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_4126286
_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         'C27 H38 N4 O8 Zn2'
_chemical_formula_sum            'C27 H38 N4 O8 Zn2'
_chemical_formula_weight         677.38
_chemical_name_common            Zn2(dobpdc)(e-2-e-CO2)(e-2-e)
_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 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                   21.6857(8)
_cell_length_b                   21.6857(8)
_cell_length_c                   6.8891(3)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    195
_cell_measurement_theta_max      25.491
_cell_measurement_theta_min      2.365
_cell_volume                     2805.69(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      195
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            28756
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.517
_diffrn_reflns_theta_max         25.517
_diffrn_reflns_theta_min         2.365
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1496 before and 0.0789 after correction.
The Ratio of minimum to maximum transmission is 0.7655.
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    1.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.37(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2706
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0602P)^2^+11.4113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1628
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2572
_reflns_number_total             2706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05858_si_012.cif
_cod_data_source_block           gcell079s
_cod_original_cell_volume        2805.7(2)
_cod_database_code               4126286
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.891
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.63(5) 0.37(5)
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
 O4-C8 \\sim O5-C8
 with sigma of 0.02
 N2-C10 \\sim N2-C12
 with sigma of 0.02
 N3-C13 \\sim N3-C12
 with sigma of 0.02
 C14-C13 \\sim C10-C9
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim N2 \\sim N3 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12
\\sim C13 \\sim C14: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
O4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O4, O5, N2, N3, C8, C9, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O5(0.5) C8(0.5) N2(0.5) N3(0.5) H3A(0.5) H3B(0.5) C9(0.5) H9A(0.5)
 H9B(0.5) C10(0.5) H10A(0.25) H10B(0.25) H10C(0.25) H10D(0.25) H10E(0.25)
 H10F(0.25) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5) C13(0.5)
 H13A(0.5) H13B(0.5) C14(0.5) H14A(0.25) H14B(0.25) H14C(0.25) H14D(0.25)
 H14E(0.25) H14F(0.25)
7.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
7.c Disordered Me refined with riding coordinates:
 C10(H10A,H10B,H10C,H10D,H10E,H10F), C14(H14A,H14B,H14C,H14D,H14E,H14F)
;
_shelx_res_checksum              31108
_shelx_hkl_checksum              52855
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'