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_4126402
_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         'C25.39 H32.07 N3.52 O6 Zn2'
_chemical_formula_sum            'C25.39 H32.07 N3.52 O6 Zn2'
_chemical_formula_weight         616.59
_chemical_name_common            Zn2(dobpdc)(mpn)1.758(C7H8)0.622
_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     dual
_audit_creation_date             2017-05-21
_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                   21.527(2)
_cell_length_b                   21.527(2)
_cell_length_c                   6.8199(8)
_cell_measurement_reflns_used    9373
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.268
_cell_measurement_theta_min      3.152
_cell_volume                     2737.0(5)
_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 0.996
_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     0.7749
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.996
_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            46798
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         35.278
_diffrn_reflns_theta_min         3.152
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1546 before and 0.0995 after correction.
The Ratio of minimum to maximum transmission is 0.7691.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    'pale yellow'
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.117
_refine_diff_density_min         -2.818
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         6333
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0290P)^2^+9.7772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1418
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6206
_reflns_number_total             6333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07612_si_003.cif
_cod_data_source_block           rls113s
_cod_original_cell_volume        2737.0(7)
_cod_database_code               4126402
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.712
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.64(2)
 0.36(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. Restrained distances
 C11-C17
 1.51 with sigma of 0.02
 C10A-C9A \\sim C9B-C8B
 with sigma of 0.02
 C17-C12 \\sim C17-C16
 with sigma of 0.02
4. Restrained planarity
 C16, C15, C14, C13, C12, C11, C17
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
N1 \\sim N2B \\sim C7B \\sim C8B \\sim C9B \\sim C10B: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C16 \\sim C13 \\sim C12 \\sim C11 \\sim C17: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C16 \\sim C15 \\sim C14 \\sim C13 \\sim C12 \\sim C11 \\sim C17: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
6. Rigid body (RIGU) restrains
 N1, N2A, C8A, C9A, C10A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, N2B, C7B, C8B, C9B, C10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C15, C14, C13, C12, C11, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: H1AA(0.571) H1AB(0.571) H1BC(0.308) H1BD(0.308) N2A(0.571)
 H2AA(0.381) H2AB(0.381) H2AC(0.381) C8A(0.571) H8AA(0.571) H8AB(0.571)
 C9A(0.571) H9A(0.571) C10A(0.571) H10A(0.571) H10B(0.571) H10C(0.571)
 C11A(0.571) H11A(0.571) H11B(0.571) N2B(0.308) H2BA(0.205) H2BB(0.205)
 H2BC(0.205) C7B(0.308) H7BA(0.308) H7BB(0.308) C8B(0.308) H8B(0.308)
 C9B(0.308) H9BA(0.308) H9BB(0.308) H9BC(0.308) C10B(0.308) H10D(0.308)
 H10E(0.308) C16(0.311) H16(0.311) C15(0.311) H15(0.311) C14(0.311) H14(0.311)
 C13(0.311) H13(0.311) C12(0.311) H12(0.311) C11(0.311) C17(0.311) H17A(0.311)
 H17B(0.311) H17C(0.311)
8.a Ternary CH refined with riding coordinates:
 C9A(H9A), C8B(H8B)
8.b Secondary CH2 refined with riding coordinates:
 N1(H1AA,H1AB), N1(H1BC,H1BD), C8A(H8AA,H8AB), C11A(H11A,H11B), C7B(H7BA,H7BB),
  C10B(H10D,H10E)
8.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C16(H16), C15(H15), C14(H14), C13(H13), C12(H12)
8.d Fitted hexagon refined as free rotating group:
 C16(C15,C14,C13,C12,C11)
8.e Idealised Me refined as rotating group:
 N2A(H2AA,H2AB,H2AC), C10A(H10A,H10B,H10C), N2B(H2BA,H2BB,H2BC), C9B(H9BA,H9BB,
 H9BC), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              94124
_shelx_hkl_checksum              33244
_olex2_submission_special_instructions 'No special instructions were received'