#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:15:17 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180471 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/40/7214021.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_7214021
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 Na O8'
_chemical_formula_weight         254.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.272(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.3722(2)
_cell_length_b                   13.4257(11)
_cell_length_c                   12.4510(10)
_cell_measurement_reflns_used    31005
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      3.27
_cell_volume                     897.81(11)
_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 six ω scans with 2° steps (450 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  0.0262
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31005
_diffrn_reflns_theta_full        30.49
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0369
_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)+(0.0549P)²+0.1647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                2148
_reflns_number_total             2734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41565a.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7214021
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Na Na 0.25226(10) 0.72590(4) 0.94669(4) 0.02616(15) Uani 1 1 d .
O1 O 0.35282(18) 0.74555(8) 0.76215(8) 0.0258(2) Uani 1 1 d .
O2 O 0.49857(18) 0.76641(8) 0.59739(8) 0.0243(2) Uani 1 1 d .
O3 O 0.65641(19) 0.63096(8) 0.97875(8) 0.0293(2) Uani 1 1 d .
H3 H 0.7628 0.6491 1.0354 0.035 Uiso 1 1 d R
O4 O 1.01869(18) 0.58171(8) 0.90945(8) 0.0253(2) Uani 1 1 d .
O5 O 0.58632(17) 0.35169(7) 0.62007(8) 0.0226(2) Uani 1 1 d .
O6 O 0.44640(19) 0.38004(7) 0.78424(8) 0.0249(2) Uani 1 1 d .
H6 H 0.3396 0.3293 0.7674 0.030 Uiso 1 1 d R
O7 O 1.02527(18) 0.64820(8) 0.50605(8) 0.0254(2) Uani 1 1 d .
H7 H 1.1903 0.6451 0.4739 0.030 Uiso 1 1 d R
O8 O 1.20651(18) 0.53486(8) 0.61331(9) 0.0286(2) Uani 1 1 d .
C1 C 0.7054(2) 0.65155(10) 0.71434(10) 0.0182(2) Uani 1 1 d .
H1 H 0.8578 0.6871 0.7358 0.022 Uiso 1 1 calc R
C2 C 0.6479(2) 0.57044(9) 0.80017(10) 0.0192(2) Uani 1 1 d .
H2 H 0.4693 0.5627 0.8121 0.023 Uiso 1 1 calc R
C3 C 0.7516(2) 0.49081(10) 0.72355(10) 0.0187(2) Uani 1 1 d .
H3A H 0.9180 0.4695 0.7478 0.022 Uiso 1 1 calc R
C4 C 0.7701(2) 0.56834(9) 0.63210(10) 0.0185(2) Uani 1 1 d .
H4 H 0.6389 0.5596 0.5770 0.022 Uiso 1 1 calc R
C5 C 0.5033(2) 0.72603(10) 0.68742(10) 0.0193(3) Uani 1 1 d .
C6 C 0.7940(3) 0.59100(10) 0.90193(10) 0.0216(3) Uani 1 1 d .
C7 C 0.5849(2) 0.40116(10) 0.70379(10) 0.0197(3) Uani 1 1 d .
C8 C 1.0231(2) 0.58017(10) 0.58433(10) 0.0199(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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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 Na O7 94.97(4) 4_576 4_576
O2 Na O4 82.92(4) 4_576 1_455
O7 Na O4 169.67(4) 4_576 1_455
O2 Na O1 155.95(4) 4_576 .
O7 Na O1 94.03(4) 4_576 .
O4 Na O1 91.86(4) 1_455 .
O2 Na O3 113.95(4) 4_576 .
O7 Na O3 77.64(4) 4_576 .
O4 Na O3 93.92(4) 1_455 .
O1 Na O3 89.76(4) . .
O2 Na O5 79.21(4) 4_576 2_556
O7 Na O5 93.48(4) 4_576 2_556
O4 Na O5 96.04(4) 1_455 2_556
O1 Na O5 78.02(4) . 2_556
O3 Na O5 164.45(4) . 2_556
C5 O1 Na 147.32(9) . .
C5 O2 Na 137.63(9) . 4_675
C6 O3 Na 125.03(8) . .
C6 O3 H3 107.9 . .
Na O3 H3 119.7 . .
C6 O4 Na 117.15(9) . 1_655
C7 O5 Na 126.89(8) . 2_546
C7 O6 H6 110.8 . .
C8 O7 Na 134.96(8) . 4_675
C8 O7 H7 106.9 . .
Na O7 H7 117.8 4_675 .
C5 C1 C4 119.92(10) . .
C5 C1 C2 117.54(10) . .
C4 C1 C2 90.01(9) . .
C5 C1 H1 109.3 . .
C4 C1 H1 109.3 . .
C2 C1 H1 109.3 . .
C6 C2 C3 117.37(11) . .
C6 C2 C1 110.00(10) . .
C3 C2 C1 88.89(9) . .
C6 C2 H2 112.8 . .
C3 C2 H2 112.8 . .
C1 C2 H2 112.8 . .
C7 C3 C2 115.46(10) . .
C7 C3 C4 117.50(11) . .
C2 C3 C4 91.08(9) . .
C7 C3 H3A 110.5 . .
C2 C3 H3A 110.5 . .
C4 C3 H3A 110.5 . .
C8 C4 C3 115.82(11) . .
C8 C4 C1 113.61(11) . .
C3 C4 C1 88.85(9) . .
C8 C4 H4 112.2 . .
C3 C4 H4 112.2 . .
C1 C4 H4 112.2 . .
O2 C5 O1 124.59(12) . .
O2 C5 C1 119.28(11) . .
O1 C5 C1 116.07(11) . .
O4 C6 O3 123.45(12) . .
O4 C6 C2 123.09(12) . .
O3 C6 C2 113.04(11) . .
O5 C7 O6 123.36(12) . .
O5 C7 C3 123.27(11) . .
O6 C7 C3 113.35(11) . .
O8 C8 O7 122.85(12) . .
O8 C8 C4 124.59(12) . .
O7 C8 C4 112.56(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na O2 2.3457(11) 4_576
Na O7 2.3465(11) 4_576
Na O4 2.3477(12) 1_455
Na O1 2.3866(11) .
Na O3 2.5416(12) .
Na O5 2.6047(11) 2_556
O1 C5 1.2734(16) .
O2 C5 1.2448(16) .
O2 Na 2.3457(11) 4_675
O3 C6 1.3343(17) .
O3 H3 0.9301 .
O4 C6 1.2150(17) .
O4 Na 2.3477(12) 1_655
O5 C7 1.2362(16) .
O5 Na 2.6047(11) 2_546
O6 C7 1.2926(16) .
O6 H6 0.9120 .
O7 C8 1.3360(16) .
O7 Na 2.3465(11) 4_675
O7 H7 0.9819 .
O8 C8 1.2066(17) .
C1 C5 1.5082(18) .
C1 C4 1.5599(18) .
C1 C2 1.5612(18) .
C1 H1 0.9800 .
C2 C6 1.5011(18) .
C2 C3 1.5449(18) .
C2 H2 0.9800 .
C3 C7 1.5167(18) .
C3 C4 1.5475(18) .
C3 H3A 0.9800 .
C4 C8 1.5039(17) .
C4 H4 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
O3 H3 O2 0.93 1.86 2.7090(14) 151.4 4_676
O3 H3 O6 0.93 2.56 3.0179(14) 110.5 3_667
O6 H6 O1 0.91 1.57 2.4773(14) 177.5 2_546
O6 H6 O2 0.91 2.64 3.2203(13) 122.0 2_546
O7 H7 O5 0.98 1.69 2.6392(13) 160.1 3_766
