A cooperative adsorbent for the switch-like capture of carbon dioxide from crude natural gas
Siegelman, Rebecca L.; Thompson, Joshua A.; Mason, Jarad; McDonald, Thomas M.; Long, Jeffrey R.; Chemical Science  (2022) –; doi:10.1039/D2SC03570G

data_1567635
_publ_section_title
;
 A cooperative adsorbent for the switch-like capture of carbon dioxide
 from crude natural gas
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03570G
_journal_year                    2022
_chemical_formula_moiety         'C24.24 H31.47 N3.18 O7.38 Zn2'
_chemical_formula_sum            'C24.24 H31.47 N3.18 O7.38 Zn2'
_chemical_formula_weight         616.33
_chemical_name_common            Zn2(dobpdc)(ee-2)0.902(ee-2-CO2)0.690
_chemical_properties_physical    Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-02-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-29 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.5982(10)
_cell_length_b                   21.5982(10)
_cell_length_c                   6.9071(4)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.466
_cell_measurement_theta_min      2.954
_cell_volume                     2790.4(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, Madison WI, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, Madison WI, 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      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            55047
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         29.907
_diffrn_reflns_theta_min         1.934
_diffrn_source
;
Advanced Light Source, station 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1850 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.8448.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             965
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.495(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5009
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0475P)^2^+1.0865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4509
_reflns_number_total             5009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03570g2.cif
_cod_data_source_block           rls206s
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        2790.4(3)
_cod_database_code               1567635
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.505(18)
 0.495(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H,H,H) groups, All N(H)
  groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-C11 = N2-C13
 1.49 with sigma of 0.02
 C20-C19 \\sim C18-C17 \\sim C12-C11 \\sim C14-C13
 with sigma of 0.02
 N4-C19 \\sim N4-C17 \\sim N4-C16
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N3 \\sim N4 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 N3, N4, C15, C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N3(0.451) H3A(0.451) H3B(0.451) N4(0.451) C15(0.451) H15A(0.451)
 H15B(0.451) C16(0.451) H16A(0.451) H16B(0.451) C17(0.451) H17A(0.451)
 H17B(0.451) C18(0.451) H18A(0.2255) H18E(0.2255) H18D(0.2255) H18B(0.2255)
 H18C(0.2255) H18F(0.2255) C19(0.451) H19A(0.451) H19B(0.451) C20(0.451)
 H20A(0.2255) H20B(0.2255) H20C(0.2255) H20D(0.2255) H20E(0.2255) H20F(0.2255)
 O4(0.549) O5(0.345) N1(0.345) H1(0.345) N2(0.345) H2(0.345) C8(0.345)
 C9(0.345) H9A(0.345) H9B(0.345) C10(0.345) H10A(0.345) H10B(0.345) C11(0.345)
 H11A(0.345) H11B(0.345) C12(0.345) H12A(0.345) H12B(0.345) H12C(0.345)
 C13(0.345) H13A(0.345) H13B(0.345) C14(0.345) H14A(0.345) H14B(0.345)
 H14C(0.345)
7.a Ternary CH refined with riding coordinates:
 N2(H2)
7.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), N1(H1)
7.d Disordered Me refined with riding coordinates:
 C18(H18A,H18E,H18D,H18B,H18C,H18F), C20(H20A,H20B,H20C,H20D,H20E,H20F)
7.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              44612
_shelx_hkl_checksum              33010
_olex2_submission_special_instructions 'No special instructions were received'