Fine-tuning of the confined space in microporous metal‒organic frameworks for efficient mercury removal
Mon, Marta; Qu, Xiaoni; Ferrando-Soria, Jesús; Pellicer-Carreño, Isaac; Sepúlveda-Escribano, Antonio; Ramos-Fernandez, Enrique V.; Jansen, Johannes C.; Armentano, Donatella; Pardo, Emilio; Journal of Materials Chemistry A 5 (2017) 20120–; doi:10.1039/C7TA06199D

data_7236644
_publ_section_title
;
 Fine-tuning of the confined space in microporous metal--organic
 frameworks for efficient mercury removal
;
_journal_issue                   38
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              20120
_journal_paper_doi               10.1039/C7TA06199D
_journal_volume                  5
_journal_year                    2017
_chemical_formula_sum            'C24 H42 Cu4 N4 O17 S4'
_chemical_formula_weight         1041.01
_space_group_crystal_system      tetragonal
_space_group_IT_number           77
_space_group_name_Hall           'P 4c'
_space_group_name_H-M_alt        'P 42'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-06-23 deposited with the CCDC.
2017-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6593(2)
_cell_length_b                   13.6593(2)
_cell_length_c                   12.0051(4)
_cell_measurement_reflns_used    1684
_cell_measurement_temperature    45(2)
_cell_measurement_theta_max      29.5850
_cell_measurement_theta_min      2.1100
_cell_volume                     2239.87(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CRYSTAL MAKER'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      45(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2930
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9891
_diffrn_measured_fraction_theta_max 0.9484
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67165
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7323
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        24.6602
_diffrn_reflns_theta_max         24.6939
_diffrn_reflns_theta_min         1.4908
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.751
_exptl_absorpt_correction_T_max  0.67867
_exptl_absorpt_correction_T_min  0.67082
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1060
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 1137 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3630
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0682P)^2^+3.5913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_full    0.851
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                2936
_reflns_number_total             3630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta06199d2.cif
_cod_data_source_block           1_45K
_cod_original_cell_volume        2239.88(10)
_cod_database_code               7236644
_oxdiff_exptl_absorpt_empirical_full_min 0.919
_oxdiff_exptl_absorpt_empirical_full_max 1.087
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2013-4
_shelx_res_checksum              94537