Water Enables Efficient CO<sub>2</sub> Capture from Natural Gas Flue Emissions in an Oxidation-Resistant Diamine-Appended Metal-Organic Framework.
Siegelman, Rebecca L.; Milner, Phillip J.; Forse, Alexander C.; Lee, Jung-Hoon; Colwell, Kristen A.; Neaton, Jeffrey B.; Reimer, Jeffrey A.; Weston, Simon C.; Long, Jeffrey R.; Journal of the American Chemical Society 141 (2019) 13171–13186; doi:10.1021/jacs.9b05567

data_4127847
_publ_section_title
;
 Water Enables Efficient CO<sub>2</sub> Capture from Natural Gas Flue
 Emissions in an Oxidation-Resistant Diamine-Appended Metal-Organic
 Framework.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13171
_journal_page_last               13186
_journal_paper_doi               10.1021/jacs.9b05567
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C30.09 H36.96 N3.52 O6 Zn2'
_chemical_formula_sum            'C30.09 H36.96 N3.52 O6 Zn2'
_chemical_formula_weight         674.73
_chemical_name_common            Zn2(dobpdc)(2-ampd)1.76(C7H8)0.79
_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 space'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-01-08
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.4691(5)
_cell_length_b                   21.4691(5)
_cell_length_c                   6.8480(2)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.386
_cell_measurement_theta_min      2.247
_cell_volume                     2733.52(12)
_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  0.0743
_diffrn_reflns_av_unetI/netI     0.0342
_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            53834
_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         30.396
_diffrn_reflns_theta_min         1.945
_diffrn_source
;
Advanced Light Source, station 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.451
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1138 before and 0.0686 after correction.
The Ratio of minimum to maximum transmission is 0.9313.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1062
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         5134
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0482P)^2^+1.8283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4441
_reflns_number_total             5134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05567_si_002.cif
_cod_data_source_block           rls208s
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2733.52(15)
_cod_database_code               4127847
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.903
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(2)
 0.49(2)
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,H)
  groups, All N(H,H,H,H) groups
3. Restrained distances
 C18-C17
 1.5 with sigma of 0.02
 N1-C8B \\sim N1-C8A
 with sigma of 0.02
 C9A-C8A \\sim C9B-C8B
 with sigma of 0.02
 C9B-C13B \\sim C13B-C12B \\sim C12B-C11B \\sim C11B-C10B \\sim C9A-C13A \\sim
C13A-C12A \\sim C12A-
 C11A \\sim C11A-C10A
 with sigma of 0.02
 N2A-C9A \\sim N2B-C9B \\sim N2A-C10A \\sim N2B-C10B
 with sigma of 0.02
 C17-C16 \\sim C16-C15 \\sim C15-C14
 with sigma of 0.02
 C17-C15 \\sim C16-C14 \\sim C15-C15_$1 \\sim C14-C16_$1 \\sim C15_$1-C17
 with sigma of 0.02
 C17-C14 \\sim C16-C15_$1 \\sim C15-C16_$1
 with sigma of 0.02
4. Restrained planarity
 C14, C15, C15_$1, C16, C16_$1, C17, C18
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 N1, N2A, C8A, C9A, C10A, C11A, C12A, C13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, N2B, C8B, C9B, C10B, C11B, C12B, C13B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: H1AA(0.589) H1AB(0.589) H1BC(0.291) H1BD(0.291) N2A(0.589)
 H2AA(0.2945) H2AB(0.2945) C8A(0.589) H8AA(0.589) H8AB(0.589) C9A(0.589)
 H9A(0.589) C10A(0.589) H10A(0.589) H10B(0.589) C11A(0.589) H11A(0.589)
 H11B(0.589) C12A(0.589) H12B(0.589) H12A(0.589) C13A(0.589) H13A(0.589)
 H13B(0.589) N2B(0.291) H2BA(0.1455) H2BB(0.1455) C8B(0.291) H8BA(0.291)
 H8BB(0.291) C9B(0.291) H9B(0.291) C10B(0.291) H10C(0.291) H10D(0.291)
 C11B(0.291) H11C(0.291) H11D(0.291) C12B(0.291) H12C(0.291) H12D(0.291)
 C13B(0.291) H13D(0.291) H13C(0.291) C14(0.3935) H14(0.3935) C15(0.787)
 H15(0.787) C16(0.787) H16(0.787) C17(0.3935) C18(0.3935) H18A(0.3935)
 H18B(0.3935) H18C(0.3935) H18D(0.3935) H18E(0.3935) H18F(0.3935)
 Fixed U11: Zn1(0.015797) O1(0.025837) O2(0.019573) O3(0.030037) N1(0.02917)
 C1(0.016027) C2(0.022853) C3(0.02388) C4(0.026343) C5(0.026907) C6(0.02656)
 C7(0.02142)
 Fixed U12: Zn1(0.001057) O1(0.000514) O2(0.002794) O3(0.00295) N1(-0.014613)
 C1(-0.000947) C2(-0.001882) C3(0.000277) C4(-0.000167) C5(0.000762) C6(-
 0.000231) C7(-0.001051)
 Fixed U13: Zn1(0.000046) O1(-0.002587) O2(-0.000058) O3(0.000069)
 N1(0.004215) C1(0.001432) C2(0.002229) C3(-0.000069) C4(0.000797) C5(0.002823)
 C6(-0.000502) C7(0.000762)
 Fixed U22: Zn1(0.01467) O1(0.01163) O2(0.01364) O3(0.01495) N1(0.04711)
 C1(0.0168) C2(0.01752) C3(0.01396) C4(0.01879) C5(0.01796) C6(0.02188)
 C7(0.01354)
 Fixed U23: Zn1(-0.00058) O1(0.00054) O2(0.00024) O3(-0.00194) N1(0.00678)
 C1(0.00262) C2(-0.00076) C3(0.00056) C4(0.00104) C5(-0.00209) C6(-0.00253) C7(-
 0.00086)
 Fixed U33: Zn1(0.008) O1(0.0103) O2(0.0085) O3(0.0104) N1(0.02679)
 C1(0.00987) C2(0.00574) C3(0.01115) C4(0.00985) C5(0.01198) C6(0.01047)
 C7(0.00554)
8.a Ternary CH refined with riding coordinates:
 C9A(H9A), C9B(H9B)
8.b Secondary CH2 refined with riding coordinates:
 N1(H1AA,H1AB), N1(H1BC,H1BD), N2A(H2AA,H2AB), C8A(H8AA,H8AB), C10A(H10A,H10B),
  C11A(H11A,H11B), C12A(H12B,H12A), C13A(H13A,H13B), N2B(H2BA,H2BB), C8B(H8BA,
 H8BB), C10B(H10C,H10D), C11B(H11C,H11D), C12B(H12C,H12D), C13B(H13D,H13C)
8.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16)
8.d Disordered Me refined with riding coordinates:
 C18(H18A,H18B,H18C,H18D,H18E,H18F)
;
_shelx_res_checksum              17254
_shelx_hkl_checksum              4573
_olex2_submission_special_instructions 'No special instructions were received'