#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:15:17 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180471 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/40/7214019.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_7214019
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_absolute_configuration unk
_chemical_formula_sum            'C8 H10 Li2 O10'
_chemical_formula_weight         280.04
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   4.9227(2)
_cell_length_b                   13.9837(3)
_cell_length_c                   15.7876(3)
_cell_measurement_reflns_used    26925
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.96
_cell_volume                     1086.78(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and three ω scans with 1° steps (683 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  0.0126
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26925
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.6(10)
_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     182
_refine_ls_number_reflns         1911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0308
_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)+(0.0582P)²+0.1623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                1803
_reflns_number_total             1911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41565a.txt
_cod_data_source_block           1
_cod_database_code               7214019
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+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
Li1 Li 0.6806(6) 0.7076(2) 0.56522(18) 0.0258(5) Uani 1 1 d .
Li2 Li 0.6576(6) 0.3057(2) 0.56084(17) 0.0249(5) Uani 1 1 d .
O1 O 0.8616(3) 0.58585(8) 0.57806(6) 0.0231(2) Uani 1 1 d .
O2 O 0.8415(2) 0.42697(7) 0.56887(6) 0.0220(2) Uani 1 1 d .
O3 O 0.3728(3) 0.29059(7) 0.64514(6) 0.0215(2) Uani 1 1 d .
O4 O 0.1334(3) 0.32790(8) 0.76125(7) 0.0231(2) Uani 1 1 d .
H4 H 0.0464 0.2739 0.7527 0.028 Uiso 1 1 d R
O5 O 0.7655(3) 0.47825(9) 0.88646(7) 0.0285(3) Uani 1 1 d .
O6 O 0.3880(2) 0.55102(8) 0.93234(6) 0.0261(2) Uani 1 1 d .
H6 H 0.4882 0.5506 0.9808 0.031 Uiso 1 1 d R
O7 O 0.1279(3) 0.68205(8) 0.76006(6) 0.0221(2) Uani 1 1 d .
O8 O 0.3806(3) 0.72011(8) 0.64705(6) 0.0224(2) Uani 1 1 d .
O9 O 0.9929(3) 0.79854(8) 0.54952(7) 0.0242(2) Uani 1 1 d .
H9A H 0.9601 0.8589 0.5617 0.029 Uiso 1 1 d R
H9B H 1.1029 0.7710 0.5862 0.029 Uiso 1 1 d R
O10 O 0.9645(2) 0.20990(8) 0.55126(6) 0.0219(2) Uani 1 1 d .
H10A H 1.0933 0.2217 0.5853 0.026 Uiso 1 1 d R
H10B H 0.9175 0.1566 0.5670 0.026 Uiso 1 1 d R
C1 C 0.5148(3) 0.50547(9) 0.65526(8) 0.0176(2) Uani 1 1 d .
H1 H 0.3461 0.5054 0.6223 0.021 Uiso 1 1 calc R
C2 C 0.5021(3) 0.42786(9) 0.72555(8) 0.0177(3) Uani 1 1 d .
H2 H 0.6861 0.4073 0.7407 0.021 Uiso 1 1 calc R
C3 C 0.4011(3) 0.50394(9) 0.78874(8) 0.0178(2) Uani 1 1 d .
H3 H 0.2027 0.5035 0.7939 0.021 Uiso 1 1 calc R
C4 C 0.5004(3) 0.58216(10) 0.72598(8) 0.0178(3) Uani 1 1 d .
H4A H 0.6842 0.6028 0.7413 0.021 Uiso 1 1 calc R
C5 C 0.7579(3) 0.50775(11) 0.59653(8) 0.0189(2) Uani 1 1 d .
C6 C 0.3262(3) 0.34213(10) 0.70831(9) 0.0184(3) Uani 1 1 d .
C7 C 0.5373(3) 0.50761(10) 0.87377(8) 0.0193(3) Uani 1 1 d .
C8 C 0.3253(3) 0.66780(10) 0.70939(9) 0.0189(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
O1 Li1 O8 110.82(14) . .
O1 Li1 O9 102.57(15) . .
O8 Li1 O9 126.70(15) . .
O1 Li1 O9 105.41(14) . 4_466
O8 Li1 O9 104.31(15) . 4_466
O9 Li1 O9 105.31(13) . 4_466
O2 Li2 O3 112.89(14) . .
O2 Li2 O10 111.92(14) . 4_456
O3 Li2 O10 104.38(15) . 4_456
O2 Li2 O10 103.70(15) . .
O3 Li2 O10 121.17(15) . .
O10 Li2 O10 102.38(12) 4_456 .
C5 O1 Li1 127.63(14) . .
C5 O2 Li2 130.46(14) . .
C6 O3 Li2 127.95(13) . .
C6 O4 H4 113.2 . .
C7 O6 H6 106.4 . .
C8 O8 Li1 128.64(13) . .
Li1 O9 Li1 115.48(9) . 4_566
Li1 O9 H9A 116.1 . .
Li1 O9 H9A 108.5 4_566 .
Li1 O9 H9B 96.5 . .
Li1 O9 H9B 106.7 4_566 .
H9A O9 H9B 112.8 . .
Li2 O10 Li2 119.20(9) 4_556 .
Li2 O10 H10A 103.0 4_556 .
Li2 O10 H10A 112.5 . .
Li2 O10 H10B 107.5 4_556 .
Li2 O10 H10B 111.7 . .
H10A O10 H10B 101.2 . .
C5 C1 C4 117.55(11) . .
C5 C1 C2 118.95(11) . .
C4 C1 C2 88.11(9) . .
C5 C1 H1 110.2 . .
C4 C1 H1 110.2 . .
C2 C1 H1 110.2 . .
C6 C2 C3 118.80(12) . .
C6 C2 C1 116.81(11) . .
C3 C2 C1 89.61(10) . .
C6 C2 H2 110.0 . .
C3 C2 H2 110.0 . .
C1 C2 H2 110.0 . .
C7 C3 C2 117.28(11) . .
C7 C3 C4 113.90(11) . .
C2 C3 C4 88.37(9) . .
C7 C3 H3 111.8 . .
C2 C3 H3 111.8 . .
C4 C3 H3 111.8 . .
C8 C4 C1 116.95(11) . .
C8 C4 C3 119.51(12) . .
C1 C4 C3 89.23(9) . .
C8 C4 H4A 109.8 . .
C1 C4 H4A 109.8 . .
C3 C4 H4A 109.8 . .
O1 C5 O2 124.39(13) . .
O1 C5 C1 119.20(13) . .
O2 C5 C1 116.40(12) . .
O3 C6 O4 124.50(14) . .
O3 C6 C2 119.86(13) . .
O4 C6 C2 115.64(12) . .
O5 C7 O6 123.52(13) . .
O5 C7 C3 123.36(13) . .
O6 C7 C3 113.03(12) . .
O8 C8 O7 124.47(14) . .
O8 C8 C4 118.54(14) . .
O7 C8 C4 117.00(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Li1 O1 1.932(3) .
Li1 O8 1.970(3) .
Li1 O9 2.011(3) .
Li1 O9 2.035(3) 4_466
Li1 Li1 3.422(4) 4_466
Li2 O2 1.927(3) .
Li2 O3 1.945(3) .
Li2 O10 2.021(3) 4_456
Li2 O10 2.024(3) .
Li2 Li2 3.489(4) 4_556
O1 C5 1.2404(18) .
O2 C5 1.2790(17) .
O3 C6 1.2517(17) .
O4 C6 1.2802(19) .
O4 H4 0.8784 .
O5 C7 1.2129(19) .
O6 C7 1.3278(17) .
O6 H6 0.9101 .
O7 C8 1.2747(19) .
O8 C8 1.2562(17) .
O9 Li1 2.035(3) 4_566
O9 H9A 0.8806 .
O9 H9B 0.8817 .
O10 Li2 2.021(3) 4_556
O10 H10A 0.8476 .
O10 H10B 0.8196 .
C1 C5 1.5141(18) .
C1 C4 1.5498(18) .
C1 C2 1.5533(18) .
C1 H1 0.9800 .
C2 C6 1.504(2) .
C2 C3 1.5410(18) .
C2 H2 0.9800 .
C3 C7 1.5013(18) .
C3 C4 1.5549(18) .
C3 H3 0.9800 .
C4 C8 1.499(2) .
C4 H4A 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
O4 H4 O7 0.88 1.56 2.4345(15) 175.6 3_546
O6 H6 O2 0.91 1.65 2.5523(15) 168.6 2_665
O9 H9A O5 0.88 2.30 2.9583(16) 131.8 3_756
O9 H9B O8 0.88 1.82 2.6864(16) 168.9 1_655
O10 H10A O3 0.85 1.93 2.7403(16) 160.4 1_655
O10 H10B O6 0.82 2.11 2.8310(16) 147.2 3_646
