Molecular sieving of ethylene from ethane using a rigid metal-organic framework
Rui-Biao Lin; Libo Li; Hao-Long Zhou; Hui Wu; Chaohui He; Shun Li; Rajamani Krishna; Jinping Li; Wei Zhou; Banglin Chen; Nature Materials 17 (2018) 1128–1133; doi:10.1038/s41563-018-0206-2

data_1550335
_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         'C4 Ca O4, (O), O'
_chemical_formula_sum            'C4 Ca O6'
_chemical_formula_weight         184.12
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.575(2)
_cell_length_b                   13.575(2)
_cell_length_c                   7.687(2)
_cell_measurement_reflns_used    4890
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      66.567
_cell_measurement_theta_min      4.606
_cell_volume                     1416.6(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  Burker
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4890
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.570
_diffrn_reflns_theta_max         66.570
_diffrn_reflns_theta_min         6.618
_exptl_absorpt_coefficient_mu    7.615
_exptl_absorpt_correction_T_max  66.567
_exptl_absorpt_correction_T_min  4.606
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       prism
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.15(7)
_refine_ls_extinction_coef       0.0036(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         623
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+16.3881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_full    1.004
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                622
_reflns_number_total             623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            File-4.cif
_cod_data_source_block           CaC4O4_H2O
_cod_original_cell_volume        1416.6(6)
_cod_database_code               1550335
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.85(7)
 0.15(7)
2. Rigid bond restraints
 O3B, O3B, O3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O3B \\sim O3A \\sim O3B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O3B) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O3B) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O3B, O3A, O3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O3A(0.16667) O3B(0.33333)
;
_olex2_submission_special_instructions 'No special instructions were received'