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_4126288
_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         '(C23.89 H32.37 N3.30 O6.80 Zn2), 0.8(H2O)'
_chemical_formula_sum            'C23.89 H33.97 N3.3 O6.8 Zn2'
_chemical_formula_weight         606.88
_chemical_name_common            Zn2(dobpdc)(ee-2)1.65
_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             2016-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3368 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.6620(6)
_cell_length_b                   21.6620(6)
_cell_length_c                   6.8262(2)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.968
_cell_measurement_theta_min      2.706
_cell_volume                     2774.00(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX II'
_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
_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 PHOTON100 CMOS diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8856
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            37787
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        32.097
_diffrn_reflns_theta_max         37.968
_diffrn_reflns_theta_min         2.343
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1349 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.9025.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_modifier   pale
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       prism
_exptl_crystal_F_000             953
_exptl_crystal_size_max          0.043
_exptl_crystal_size_mid          0.0071
_exptl_crystal_size_min          0.0071
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.468(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5217
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0472P)^2^+1.2480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4476
_reflns_number_total             5217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05858_si_009.cif
_cod_data_source_block           rls009s
_cod_original_cell_volume        2774.00(17)
_cod_original_formula_sum        'C23.89 H33.97 N3.30 O6.80 Zn2'
_cod_database_code               4126288
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.532(15) 0.468(15)
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,H,
  H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2B-C9B = N2B-C10B = N2B-C12B = N2C-C9A = N2C-C10C = N2C-C12C = N2A-C10A =
 N2A-C12A = N2A-C9A
 1.47 with sigma of 0.02
 C11B-C10B = C10C-C11C = C12B-C13B = C12C-C13C = C12A-C13A = C10A-C11A
 1.58 with sigma of 0.02
 C9B-C10B \\sim C9B-C12B \\sim C12B-C10B
 with sigma of 0.02
 N2B-C11B \\sim N2B-C13B
 with sigma of 0.02
 C9A-C12C \\sim C9A-C10C \\sim C12C-C10C
 with sigma of 0.02
 N2C-C13C \\sim N2C-C11C
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim N2B \\sim C8B \\sim C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B
\\sim N2C \\sim C10C \\sim C11C \\sim C12C \\sim C13C \\sim N2A \\sim C10A
\\sim C11A \\sim C12A \\sim C13A \\sim C8A \\sim C9A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 N2B, C8B, C9B, C10B, C11B, C12B, C13B, N2C, C10C, C11C, C12C, C13C, N2A, C10A,
  C11A, C12A, C13A, C8A, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N2C)=Sof(C10C)=Sof(H10C)=Sof(H10D)=Sof(C11C)=Sof(H11G)=Sof(H11H)=
 Sof(H11I)=Sof(H11J)=Sof(H11K)=Sof(H11L)=Sof(C12C)=Sof(H12C)=Sof(H12D)=
 Sof(C13C)=Sof(H13G)=Sof(H13H)=Sof(H13I)=Sof(H13J)=Sof(H13K)=Sof(H13L)=0.45*
 FVAR(2)
 Sof(N2A)=Sof(C10A)=Sof(H10E)=Sof(H10F)=Sof(C11A)=Sof(H11M)=Sof(H11N)=
 Sof(H11O)=Sof(C12A)=Sof(H12E)=Sof(H12F)=Sof(C13A)=Sof(H13M)=Sof(H13N)=
 Sof(H13O)=Sof(H13P)=Sof(H13Q)=Sof(H13R)=0.55*FVAR(2)
 Sof(H1BC)=Sof(H1BD)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=FVAR(1)
 Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(H13A)=
 Sof(H13B)=Sof(H13C)=Sof(H13D)=Sof(H13E)=Sof(H13F)=0.5*FVAR(3)
 Sof(H1AA)=Sof(H1AB)=Sof(N2B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=
 Sof(H9BB)=Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(C11B)=Sof(C12B)=Sof(H12A)=
 Sof(H12B)=Sof(C13B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 N1(H1BC,H1BD), N1(H1AA,H1AB), C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10A,H10B),
  C12B(H12A,H12B), C10C(H10C,H10D), C12C(H12C,H12D), C10A(H10E,H10F), C12A(H12E,
 H12F), C8A(H8AA,H8AB)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
7.c Disordered Me refined with riding coordinates:
 C11B(H11A,H11B,H11C,H11D,H11E,H11F), C13B(H13A,H13B,H13C,H13D,H13E,H13F),
 C11C(H11G,H11H,H11I,H11J,H11K,H11L), C13C(H13G,H13H,H13I,H13J,H13K,H13L),
 C13A(H13M,H13N,H13O,H13P,H13Q,H13R)
7.d Idealised Me refined as rotating group:
 C11A(H11M,H11N,H11O)
;
_shelx_res_checksum              4285
_shelx_hkl_checksum              92243
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'