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_4126285
_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         'C20.48 H22.20 N3.24 O9.24 Zn2'
_chemical_formula_sum            'C20.48 H22.2 N3.24 O9.24 Zn2'
_chemical_formula_weight         592.31
_chemical_name_common            Zn2(dobpdc)(m-2-CO2)1.62
_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             2017-01-05
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 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                   21.2594(11)
_cell_length_b                   21.2594(11)
_cell_length_c                   6.7655(4)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.19
_cell_measurement_theta_min      2.41
_cell_volume                     2648.1(2)
_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 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON100 CMOS 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  0.0544
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            53044
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         37.226
_diffrn_reflns_theta_min         2.089
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.758
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1276 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.7914.
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    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             905
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.823
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.497(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         7037
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0558P)^2^+3.4875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6578
_reflns_number_total             7037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05858_si_003.cif
_cod_data_source_block           rls131s
_cod_original_cell_volume        2648.1(3)
_cod_original_formula_sum        'C20.48 H22.20 N3.24 O9.24 Zn2'
_cod_database_code               4126285
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.503(18) 0.497(18)
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)
  groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C9A-C10A = C11B-C10B
 1.54 with sigma of 0.02
 N2A-C10A \\sim N2A-C11A \\sim N2B-C11B
 with sigma of 0.02
 N1B-C9B \\sim N1B-C10B \\sim N1A-C9A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O4A \\sim O5A \\sim N1A \\sim N2A \\sim C8A \\sim C9A \\sim C10A \\sim C11A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N2B \\sim C11B \\sim O5B \\sim C9B \\sim O4B \\sim N1B \\sim C8B \\sim C10B:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O4A, O5A, N1A, N2A, C8A, C9A, C10A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2B, C11B, O5B, C9B, O4B, N1B, C8B, C10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O4A(0.52) O5A(0.52) N1A(0.52) H1A(0.52) N2A(0.52) H2AA(0.52)
 H2AB(0.52) C8A(0.52) C9A(0.52) H9AA(0.52) H9AB(0.52) C10A(0.52) H10A(0.52)
 H10B(0.52) C11A(0.52) H11A(0.52) H11B(0.52) H11C(0.52) O4B(0.29) O5B(0.29)
 N1B(0.29) N2B(0.29) H2BA(0.29) H2BB(0.29) H2BC(0.29) C8B(0.29) C9B(0.29)
 H9BA(0.145) H9BB(0.145) H9BC(0.145) H9BD(0.145) H9BE(0.145) H9BF(0.145)
 C10B(0.29) H10C(0.29) H10D(0.29) C11B(0.29) H11D(0.29) H11E(0.29)
7.a Secondary CH2 refined with riding coordinates:
 N2A(H2AA,H2AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C10B(H10C,H10D), C11B(H11D,
 H11E)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), N1A(H1A)
7.c Disordered Me refined with riding coordinates:
 C9B(H9BA,H9BB,H9BC,H9BD,H9BE,H9BF)
7.d Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), N2B(H2BA,H2BB,H2BC)
;
_shelx_res_checksum              54149
_shelx_hkl_checksum              99856
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'