Secondary-amine-functionalized isoreticular metal‒organic frameworks for controllable and selective dye capture
Tan, Jing; Zhou, Beibei; Liang, Congcong; Zinky, Hannah; Zhou, Hao-Long; Zhang, Yue-Biao; Materials Chemistry Frontiers 2 (2018) 129–; doi:10.1039/C7QM00414A

data_1553696
_publ_section_title
;
 Secondary-amine-functionalized isoreticular metal--organic frameworks for
 controllable and selective dye capture
;
_journal_issue                   1
_journal_name_full               'Materials Chemistry Frontiers'
_journal_page_first              129
_journal_paper_doi               10.1039/C7QM00414A
_journal_volume                  2
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_moiety         '0.17(C252 H168 Cu12 N60 O48)'
_chemical_formula_sum            'C42 H28 Cu2 N10 O8'
_chemical_formula_weight         927.82
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-05
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-09 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   27.6887(13)
_cell_length_b                   27.6887(13)
_cell_length_c                   27.6887(13)
_cell_measurement_reflns_used    9227
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      42.824
_cell_measurement_theta_min      3.904
_cell_volume                     21227.9(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68406
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        42.909
_diffrn_reflns_theta_max         42.909
_diffrn_reflns_theta_min         2.257
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.7484
_exptl_absorpt_correction_T_min  0.5677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1502 before and 0.0781 after correction. The Ratio of minimum to maximum transmission is 0.7586. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.435
_exptl_crystal_description       cube
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.093
_refine_diff_density_rms         0.012
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2572
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0200
_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^)+(0.0241P)^2^+2.6021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    1.001
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2330
_reflns_number_total             2572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qm00414a2.cif
_cod_data_source_block           ST-14
_cod_original_cell_volume        21228(3)
_cod_database_code               1553696
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.929
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(4)
 0.50(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained distances
 C11-C11_$6
 1.48 with sigma of 0.01
 N1-C10 \\sim N1-C10_$1 \\sim C10-C10_$1 \\sim C11-C9 \\sim C11-C9_$1 \\sim
C9_$1-C9
 with sigma of 0.02
 N1-C13 \\sim N1-C13_$1 \\sim C13-C13_$1 \\sim C12-C11 \\sim C11-C12_$1 \\sim
C12-C12_$1
 with sigma of 0.02
 N3_$4-N3 \\sim N3_$4-N3_$5 \\sim N3_$5-N3 \\sim C8-C8_$5 \\sim C8_$4-C8 \\sim
C8_$4-C8_$5
 with sigma of 0.02
 O2-C1 \\sim O1-C1
 with sigma of 0.02
 N1-C13 \\sim C13-C13_$1 \\sim C13_$1-N1 \\sim C12-C11 \\sim C11-C12_$1 \\sim
C12_$1-C12
 with sigma of 0.02
 N1-C12 \\sim N1-C12_$1 \\sim C13_$1-C12_$1 \\sim C13_$1-C11 \\sim C13-C11
\\sim C13-C12
 with sigma of 0.02
 N3_$4-C8 \\sim N3-C8 \\sim N3-C8_$5 \\sim N3_$5-C8_$5 \\sim N3_$5-C8_$4 \\sim
N3_$4-C8_$4
 with sigma of 0.02
 N3_$4-C8 \\sim N3_$4-C8_$4 \\sim N3_$5-C8_$4 \\sim N3_$5-C8_$5 \\sim N3-C8_$5
\\sim N3-C8
 with sigma of 0.02
 N1-C12 \\sim C13-C12 \\sim C13-C11 \\sim C13_$1-C11 \\sim C13_$1-C12_$1 \\sim
N1-C12_$1
 with sigma of 0.02
 N1-C9 \\sim C9-C10 \\sim C11-C10 \\sim C11-C10_$1 \\sim C9_$1-C10_$1 \\sim
N1-C9_$1
 with sigma of 0.02
4. Restrained planarity
 N1, C12, C12_$1, C13, C13_$1, C11
 with sigma of 0.1
 N1, C9_$1, C9, C10_$1, C10, C11
 with sigma of 0.1
 N2_$1, N2_$3, N2_$2, N3_$1, N3_$2, N3_$3, C8_$1, C8_$2, C8_$3
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(O1)
Uanis(C9) = Uanis(C10) = Uanis(C13) = Uanis(C12)
Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C7) = Uanis(C6) = Uanis(C5) =
Uanis(C1)
6. Rigid body (RIGU) restrains
 N1, C12, C9, C10, C13, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=1-FVAR(1)
 Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=FVAR(1)
8.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C6(H6), C4(H4), C3(H3), C9(H9), C12(H12), C10(H10), C13(H13)
8.b Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3)
;
_olex2_submission_special_instructions 'No special instructions were received'