Controlling Cooperative CO2 Adsorption in Diamine-Appended Mg2(dobpdc) Metal-Organic Frameworks.
Siegelman, Rebecca L.; McDonald, Thomas M.; Gonzalez, Miguel I.; Martell, Jeffrey; Milner, Phillip J.; Mason, Jarad A.; Berger, Adam H.; Bhown, Abhoyjit S.; Long, Jeffrey R.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b05858

data_4126287
_publ_section_title
;
 Controlling Cooperative CO2 Adsorption in Diamine-Appended Mg2(dobpdc)
 Metal-Organic Frameworks.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b05858
_journal_year                    2017
_chemical_formula_moiety         'C21.56 H26.16 N2.52 O6 Zn2'
_chemical_formula_sum            'C21.56 H26.16 N2.52 O6 Zn2'
_chemical_formula_weight         547.38
_chemical_name_common            Zn2(dobpdc)(e-2-e)1.26
_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             2016-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3353 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.7573(8)
_cell_length_b                   21.7573(8)
_cell_length_c                   6.9089(3)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.070
_cell_measurement_theta_min      2.935
_cell_volume                     2832.37(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      100.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 with PHOTON100 CMOS detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7293
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            40119
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         27.125
_diffrn_reflns_theta_min         2.218
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1355 before and 0.1035 after correction.
The Ratio of minimum to maximum transmission is 0.6263.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    'pale yellow'
_exptl_crystal_density_diffrn    0.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             865
_exptl_crystal_size_max          0.12495
_exptl_crystal_size_mid          0.05355
_exptl_crystal_size_min          0.05355
_refine_diff_density_max         1.705
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3873
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0836P)^2^+2.5648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3737
_reflns_number_total             3873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05858_si_007.cif
_cod_data_source_block           rls041s
_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        2832.4(2)
_cod_database_code               4126287
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.846
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(3) 0.49(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,H)
  groups
3. Restrained distances
 C8A-C9A \\sim C10B-C11B \\sim C12B-C13B \\sim C12A-C13A \\sim C11A-C10A \\sim
C9B-C8B
 with sigma of 0.02
 N2B-C11B \\sim N2B-C12B \\sim N2A-C12A \\sim N2A-C11A \\sim N1-C10A \\sim
N1-C8B \\sim N1-C9A \\sim N1-C10B
 with sigma of 0.02
 C11A-C12A \\sim C11B-C12B
 with sigma of 0.02
 N2A-C13A \\sim N2B-C13B
 with sigma of 0.02
 N1-C11B \\sim N1-C11A
 with sigma of 0.02
 C10B-N2B \\sim C10A-N2A
 with sigma of 0.02
 N1-C8A \\sim N1-C9B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim C8B \\sim C11B \\sim N2B \\sim C12B \\sim C13B \\sim C10A \\sim C11A
\\sim C9B \\sim N2A \\sim C12A \\sim C8A \\sim C10B \\sim C13A \\sim C9A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9A) = Uanis(C10B)
5. Rigid body (RIGU) restrains
 N1, C8B, C11B, N2B, C12B, C13B, C9B, C10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C10A, C11A, N2A, C12A, C8A, C13A, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H2BA)=Sof(H2BB)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(H9BD)=Sof(H9BE)=
 Sof(H9BF)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(H13D)=Sof(H13E)=Sof(H13F)=0.5*
 FVAR(2)
 Sof(H1B)=Sof(N2B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(C10B)=Sof(H10C)=
 Sof(H10D)=Sof(C11B)=Sof(H11A)=Sof(H11B)=Sof(C12B)=Sof(H12A)=Sof(H12B)=
 Sof(C13B)=FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(H8AD)=Sof(H8AE)=
 Sof(H8AF)=Sof(H13G)=Sof(H13H)=Sof(H13I)=Sof(H13J)=Sof(H13K)=Sof(H13L)=0.5*
 FVAR(3)
 Sof(H1A)=Sof(N2A)=Sof(C8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=
 Sof(H10B)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=
 Sof(C13A)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 N1(H1B), N1(H1A)
7.b Secondary CH2 refined with riding coordinates:
 N2A(H2AA,H2AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C11A(H11C,H11D), C12A(H12C,
 H12D), N2B(H2BA,H2BB), C8B(H8BA,H8BB), C10B(H10C,H10D), C11B(H11A,H11B),
 C12B(H12A,H12B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
7.d Disordered Me refined with riding coordinates:
 C8A(H8AA,H8AB,H8AC,H8AD,H8AE,H8AF), C13A(H13G,H13H,H13I,H13J,H13K,H13L),
 C9B(H9BA,H9BB,H9BC,H9BD,H9BE,H9BF), C13B(H13A,H13B,H13C,H13D,H13E,H13F)
;
_shelx_res_checksum              33681
_shelx_hkl_checksum              55818
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'