#------------------------------------------------------------------------------
#$Date: 2019-11-22 15:53:07 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231202 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/03/1550334.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_1550334
loop_
_publ_author_name
'Rui-Biao Lin'
'Libo Li'
'Hao-Long Zhou'
'Hui Wu'
'Chaohui He'
'Shun Li'
'Rajamani Krishna'
'Jinping Li'
'Wei Zhou'
'Banglin Chen'
_publ_section_title
;
 Molecular sieving of ethylene from ethane using a rigid metal-organic
 framework
;
_journal_name_full               'Nature Materials'
_journal_page_first              1128
_journal_page_last               1133
_journal_paper_doi               10.1038/s41563-018-0206-2
_journal_volume                  17
_journal_year                    2018
_chemical_formula_moiety         '[Ca(C4O4)(H2O)]'
_chemical_formula_sum            'C4 H2 Ca O5'
_chemical_formula_weight         170.14
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.6557(2)
_cell_length_b                   13.6557(2)
_cell_length_c                   7.7174(3)
_cell_measurement_reflns_used    1007
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.1060
_cell_measurement_theta_min      6.5580
_cell_volume                     1439.13(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  Atlas
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1248
_diffrn_reflns_theta_full        74.23
_diffrn_reflns_theta_max         74.23
_diffrn_reflns_theta_min         6.59
_exptl_absorpt_coefficient_mu    7.327
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Columnar
_exptl_crystal_F_000             688
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         670
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0649
_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)+(0.0811P)²+24.1677P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1702
_reflns_number_gt                663
_reflns_number_total             670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            File-3.cif
_cod_data_source_block           UTSA-280_activated
_cod_database_code               1550334
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.30602(10) 0.2500 0.1250 0.0037(4) Uiso 1 2 d S . .
O1 O 0.2755(3) 0.0852(3) 0.0804(6) 0.0163(11) Uani 1 1 d U A .
O2 O 0.2686(4) -0.1558(3) 0.0720(6) 0.0150(11) Uani 1 1 d . . .
C1 C 0.2612(5) 0.0212(4) -0.0323(8) 0.0125(13) Uiso 1 1 d . . .
C2 C 0.2599(5) -0.0859(4) -0.0326(8) 0.0094(12) Uani 1 1 d U . .
O3A O 0.4778(8) 0.2500 0.1250 0.001(3) Uiso 0.50 2 d SP A 1
H3AA H 0.4978 0.2415 0.2240 0.002 Uiso 0.50 1 calc PR A 1
O3B O 0.4733(13) 0.2825(14) 0.132(3) 0.006(3) Uiso 0.25 1 d P . 2
H3BA H 0.4967 0.3088 0.0461 0.009 Uiso 0.50 1 calc PR . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 '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 Ca1 O1 159.3(2) . 14_454
O1 Ca1 O3B 111.4(5) . .
O1 Ca1 O3B 89.3(5) 14_454 .
O1 Ca1 O3B 89.3(5) . 14_454
O1 Ca1 O3B 111.4(5) 14_454 14_454
O3B Ca1 O3B 22.2(10) . 14_454
O1 Ca1 O3A 100.36(11) . .
O1 Ca1 O3A 100.36(11) 14_454 .
O3B Ca1 O3A 11.1(5) . .
O3B Ca1 O3A 11.1(5) 14_454 .
O1 Ca1 O2 89.84(16) . 8_554
O1 Ca1 O2 94.62(16) 14_454 8_554
O3B Ca1 O2 77.9(5) . 8_554
O3B Ca1 O2 77.6(5) 14_454 8_554
O3A Ca1 O2 77.52(11) . 8_554
O1 Ca1 O2 94.62(16) . 11
O1 Ca1 O2 89.84(16) 14_454 11
O3B Ca1 O2 77.6(5) . 11
O3B Ca1 O2 77.9(5) 14_454 11
O3A Ca1 O2 77.52(11) . 11
O2 Ca1 O2 155.0(2) 8_554 11
O1 Ca1 O2 82.21(16) . 4
O1 Ca1 O2 81.25(16) 14_454 4
O3B Ca1 O2 141.2(5) . 4
O3B Ca1 O2 142.1(5) 14_454 4
O3A Ca1 O2 143.07(10) . 4
O2 Ca1 O2 65.61(16) 8_554 4
O2 Ca1 O2 139.33(13) 11 4
O1 Ca1 O2 81.25(16) . 15_454
O1 Ca1 O2 82.21(16) 14_454 15_454
O3B Ca1 O2 142.1(5) . 15_454
O3B Ca1 O2 141.2(5) 14_454 15_454
O3A Ca1 O2 143.07(10) . 15_454
O2 Ca1 O2 139.33(13) 8_554 15_454
O2 Ca1 O2 65.61(16) 11 15_454
O2 Ca1 O2 73.9(2) 4 15_454
O1 Ca1 C2 80.41(16) . 4
O1 Ca1 C2 79.45(17) 14_454 4
O3B Ca1 C2 162.0(5) . 4
O3B Ca1 C2 163.1(5) 14_454 4
O3A Ca1 C2 166.42(11) . 4
O2 Ca1 C2 88.95(15) 8_554 4
O2 Ca1 C2 116.02(16) 11 4
O2 Ca1 C2 23.36(15) 4 4
O2 Ca1 C2 50.51(15) 15_454 4
O1 Ca1 C2 79.45(17) . 15_454
O1 Ca1 C2 80.41(16) 14_454 15_454
O3B Ca1 C2 163.1(5) . 15_454
O3B Ca1 C2 162.0(5) 14_454 15_454
O3A Ca1 C2 166.42(11) . 15_454
O2 Ca1 C2 116.02(16) 8_554 15_454
O2 Ca1 C2 88.95(15) 11 15_454
O2 Ca1 C2 50.51(15) 4 15_454
O2 Ca1 C2 23.36(15) 15_454 15_454
C2 Ca1 C2 27.2(2) 4 15_454
O1 Ca1 Ca1 78.20(11) . 10_554
O1 Ca1 Ca1 94.12(11) 14_454 10_554
O3B Ca1 Ca1 112.6(5) . 10_554
O3B Ca1 Ca1 109.8(5) 14_454 10_554
O3A Ca1 Ca1 111.63(3) . 10_554
O2 Ca1 Ca1 34.65(10) 8_554 10_554
O2 Ca1 Ca1 169.10(12) 11 10_554
O2 Ca1 Ca1 32.27(10) 4 10_554
O2 Ca1 Ca1 104.85(11) 15_454 10_554
C2 Ca1 Ca1 55.06(11) 4 10_554
C2 Ca1 Ca1 81.73(12) 15_454 10_554
C1 O1 Ca1 144.3(4) . .
C2 O2 Ca1 141.1(4) . 12_545
C2 O2 Ca1 102.6(4) . 3
Ca1 O2 Ca1 113.08(16) 12_545 3
O1 C1 C2 134.7(6) . .
O1 C1 C1 135.6(3) . 5_554
C2 C1 C1 89.8(4) . 5_554
O2 C2 C2 130.5(3) . 5_554
O2 C2 C1 139.3(6) . .
C2 C2 C1 90.2(4) 5_554 .
O2 C2 Ca1 54.1(3) . 3
C2 C2 Ca1 76.42(11) 5_554 3
C1 C2 Ca1 166.6(4) . 3
Ca1 O3A H3AA 109.5 . .
O3B O3B Ca1 78.9(5) 14_454 .
O3B O3B H3BA 109.5 14_454 .
Ca1 O3B H3BA 116.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.314(4) .
Ca1 O1 2.314(4) 14_454
Ca1 O3B 2.327(18) .
Ca1 O3B 2.327(18) 14_454
Ca1 O3A 2.345(12) .
Ca1 O2 2.409(5) 8_554
Ca1 O2 2.409(5) 11
Ca1 O2 2.566(5) 4
Ca1 O2 2.566(5) 15_454
Ca1 C2 3.093(6) 4
Ca1 C2 3.093(6) 15_454
Ca1 Ca1 4.1510(10) 10_554
O1 C1 1.249(8) .
O2 C2 1.256(7) .
O2 Ca1 2.409(5) 12_545
O2 Ca1 2.566(5) 3
C1 C2 1.463(8) .
C1 C1 1.463(13) 5_554
C2 C2 1.452(12) 5_554
C2 Ca1 3.093(6) 3
O3A H3AA 0.8200 .
O3B O3B 0.89(4) 14_454
O3B H3BA 0.8200 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O1 Ca1 O1 C1 88.9(7) 14_454 . . .
O3B Ca1 O1 C1 -90.7(9) . . . .
O3B Ca1 O1 C1 -91.4(8) 14_454 . . .
O3A Ca1 O1 C1 -91.1(7) . . . .
O2 Ca1 O1 C1 -13.8(7) 8_554 . . .
O2 Ca1 O1 C1 -169.2(7) 11 . . .
O2 Ca1 O1 C1 51.6(7) 4 . . .
O2 Ca1 O1 C1 126.4(7) 15_454 . . .
C2 Ca1 O1 C1 75.2(7) 4 . . .
C2 Ca1 O1 C1 102.7(7) 15_454 . . .
Ca1 Ca1 O1 C1 19.1(7) 10_554 . . .
Ca1 O1 C1 C2 166.7(6) . . . .
Ca1 O1 C1 C1 -13.3(16) . . . 5_554
Ca1 O2 C2 C2 -153.9(7) 12_545 . . 5_554
Ca1 O2 C2 C2 2.4(11) 3 . . 5_554
Ca1 O2 C2 C1 24.1(14) 12_545 . . .
Ca1 O2 C2 C1 -179.6(8) 3 . . .
Ca1 O2 C2 Ca1 -156.3(8) 12_545 . . 3
O1 C1 C2 O2 2.9(16) . . . .
C1 C1 C2 O2 -177.1(8) 5_554 . . .
O1 C1 C2 C2 -178.7(8) . . . 5_554
C1 C1 C2 C2 1.3(8) 5_554 . . 5_554
O1 C1 C2 Ca1 -175.9(15) . . . 3
C1 C1 C2 Ca1 4(2) 5_554 . . 3
O1 Ca1 O3B O3B -2(3) . . . 14_454
O1 Ca1 O3B O3B 178(2) 14_454 . . 14_454
O3A Ca1 O3B O3B 0.000(1) . . . 14_454
O2 Ca1 O3B O3B -87(2) 8_554 . . 14_454
O2 Ca1 O3B O3B 88(2) 11 . . 14_454
O2 Ca1 O3B O3B -107(2) 4 . . 14_454
O2 Ca1 O3B O3B 102(2) 15_454 . . 14_454
C2 Ca1 O3B O3B -130.7(19) 4 . . 14_454
C2 Ca1 O3B O3B 126(2) 15_454 . . 14_454
Ca1 Ca1 O3B O3B -87(2) 10_554 . . 14_454
