Secondary amine-functionalised metal‒organic frameworks: direct syntheses versus tandem post-synthetic modifications
Keenan, Luke L.; Hamzah, Harina Amer; Mahon, Mary F.; Warren, Mark R.; Burrows, Andrew D.; CrystEngComm 18 (2016) 5710–; doi:10.1039/C6CE01270A

data_7225726
_publ_section_title
;
 Secondary amine-functionalised metal--organic frameworks: direct
 syntheses versus tandem post-synthetic modifications
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5710
_journal_paper_doi               10.1039/C6CE01270A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.25(C96 N12 O52 Zn16)'
_chemical_formula_sum            'C76.6 H78.2 N3 O13 Zn4'
_chemical_formula_weight         1510.30
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-29 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9940(3)
_cell_length_b                   25.9940(3)
_cell_length_c                   25.9940(3)
_cell_measurement_reflns_used    9423
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.6279
_cell_measurement_theta_min      2.5189
_cell_volume                     17563.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43780
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.565
_diffrn_reflns_theta_min         2.519
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             6262
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
TITL DLK16 in Fm-3m
CELL   25.9940   25.9940   25.9940     90.00     90.00     90.00
SPGR Fm-3m
Q101 0.294 0.206 0.206 !       1.32 eA-3
Q102 0.209 0.326 0.215 !       0.84 eA-3
Q103 0.880 0.207 0.207 !       0.80 eA-3
Q104 0.295 0.245 0.202 !       0.74 eA-3
C105 0.136 0.138 0.152 !       0.67 eA-3
Q106 0.155 0.250 0.250 !       0.58 eA-3
C107 0.347 0.403 0.156 !       0.53 eA-3
Q108 0.721 0.283 0.217 !       0.52 eA-3
;
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         1064
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0550
_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^)+(0.1119P)^2^+60.7871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                748
_reflns_number_total             1064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01270a2.cif
_cod_data_source_block           dlk16_sq
_cod_depositor_comments
'Adding full bibliography for 7225726--7225730.cif.'
_cod_original_cell_volume        17563.8(5)
_cod_original_formula_sum        'C76.60 H78.20 N3 O13 Zn4'
_cod_database_code               7225726
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.867
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
2. Others
 Fixed Sof: N1(0.125)
;
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20