Unexpected Diffusion Anisotropy of Carbon Dioxide in the Metal-Organic Framework Zn2(dobpdc).
Forse, Alexander C.; Gonzalez, Miguel I.; Siegelman, Rebecca L.; Witherspoon, Velencia J.; Jawahery, Sudi; Mercado, Rocio; Milner, Phillip J.; Martell, Jeffrey D.; Smit, Berend; Blümich, Bernhard; Long, Jeffrey R.; Reimer, Jeffrey A.; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b09453

data_4127080
_publ_section_title
;
 Unexpected Diffusion Anisotropy of Carbon Dioxide in the Metal-Organic
 Framework Zn2(dobpdc).
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09453
_journal_year                    2018
_chemical_formula_moiety         '(C14 H6 O6 Zn2), 1.26(C O2)'
_chemical_formula_sum            'C15.23 H6 O8.46 Zn2'
_chemical_formula_weight         455.06
_chemical_name_common            Zn2(dobpdc)(CO2)1.26
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.640(2)
_cell_length_b                   21.640(2)
_cell_length_c                   6.7928(8)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.370
_cell_volume                     2754.8(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON100 CMOS detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            25719
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         28.572
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1913 before and 0.0605 after correction.
The Ratio of minimum to maximum transmission is 0.7070.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    'pale yellow'
_exptl_crystal_density_diffrn    0.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             675
_exptl_crystal_size_max          0.1071
_exptl_crystal_size_mid          0.05355
_exptl_crystal_size_min          0.05355
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3627
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.7922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3344
_reflns_number_total             3627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09453_si_003.cif
_cod_data_source_block           gcell134s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2754.8(7)
_cod_database_code               4127080
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.841
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.60(2)
 0.40(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 O5A-C8A = O4-C8A = O4-C8B = O5B-C8B
 1.163 with sigma of 0.02
 O5A-O4
 2.326 with sigma of 0.005
 O4-O5B
 2.326 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
O4 \\sim O5B \\sim C8B \\sim C8A \\sim O5A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O4, C8B, C8A, O5A, O5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O4(0.631) O5B(0.296) C8B(0.296) C8A(0.335) O5A(0.335)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C5(H5)
;
_shelx_res_checksum              91317
_shelx_hkl_checksum              97855
_olex2_submission_special_instructions 'No special instructions were received'