Self-Assembly of Catalytically Active Supramolecular Coordination Compounds within Metal-Organic Frameworks.
Adam, Rosa; Mon, Marta; Greco, Rossella; Kalinke, Lucas H. G.; Vidal-Moya, Alejandro; Fernandez, Antonio; Winpenny, Richard E. P.; Doménech-Carbó, Antonio; Leyva-Pérez, Antonio; Armentano, Donatella; Pardo, Emilio; Ferrando-Soria, Jesús; Journal of the American Chemical Society 141 (2019) 10350–10360; doi:10.1021/jacs.9b03914

data_4128037
_publ_section_title
;
 Self-Assembly of Catalytically Active Supramolecular Coordination
 Compounds within Metal-Organic Frameworks.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10350
_journal_page_last               10360
_journal_paper_doi               10.1021/jacs.9b03914
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C101 H174 Au2 Cl3 Cu6 N20 Ni4 O77.5 Pd2 S'
_chemical_formula_weight         4269.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           123
_space_group_name_Hall           '-P 4 2'
_space_group_name_H-M_alt        'P 4/m m m'
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-16
_audit_creation_method           'XIA2 0.5.542-g41349194-dials-1.9'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.725(2)
_cell_length_b                   35.725(2)
_cell_length_c                   15.2666(8)
_cell_measurement_reflns_used    26353
_cell_measurement_temperature    30(2)
_cell_measurement_theta_max      33.9117683767
_cell_measurement_theta_min      0.550453324127
_cell_volume                     19484.4(18)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.9.1-g449277ff-release'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.9.1-g449277ff-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.542-g41349194-dials-1.9 (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      30(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'data_PILATUS_2M_S_N_24_0107_Diamond'
_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  0.1736
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            244768
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.552
_exptl_absorpt_coefficient_mu    2.506
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.980870699954
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.052: AIMLESS, version 0.6.2 : 15/01/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       prism
_exptl_crystal_F_000             8572
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.896
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         10377
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      2.021
_refine_ls_R_factor_all          0.4234
_refine_ls_R_factor_gt           0.3098
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.6579
_refine_ls_wR_factor_ref         0.6865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3377
_reflns_number_total             10377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03914_si_004.cif
_cod_data_source_block           MARMON138B_SQn
_cod_original_cell_volume        19485(2)
_cod_original_formula_sum        'C101 H174 Au2 Cl3 Cu6 N20 Ni4 O77.50 Pd2 S'
_cod_database_code               4128037
_shelxl_version_number           2013-4
_shelx_res_checksum              86973
_shelx_hkl_checksum              68544