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_4126401
_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         'C21.89 H25.94 N2.85 O7.55 Zn2'
_chemical_formula_sum            'C21.89 H25.94 N2.85 O7.55 Zn2'
_chemical_formula_weight         580.52
_chemical_name_common            Zn2(dobpdc)(dmpn)0.65(dmpn-CO2)0.774
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-22
_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                   21.6530(11)
_cell_length_b                   21.6530(11)
_cell_length_c                   6.7873(4)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.910
_cell_measurement_theta_min      2.785
_cell_volume                     2755.9(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_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 0.998
_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     0.6888
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            57085
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.411
_diffrn_reflns_theta_max         30.954
_diffrn_reflns_theta_min         2.105
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.7664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1126 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.8535.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    'pale yellow'
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.838
_refine_diff_density_min         -1.821
_refine_diff_density_rms         0.112
_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   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         6402
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0411P)^2^+6.2666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5853
_reflns_number_total             6402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07612_si_001.cif
_cod_data_source_block           rls134s
_cod_database_code               4126401
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.779
_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 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
 C10A-C9 \\sim C10B-C9 \\sim C11A-C9 \\sim C11B-C9 \\sim C12B-C9 \\sim C12A-C9
\\sim C9-C8
 with sigma of 0.02
 N2B-C12B \\sim N2A-C12A
 with sigma of 0.02
 C10B-C11B \\sim C10A-C11A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim C8 \\sim C9 \\sim N2B \\sim C10B \\sim C11B \\sim C12B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
N1 \\sim C8 \\sim C9 \\sim O4 \\sim O5 \\sim N2A \\sim C10A \\sim C11A \\sim
C12A \\sim C13: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C10A \\sim C11A \\sim C10B \\sim C11B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 N1, C8, C9, O4, O5, N2A, C10A, C11A, C12A, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C8, C9, N2B, 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: C8(0.712) H8A(0.712) H8B(0.712) C9(0.712) O4(0.387) O5(0.387)
 N2A(0.387) H2A(0.387) C10A(0.387) H10A(0.387) H10B(0.387) H10C(0.387)
 C11A(0.387) H11A(0.387) H11B(0.387) H11C(0.387) C12A(0.387) H12A(0.387)
 H12B(0.387) C13(0.387) N2B(0.325) H2BA(0.217) H2BB(0.217) H2BC(0.217)
 C10B(0.325) H10D(0.325) H10E(0.325) H10F(0.325) C11B(0.325) H11D(0.325)
 H11E(0.325) H11F(0.325) C12B(0.325) H12C(0.325) H12D(0.325)
7.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C8(H8A,H8B), C12A(H12A,H12B), C12B(H12C,H12D)
7.b Me refined with riding coordinates:
 C10A(H10A,H10B,H10C)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), N2A(H2A)
7.d Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), N2B(H2BA,H2BB,H2BC), C10B(H10D,H10E,H10F), C11B(H11D,
 H11E,H11F)
;
_shelx_res_checksum              29409
_shelx_hkl_checksum              90880
_olex2_submission_special_instructions 'No special instructions were received'