A Diaminopropane-Appended Metal‒Organic Framework Enabling Efficient CO2 Capture from Coal Flue Gas via a Mixed Adsorption Mechanism
Milner, Phillip J.; Siegelman, Rebecca L.; Forse, Alexander C.; Gonzalez, Miguel I.; Runčevski, Tomče; Martell, Jeffrey D.; Reimer, Jeffrey A.; Long, Jeffrey R.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07612

data_4126403
_publ_section_title
;
 A Diaminopropane-Appended Metal--Organic Framework Enabling Efficient CO2
 Capture from Coal Flue Gas via a Mixed Adsorption Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07612
_journal_year                    2017
_chemical_formula_moiety         '0.33(C65.74 H80.45 N10.4 O23.86 Zn6)'
_chemical_formula_sum            'C21.91 H26.82 N3.47 O7.95 Zn2'
_chemical_formula_weight         596.77
_chemical_name_common            Zn2(dobpdc)(dmen)0.976(dmen-CO2)0.758
_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             2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 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                   21.3008(9)
_cell_length_b                   21.3008(9)
_cell_length_c                   6.8770(3)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.894
_cell_measurement_theta_min      3.186
_cell_volume                     2702.2(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 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  0.0778
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            40910
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         33.600
_diffrn_reflns_theta_min         2.085
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.725
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.5886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1400 before and 0.0848 after correction.
The Ratio of minimum to maximum transmission is 0.6628.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             919
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.571
_refine_diff_density_min         -2.196
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5513
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0728
_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^)+(0.0434P)^2^+15.4066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1775
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5333
_reflns_number_total             5513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07612_si_004.cif
_cod_data_source_block           rls132s
_cod_original_cell_volume        2702.2(3)
_cod_database_code               4126403
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.748
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(3)
 0.47(3)
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, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2A-C10A
 1.47 with sigma of 0.02
 C10B-C11B \\sim C10B-C9B \\sim C10B-C12B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim N1A \\sim N2A \\sim C8 \\sim C9A \\sim C10A \\sim C11A \\sim
C12A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N1B \\sim N2B \\sim C9B \\sim C10B \\sim C11B \\sim C12B: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
O4 \\sim N1B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O4, O5, N1A, N2A, C8, C9A, C10A, C11A, C12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1B, N2B, C9B, C10B, C11B, C12B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O4(0.488) O5(0.488) N1A(0.488) H1A(0.488) N2A(0.488) H2AA(0.488)
 H2AB(0.488) H2AC(0.488) C8(0.488) C9A(0.488) H9AA(0.488) H9AB(0.488)
 C10A(0.488) C11A(0.488) H11A(0.488) H11B(0.488) H11C(0.488) C12A(0.488)
 H12A(0.488) H12B(0.488) H12C(0.488) N1B(0.379) H1BA(0.379) H1BB(0.379)
 N2B(0.379) H2BA(0.253) H2BB(0.253) H2BC(0.253) C9B(0.379) H9BA(0.379)
 H9BB(0.379) C10B(0.379) C11B(0.379) H11D(0.19) H11E(0.19) H11F(0.19)
 H11G(0.19) H11H(0.19) H11I(0.19) C12B(0.379) H12D(0.379) H12E(0.379)
 H12F(0.379)
7.a Secondary CH2 refined with riding coordinates:
 C9A(H9AA,H9AB), N1B(H1BA,H1BB), C9B(H9BA,H9BB)
7.b Me refined with riding coordinates:
 N2B(H2BA,H2BB,H2BC)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), N1A(H1A)
7.d Disordered Me refined with riding coordinates:
 C11B(H11D,H11E,H11F,H11G,H11H,H11I)
7.e Idealised Me refined as rotating group:
 N2A(H2AA,H2AB,H2AC), C11A(H11A,H11B,H11C), C12A(H12A,H12B,H12C), C12B(H12D,
 H12E,H12F)
;
_shelx_res_checksum              33041
_shelx_hkl_checksum              17643
_olex2_submission_special_instructions 'No special instructions were received'