Direct synthesis of an aliphatic amine functionalized metal-organic framework for efficient CO2 removal and CH4 purification
Huang, Ning-Yu; Mo, Zong-Wen; Li, Lu-Jian; Xu, Wei-Jian; Zhou, Hao-Long; Zhou, Dong-Dong; Liao, Pei-Qin; Zhang, Jie-Peng; Chen, Xiao-Ming; CrystEngComm  (2018) –; doi:10.1039/C8CE00574E

data_7230657
_publ_section_title
;
 Direct synthesis of an aliphatic amine functionalized metal-organic
 framework for efficient CO2 removal and CH4 purification
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE00574E
_journal_year                    2018
_chemical_formula_moiety         '0.11(C432 H351 N27 O108 Zn27)'
_chemical_formula_sum            'C48 H39 N3 O12 Zn3'
_chemical_formula_weight         1045.93
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-12-28 deposited with the CCDC.
2018-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   42.4897(8)
_cell_length_b                   42.4897(8)
_cell_length_c                   10.4000(4)
_cell_measurement_reflns_used    1786
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      40.4
_cell_measurement_theta_min      6.7
_cell_volume                     16260.4(8)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      203
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29635
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.482
_diffrn_reflns_theta_max         67.482
_diffrn_reflns_theta_min         2.079
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.961
_exptl_crystal_description       block
_exptl_crystal_F_000             4806
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6487
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1567P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5024
_reflns_number_total             6487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00574e2.cif
_cod_data_source_block           beta_Zn
_cod_original_cell_volume        16260.4(9)
_cod_database_code               7230657
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C24B-N2
 1.48 with sigma of 0.02
 C21B-C24B
 1.48 with sigma of 0.02
 C24A-C21A
 1.48 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C19A) = Uanis(C18A) = Uanis(C23A) = Uanis(C22A) = Uanis(C21A) =
Uanis(C20A) = Uanis(C24A) = Uanis(C19B) = Uanis(C18B) = Uanis(C23B) =
Uanis(C20B) = Uanis(C21B) = Uanis(C22B) = Uanis(C24B)
4. Others
 Fixed Sof: C17B(0.5) C19B(0.5) H19B(0.5) C18B(0.5) C23B(0.5) H23B(0.5)
 C22B(0.5) H22B(0.5) C21B(0.5) C20B(0.5) H20B(0.5) N2(0.5) H2(0.5) C19A(0.5)
 H19A(0.5) C18A(0.5) C23A(0.5) H23A(0.5) C22A(0.5) H22A(0.5) C21A(0.5)
 C20A(0.5) H20A(0.5) C24B(0.5) H24A(0.5) H24B(0.5) C24A(0.5) H24C(0.5)
 H24D(0.5) C17A(0.5)
5.a Ternary CH refined with riding coordinates:
 N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C24B(H24A,H24B), C24A(H24C,H24D)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C14(H14), C3(H3), C12(H12), C11(H11), C15(H15), C4(H4),
 C19B(H19B), C23B(H23B), C22B(H22B), C20B(H20B), N2(H2), C19A(H19A), C23A(H23A),
  C22A(H22A), C20A(H20A)
5.d Fitted hexagon refined as free rotating group:
 C19B(C18B,C23B,C22B,C21B,C20B), C19A(C18A,C23A,C22A,C21A,C20A)
;
_shelx_fab_checksum              39857
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'