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_7236646
_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 H34 Cl2 Cu4 Hg N4 O14 S4'
_chemical_formula_weight         1256.44
_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_date             2017-05-11
_audit_creation_method           'XIA2 0.5.277-gc78b72c6-dials-1.5'
_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                   12.9735(2)
_cell_length_b                   12.9735(2)
_cell_length_c                   11.5283(3)
_cell_measurement_reflns_used    12343
_cell_measurement_temperature    45(2)
_cell_measurement_theta_max      33.0684776087
_cell_measurement_theta_min      1.51201120452
_cell_volume                     1940.35(7)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.5.1-gf72becc3-release'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.5.1-gf72becc3-release
pointless (Evans, P., 2006)
XIA2 0.5.277-gc78b72c6-dials-1.5 (Winter, G., 2010)
;
_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                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29039
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.521
_exptl_absorpt_coefficient_mu    5.805
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.988145696935
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.035: AIMLESS, version 0.5.31 : 12/12/16
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.151
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.994
_refine_diff_density_min         -2.431
_refine_diff_density_rms         0.242
_refine_ls_abs_structure_details
;
 Flack x determined using 2097 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.030(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5164
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0799
_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^)+(0.1798P)^2^+5.7459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2319
_refine_ls_wR_factor_ref         0.2370
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4754
_reflns_number_total             5164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta06199d2.cif
_cod_data_source_block           MARMON87_45K
_cod_original_cell_volume        1940.35(8)
_cod_database_code               7236646
_shelxl_version_number           2013-4
_shelx_res_checksum              12231