)
_cell_length_b                   8.1817(4)
_cell_length_c                   8.1299(6)
_cell_measurement_reflns_used    23295
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.66
_cell_volume                     1425.10(16)
_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 five ω scans with 2° steps (441 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  0.0271
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            23295
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0327
_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)+(0.0494P)²+1.0728P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                1203
_reflns_number_total             1348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41565a.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7214020
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Li1 Li 0.80108(12) 0.6644(3) 0.9447(3) 0.0237(6) Uani 1 1 d .
Li2 Li 0.91913(13) 0.8181(3) 1.0892(3) 0.0266(6) Uani 1 1 d .
O1 O 0.86393(5) 0.80760(13) 0.87531(13) 0.0219(3) Uani 1 1 d .
O2 O 0.90841(5) 1.00731(14) 0.74843(13) 0.0259(3) Uani 1 1 d .
O3 O 0.72265(5) 0.77289(13) 0.84112(12) 0.0224(3) Uani 1 1 d .
O4 O 0.68797(5) 0.95141(13) 0.64312(12) 0.0212(3) Uani 1 1 d .
O5 O 0.91694(5) 0.60635(14) 1.21679(14) 0.0295(3) Uani 1 1 d .
H5A H 0.8801 0.5739 1.2546 0.035 Uiso 1 1 d R
H5B H 0.9395 0.5146 1.2142 0.035 Uiso 1 1 d R
O6 O 1.00764(5) 0.81042(15) 1.05438(14) 0.0277(3) Uani 1 1 d .
H6A H 1.0296 0.7223 1.1166 0.033 Uiso 1 1 d R
H6B H 1.0316 0.9004 1.0892 0.033 Uiso 1 1 d R
O7 O 1.0000 0.3455(2) 1.2500 0.0290(4) Uani 1 2 d S
H7 H 1.0000 0.2798 1.1539 0.035 Uiso 1 1 d R
C1 C 0.86821(7) 0.89680(18) 0.75030(18) 0.0201(3) Uani 1 1 d .
C2 C 0.82374(7) 0.87409(19) 0.58837(17) 0.0216(3) Uani 1 1 d .
H2A H 0.8478 0.8327 0.5057 0.026 Uiso 1 1 calc R
H2B H 0.8083 0.9811 0.5511 0.026 Uiso 1 1 calc R
C3 C 0.76738(7) 0.76169(19) 0.58942(17) 0.0190(3) Uani 1 1 d .
H3 H 0.7819 0.6550 0.6344 0.023 Uiso 1 1 calc R
C4 C 0.72280(7) 0.83446(18) 0.69901(18) 0.0186(3) Uani 1 1 d .
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'
Li Li -0.0003 0.0001 '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'
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 Li1 O1 108.08(13) 4_646 .
O4 Li1 O3 129.46(14) 4_646 7_667
O1 Li1 O3 112.85(14) . 7_667
O4 Li1 O3 113.21(14) 4_646 .
O1 Li1 O3 101.49(12) . .
O3 Li1 O3 86.51(11) 7_667 .
O1 Li2 O2 120.02(14) . 6_576
O1 Li2 O6 110.35(14) . .
O2 Li2 O6 109.19(14) 6_576 .
O1 Li2 O5 111.07(14) . .
O2 Li2 O5 105.72(13) 6_576 .
O6 Li2 O5 98.21(13) . .
C1 O1 Li1 135.97(12) . .
C1 O1 Li2 125.40(13) . .
Li1 O1 Li2 97.50(12) . .
C1 O2 Li2 132.90(12) . 6_575
C4 O3 Li1 138.39(13) . 7_667
C4 O3 Li1 116.62(12) . .
Li1 O3 Li1 93.49(11) 7_667 .
C4 O4 Li1 136.53(13) . 4_656
Li2 O5 H5A 119.8 . .
Li2 O5 H5B 130.6 . .
H5A O5 H5B 105.3 . .
Li2 O6 H6A 111.2 . .
Li2 O6 H6B 116.4 . .
H6A O6 H6B 102.9 . .
O2 C1 O1 123.90(13) . .
O2 C1 C2 115.34(13) . .
O1 C1 C2 120.76(13) . .
C1 C2 C3 118.15(12) . .
C1 C2 H2A 107.8 . .
C3 C2 H2A 107.8 . .
C1 C2 H2B 107.8 . .
C3 C2 H2B 107.8 . .
H2A C2 H2B 107.1 . .
C4 C3 C2 110.05(12) . .
C4 C3 C3 109.53(14) . 7_666
C2 C3 C3 110.31(14) . 7_666
C4 C3 H3 109.0 . .
C2 C3 H3 109.0 . .
C3 C3 H3 109.0 7_666 .
O3 C4 O4 123.42(13) . .
O3 C4 C3 117.78(13) . .
O4 C4 C3 118.80(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Li1 O4 1.911(3) 4_646
Li1 O1 1.942(3) .
Li1 O3 1.956(3) 7_667
Li1 O3 1.990(3) .
Li2 O1 1.961(3) .
Li2 O2 1.964(3) 6_576
Li2 O6 1.980(3) .
Li2 O5 2.023(3) .
O1 C1 1.2657(18) .
O2 C1 1.2570(18) .
O2 Li2 1.964(3) 6_575
O3 C4 1.2609(18) .
O3 Li1 1.956(3) 7_667
O4 C4 1.2609(19) .
O4 Li1 1.911(3) 4_656
O5 H5A 0.9357 .
O5 H5B 0.8970 .
O6 H6A 0.9652 .
O6 H6B 0.9215 .
O7 H7 0.9485 .
C1 C2 1.523(2) .
C2 C3 1.529(2) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.528(2) .
C3 C3 1.547(3) 7_666
C3 H3 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
O5 H5A O4 0.94 1.81 2.7298(15) 167.7 7_667
O5 H5B O7 0.90 1.90 2.7785(17) 166.3 .
O6 H6B O2 0.92 1.87 2.6903(15) 147.3 5_777
O6 H6A O5 0.97 1.90 2.8317(17) 161.5 2_757
O7 H7 O6 0.95 1.83 2.7673(13) 168.2 5_767
