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_4126284
_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         'C21.32 H27.96 N3.66 O6 Zn2'
_chemical_formula_sum            'C21.32 H27.96 N3.66 O6 Zn2'
_chemical_formula_weight         562.33
_chemical_name_common            Zn2(dobpdc)(mm-2)1.83
_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             2016-11-23
_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                   21.4759(11)
_cell_length_b                   21.4759(11)
_cell_length_c                   6.8613(4)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.65
_cell_measurement_theta_min      2.388
_cell_volume                     2740.6(3)
_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
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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     0.7749
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       30
_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            47338
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         33.645
_diffrn_reflns_theta_min         2.388
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.692
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1328 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.8963.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_colour_primary    'pale yellow'
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             871
_exptl_crystal_size_max          0.1428
_exptl_crystal_size_mid          0.04641
_exptl_crystal_size_min          0.04641
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.328(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0913P)^2^+0.8608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                4998
_reflns_number_total             5559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b05858_si_004.cif
_cod_data_source_block           rls056s
_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_database_code               4126284
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.794
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.672(19) 0.328(19)
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
 N2A-C11A \\sim N2A-C10A \\sim N2A-C9A \\sim N2B-C9B \\sim N2B-C11B \\sim
N2B-C10B
 with sigma of 0.02
 C9B-C8B \\sim C9A-C8A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim C8B \\sim C8A \\sim C9A \\sim C9B \\sim N2B \\sim N2A \\sim C10B \\sim
C10A \\sim C11B \\sim C11A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Others
 Fixed Sof: H1AA(0.41) H1AB(0.41) H1BC(0.5) H1BD(0.5) N2B(0.41) C8B(0.41)
 H8BA(0.41) H8BB(0.41) C9B(0.41) H9BA(0.41) H9BB(0.41) C10B(0.41) H10A(0.41)
 H10B(0.41) H10C(0.41) C11B(0.41) H11A(0.41) H11B(0.41) H11C(0.41) N2A(0.5)
 C8A(0.5) H8AA(0.5) H8AB(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) C10A(0.5) H10D(0.5)
 H10E(0.5) H10F(0.5) C11A(0.5) H11D(0.25) H11E(0.25) H11F(0.25) H11G(0.25)
 H11H(0.25) H11I(0.25)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1AA,H1AB), N1(H1BC,H1BD), C8B(H8BA,H8BB), C9B(H9BA,H9BB), C8A(H8AA,H8AB),
 C9A(H9AA,H9AB)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6)
6.c Disordered Me refined with riding coordinates:
 C11A(H11D,H11E,H11F,H11G,H11H,H11I)
6.d Idealised Me refined as rotating group:
 C10B(H10A,H10B,H10C), C11B(H11A,H11B,H11C), C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              79374
_shelx_hkl_checksum              65320
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'