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_4126404
_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         'C20.44 H26.72 N3.22 O6.7 Zn2'
_chemical_formula_sum            'C20.44 H26.72 N3.22 O6.7 Zn2'
_chemical_formula_weight         555.49
_chemical_name_common            Zn2(dobpdc)(dmen)1.61-(H2O)0.70
_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             2017-05-16
_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                   21.4217(8)
_cell_length_b                   21.4217(8)
_cell_length_c                   6.8386(3)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.194
_cell_measurement_theta_min      2.736
_cell_volume                     2717.73(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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     0.8856
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            35351
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        32.097
_diffrn_reflns_theta_max         36.194
_diffrn_reflns_theta_min         2.369
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.440
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1569 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission is 0.7861.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    'pale yellow'
_exptl_crystal_density_diffrn    1.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4495
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0785P)^2^+3.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4038
_reflns_number_total             4495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07612_si_005.cif
_cod_data_source_block           rls047s
_cod_original_cell_volume        2717.7(2)
_cod_database_code               4126404
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.581
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(2)
 0.46(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 N1, N2B, C8B, C9B, C10B, C11B, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, N2A, C8A, C9A, C10A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H1BC(0.494) H1BD(0.494) H1AA(0.311) H1AB(0.311) N2A(0.494)
 H2AA(0.329) H2AB(0.329) H2AC(0.329) C8A(0.494) H8AA(0.494) H8AB(0.494)
 C9A(0.494) C10A(0.494) H10A(0.494) H10B(0.494) H10C(0.494) C11A(0.494)
 H11A(0.494) H11B(0.494) H11C(0.494) N2B(0.311) H2BA(0.207) H2BB(0.207)
 H2BC(0.207) C8B(0.311) H8BA(0.311) H8BB(0.311) C9B(0.311) C10B(0.311)
 H10D(0.311) H10E(0.311) H10F(0.311) C11B(0.311) H11D(0.311) H11E(0.311)
 H11F(0.311) O4(0.35)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1BC,H1BD), N1(H1AA,H1AB), C8A(H8AA,H8AB), C8B(H8BA,H8BB)
5.b Me refined with riding coordinates:
 N2B(H2BA,H2BB,H2BC)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
5.d Idealised Me refined as rotating group:
 N2A(H2AA,H2AB,H2AC), C10A(H10A,H10B,H10C), C11A(H11A,H11B,H11C), C10B(H10D,
 H10E,H10F), C11B(H11D,H11E,H11F)
;
_shelx_res_checksum              34607
_shelx_hkl_checksum              65099
_olex2_submission_special_instructions 'No special instructions were received'