Synthesis and Selective CO2 Capture Properties of a Series of Hexatopic Linker-Based Metal-Organic Frameworks.
Nguyen, Phuong T. K.; Nguyen, Huong T. D.; Pham, Hung Q.; Kim, Jaheon; Cordova, Kyle E.; Furukawa, Hiroyasu; Inorganic chemistry 54 (2015) 10065–10072; doi:10.1021/acs.inorgchem.5b01900

data_4346654
_publ_section_title
;
 Synthesis and Selective CO2 Capture Properties of a Series of Hexatopic
 Linker-Based Metal-Organic Frameworks.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10065
_journal_page_last               10072
_journal_paper_doi               10.1021/acs.inorgchem.5b01900
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C59 H55 Mg2 N O16'
_chemical_formula_sum            'C59 H55 Mg2 N O16'
_chemical_formula_weight         1082.66
_chemical_name_systematic        MgCPB
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4973)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.876(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8582(6)
_cell_length_b                   28.0640(12)
_cell_length_c                   16.7331(8)
_cell_measurement_reflns_used    2499
_cell_measurement_temperature    298
_cell_measurement_theta_max      42.798
_cell_measurement_theta_min      3.150
_cell_volume                     5528.5(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX 2'
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.384
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0803
_diffrn_reflns_Laue_measured_fraction_full 0.384
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7456
_diffrn_reflns_point_group_measured_fraction_full 0.384
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         43.071
_diffrn_reflns_theta_min         3.091
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.900930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.0321 before and 0.0289 after correction.
The Ratio of minimum to maximum transmission is 0.9009.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_preparation       'Solvothermal reaction in DEF/EtOH/water'
_exptl_crystal_recrystallization_method 'Solvothermal reaction'
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.512
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         3836
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.0977
_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^)+(0.1370P)^2^+50.9802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2409
_refine_ls_wR_factor_ref         0.2722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2590
_reflns_number_total             3836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01900_si_003.cif
_cod_data_source_block           mgcpb
_cod_database_code               4346654
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.905
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H15A,C56,H56A,H56B,C57,H57A,H57B,H57C,C56',H56C,H56D,C57',
  H57D,H57E,H57F} of O15, {H14A,C54,H54A,H54B,C55,H55A,H55B,H55C,C54',H54C,H54D,
  C55',H55D,H55E,H55F} of O14, All C(H,H) groups, All C(H,H,H) groups, All O(H)
  groups
2. Restrained distances
 O14-C54 = O14-C54' = O15-C56 = O15-C56' = O16-C58
 1.45 with sigma of 0.005
 C54-C55 = C54'-C55'
 1.54 with sigma of 0.005
 C56-C57 = C56'-C57'
 1.54 with sigma of 0.005
 C58-C59
 1.54 with sigma of 0.005
 C50-C51 = C52-C53 = C50'-C51' = C52'-C53'
 1.54 with sigma of 0.005
 O14-H14A = O15-H15A = O16-H16
 0.85 with sigma of 0.001
 Mg1-H14A = Mg2-H15A = Mg2-H16
 2.55 with sigma of 0.02
 Mg2-C56 = Mg2-C56'
 3.12 with sigma of 0.02
 N1-C50 = N1-C52 = N1-C50' = N1-C52'
 1.45 with sigma of 0.005
 N1-C49 = N1-C49'
 1.45 with sigma of 0.005
 O13-C49 = O13-C49'
 1.2 with sigma of 0.005
 O3-H3
 0.85 with sigma of 0.001
 O8-H8
 0.85 with sigma of 0.001
 O14-C55 \\sim O14-C55' \\sim O15-C57 \\sim O15-C57' \\sim O16-C59
 with sigma of 0.005
 O14-C54 \\sim O14-C54' \\sim O15-C56 \\sim O15-C56' \\sim O16-C58
 with sigma of 0.005
 C49-C52 \\sim C49'-C52'
 with sigma of 0.005
 N1-C51 \\sim N1-C53 \\sim N1-C51' \\sim N1-C53'
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 1.7A with sigma of 0.003 and sigma for terminal atoms of
0.006
C5 \\sim C6: within 1.7A with sigma of 0.003 and sigma for terminal atoms of
0.006
C15 \\sim C16: within 1.7A with sigma of 0.003 and sigma for terminal atoms of
0.006
C39 \\sim C40: within 1.7A with sigma of 0.003 and sigma for terminal atoms of
0.006
C40 \\sim C48: within 1.7A with sigma of 0.003 and sigma for terminal atoms of
0.006
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C44) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C49(0.5) H49(0.5) C50(0.5) H50A(0.5) H50B(0.5) C51(0.5) H51A(0.5)
 H51B(0.5) H51C(0.5) C52(0.5) H52A(0.5) H52B(0.5) C53(0.5) H53A(0.5) H53B(0.5)
 H53C(0.5) C49'(0.5) H49'(0.5) C50'(0.5) H50C(0.5) H50D(0.5) C51'(0.5)
 H51D(0.5) H51E(0.5) H51F(0.5) C52'(0.5) H52C(0.5) H52D(0.5) C53'(0.5)
 H53D(0.5) H53E(0.5) H53F(0.5) C54(0.5) H54A(0.5) H54B(0.5) C55(0.5) H55A(0.5)
 H55B(0.5) H55C(0.5) C54'(0.5) H54C(0.5) H54D(0.5) C55'(0.5) H55D(0.5)
 H55E(0.5) H55F(0.5) C56(0.5) H56A(0.5) H56B(0.5) C57(0.5) H57A(0.5) H57B(0.5)
 H57C(0.5) C56'(0.5) H56C(0.5) H56D(0.5) C57'(0.5) H57D(0.5) H57E(0.5) H57F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C52(H52A,H52B), C50'(H50C,H50D), C52'(H52C,H52D), C54(H54A,
 H54B), C54'(H54C,H54D), C56(H56A,H56B), C56'(H56C,H56D), C58(H58A,H58B)
5.b Me refined with riding coordinates:
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C51'(H51D,H51E,H51F), C53'(H53D,
 H53E,H53F), C55(H55A,H55B,H55C), C55'(H55D,H55E,H55F), C57(H57A,H57B,H57C),
 C57'(H57D,H57E,H57F), C59(H59A,H59B,H59C)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8A), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15), C17(H17), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30),
  C32(H32), C33(H33), C35(H35), C36(H36), C38(H38), C39(H39), C41(H41),
 C42(H42), C49(H49), C49'(H49')
;
_olex2_exptl_crystal_mounting_method glue
_olex2_submission_original_sample_id MgCPB
_olex2_submission_special_instructions 'No special instructions were received'