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_4346653
_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         'C57 H47 Cu3 N3 O16'
_chemical_formula_sum            'C57 H47 Cu3 N3 O16'
_chemical_formula_weight         1220.59
_chemical_name_systematic        CuCPB1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.540(3)
_cell_length_b                   16.778(4)
_cell_length_c                   28.468(8)
_cell_measurement_reflns_used    4553
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.949
_cell_measurement_theta_min      3.058
_cell_volume                     5512(2)
_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 0.234
_diffrn_measured_fraction_theta_max 0.992
_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  0.0910
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.234
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12150
_diffrn_reflns_point_group_measured_fraction_full 0.220
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         34.039
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.914951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker,2003) was used for absorption correction.
R(int) was 0.1048 before and 0.0965 after correction.
The Ratio of minimum to maximum transmission is 0.9150.
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    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             2500
_exptl_crystal_preparation       'solvothermal reaction in DMF/water'
_exptl_crystal_recrystallization_method 'solvothermal reaction'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details
;
 Flack x determined using 707 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.48(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         2194
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      4.478
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.1289
_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^)+(0.1069P)^2^+379.6972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2992
_refine_ls_wR_factor_ref         0.3090
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.202
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                1947
_reflns_number_total             2194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01900_si_004.cif
_cod_data_source_block           cucpb1
_cod_original_cell_volume        5512(3)
_cod_database_code               4346653
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.814
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.001
 H1WA-H1WB
 1.36 with sigma of 0.003
 Cu2-H1WA = Cu2-H1WB
 2.31 with sigma of 0.005
 N1-C49 = N1-C50 = N1-C51
 1.45 with sigma of 0.002
 N2-C52 = N2-C53 = N2-C54
 1.45 with sigma of 0.002
 N3-C55 = N3-C56 = N3-C57
 1.45 with sigma of 0.002
3. Restrained planarity
 C16, C44, O3, O4
 with sigma of 0.1
 C40, C48, O11, O12
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Cu1 \\sim Cu2 \\sim Cu3: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(Cu1) \\sim Ueq, Uanis(Cu2) \\sim Ueq, Uanis(Cu3) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(Cu1) = Uanis(Cu3)
Uiso(C21) = Uiso(C22)
Uiso(C30) = Uiso(C31)
Uiso(C33) = Uiso(C34)
Uiso(O1) = Uiso(O2)
Uiso(C50) = Uiso(C53)
Uiso(C51) = Uiso(C54)
Uiso(C50) = Uiso(C56)
Uiso(C51) = Uiso(C57)
Uiso(N1) = Uiso(N2)
Uiso(C11) = Uiso(C15)
Uiso(C12) = Uiso(C14)
Uiso(C11) = Uiso(C23)
Uiso(C12) = Uiso(C24)
Uiso(C11) = Uiso(C39)
Uiso(C12) = Uiso(C38)
Uiso(C6) = Uiso(C8)
Uiso(C6) = Uiso(C9)
Uiso(C34) = Uiso(C48)
Uiso(C34) = Uiso(C43)
Uiso(C34) = Uiso(C44)
5. Same fragment restrains
{C43, O1, O2, C43, O1, O2, C43, O1, O2, C43, O1, O2, C43, O1, O2} sigma for
1-2: 0.02, 1-3: 0.04
as
{C44, O3, O4, C45, O5, O6, C46, O7, O8, C47, O9, O10, C48, O11, O12}
{O13, N1, C49, C50, C51, O13, N1, C49, C50, C51} sigma for 1-2: 0.02, 1-3: 0.04
as
{O14, N2, C52, C53, C54, O15, N3, C55, C56, C57}
6. Others
 Uiso(O3)=Uiso(O4)=Uiso(O5)=Uiso(O6)=Uiso(O7)=Uiso(O8)=Uiso(O9)=Uiso(O10)=
 Uiso(O11)=Uiso(O12)=FVAR(1)
 Fixed Uiso: C1(0.03) C2(0.03) C3(0.03) C4(0.03) C5(0.03) C6(0.03) C8(0.03)
 C9(0.03)
7.a Free rotating group:
 C1(C2,C3,C4,C5,C6,C7,C8,C9,C10,C11,C12,C13,C14,C15,C16,C17,C18,C19,C20,C21,
 C22,C23,C24,C25,C26,C27,C28,C29,C30,C31,C32,C33,C34,C35,C36,C37,C38,C39,C40,
 C41,C42,C43,O1,O2,C44,O3,O4,C45,O5,O6,C46,O7,O8,C47,O9,O10,C48,O11,O12,O13,N1,
 C49,C50,C51,O14,N2,C52,C53,C54,O15,N3,C55,C56,C57,O1W,H1WA,H1WB)
7.b 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), C49(H49), C52(H52), C55(H55)
7.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;
_olex2_exptl_crystal_mounting_method cryoloop
_olex2_submission_original_sample_id CuCPB1
_olex2_submission_special_instructions 'No special instructions were received'