Programmable self-assembly of water-soluble organo-heterometallic cages [M12M'4L12] using 3-(3,5-dimethyl-1H-pyrazol-4-yl)pentane-2,4-dione (H2L).
Chen, Zi-Man; Cui, Yu; Jiang, Xuan-Feng; Tong, Jin; Yu, Shu-Yan; Chemical communications (Cambridge, England) 53 (2017) 4238–4241; doi:10.1039/c7cc00425g

data_7119863
_publ_section_title
;
 Programmable self-assembly of water-soluble organo-heterometallic cages
 [M12M'4L12] using 3-(3,5-dimethyl-1H-pyrazol-4-yl)pentane-2,4-dione
 (H2L).
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4238
_journal_page_last               4241
_journal_paper_doi               10.1039/c7cc00425g
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety
'C264 H288 Fe4 N48 O24 Pd12, 12(F6 P),14(C2 H3 N)'
_chemical_formula_sum            'C292 H330 F72 Fe4 N62 O24 P12 Pd12'
_chemical_formula_weight         8331.9785
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                68.991(2)
_cell_angle_beta                 73.112(2)
_cell_angle_gamma                64.351(3)
_cell_formula_units_Z            2
_cell_length_a                   25.6021(15)
_cell_length_b                   26.9162(12)
_cell_length_c                   36.6641(13)
_cell_measurement_reflns_used    8712
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.11
_cell_volume                     20985.3(18)
_computing_cell_refinement       HKL2000
_computing_data_collection       marccd
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'mar ccd'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.8001
_diffrn_reflns_av_R_equivalents  0.0129
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            282863
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        28.689
_diffrn_reflns_theta_max         31.260
_diffrn_reflns_theta_min         0.679
_diffrn_source                   'synchroton radiation'
_exptl_absorpt_coefficient_mu    1.039
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8032
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4198
_refine_ls_number_reflns         93208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.05P)^2^+1.22P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                77559
_reflns_number_total             93208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00425g2.cif
_cod_data_source_block           jxf1_sq_sq
_cod_depositor_comments
'Adding full bibliography for 7119861--7119863.cif.'
_cod_database_code               7119863
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.860
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              68733
_shelx_fab_checksum              76142