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_4346656
_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         '0.25(C252 H244 Cu12 N12 O68)'
_chemical_formula_sum            'C63 H61 Cu3 N3 O17'
_chemical_formula_weight         1322.76
_chemical_name_systematic        CuCPB2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4973)
;
_cell_angle_alpha                91.275(2)
_cell_angle_beta                 92.433(2)
_cell_angle_gamma                106.100(2)
_cell_formula_units_Z            4
_cell_length_a                   12.6325(4)
_cell_length_b                   17.4726(6)
_cell_length_c                   27.9667(9)
_cell_measurement_reflns_used    9687
_cell_measurement_temperature    100
_cell_measurement_theta_max      50.924
_cell_measurement_theta_min      2.634
_cell_volume                     5921.7(3)
_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      100
_diffrn_measured_fraction_theta_full 0.585
_diffrn_measured_fraction_theta_max 0.986
_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  0.0727
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.585
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            125355
_diffrn_reflns_point_group_measured_fraction_full 0.585
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         50.969
_diffrn_reflns_theta_min         2.634
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.858942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker,200?) was used for absorption correction.
R(int) was 0.0816 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.8589.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2732
_exptl_crystal_preparation       'solvothermal reaction in DEF/water'
_exptl_crystal_recrystallization_method 'solvothermal reaction'
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.674
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1573
_refine_ls_number_reflns         12536
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.1072
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+152.7034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2100
_refine_ls_wR_factor_ref         0.2201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10232
_reflns_number_total             12536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01900_si_005.cif
_cod_data_source_block           cucpb2
_cod_database_code               4346656
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.786
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB = O2W-H2WA = O2W-H2WB
 0.85 with sigma of 0.001
 O3W-H3WA = O3W-H3WB = O4W-H4WA = O4W-H4WB
 0.85 with sigma of 0.001
 H1WA-H1WB = H2WA-H2WB = H3WA-H3WB = H4WA-H4WB
 1.36 with sigma of 0.003
 Cu1-H1WA = Cu1-H1WB
 2.6 with sigma of 0.001
 Cu2-H2WA = Cu2-H2WB
 2.4 with sigma of 0.001
 Cu5-H3WA = Cu5-H3WB
 2.4 with sigma of 0.001
 Cu6-H4WA = Cu6-H4WB
 2.4 with sigma of 0.001
 N6S-C27S
 1.45 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C21S \\sim N5S: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004
C32 \\sim C33: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004
C57 \\sim C59: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004
C63 \\sim C64: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004
C9S \\sim C10S: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004
C24S \\sim C25S: within 1.7A with sigma of 0.002 and sigma for terminal atoms
of 0.004
Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O21)
\\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(O1S) \\sim Ueq, Uanis(N1S) \\sim Ueq, Uanis(N4S) \\sim Ueq, Uanis(N5S)
\\sim Ueq, Uanis(N6S) \\sim Ueq, Uanis(C4S) \\sim Ueq, Uanis(C10S) \\sim Ueq,
Uanis(C23S) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C29)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C31) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C59) \\sim Ueq:
with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C61) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C79) \\sim Ueq:
with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C80) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C92) \\sim Ueq,
Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C6) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C4S(H4SA,H4SB), C7S(H7SA,H7SB), C9S(H9SA,H9SB), C12S(H12A,
 H12B), C14S(H14A,H14B), C17S(H17A,H17B), C19S(H19A,H19B), C22S(H22A,H22B),
 C24S(H24A,H24B), C27S(H27A,H27B), C29S(H29A,H29B)
4.b Me refined with riding coordinates:
 C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C8S(H8SA,H8SB,H8SC), C10S(H10A,H10B,
 H10C), C13S(H13A,H13B,H13C), C15S(H15A,H15B,H15C), C18S(H18A,H18B,H18C),
 C20S(H20A,H20B,H20C), C23S(H23A,H23B,H23C), C25S(H25A,H25B,H25C), C28S(H28A,
 H28B,H28C), C30S(H30A,H30B,H30C)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), 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), C56(H56), C57(H57), C59(H59), C60(H60), C62(H62), C63(H63), C65(H65),
  C66(H66), C68(H68), C69(H69), C71(H71), C72(H72), C74(H74), C75(H75),
 C77(H77), C78(H78), C80(H80), C81(H81), C83(H83), C84(H84), C86(H86), C87(H87),
  C89(H89), C90(H90), C1S(H1S), C6S(H6S), C11S(H11S), C16S(H16S), C21S(H21S),
 C26S(H26S)
;
_olex2_exptl_crystal_mounting_method cryoloop
_olex2_submission_original_sample_id CuCPB2
_olex2_submission_special_instructions 'No special instructions were received'