Large, heterometallic coordination cages based on ditopic metallo-ligands with 3-pyridyl donor groups
Wise, Matthew D.; Holstein, Julian J.; Pattison, Philip; Besnard, Celine; Solari, Euro; Scopelliti, Rosario; Bricogne, Gerard; Severin, Kay; Chem. Sci. 6 (2015) 1004–; doi:10.1039/C4SC03046J

data_1518255
_publ_section_title
;
 Large, heterometallic coordination cages based on ditopic metallo-ligands
 with 3-pyridyl donor groups
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1004
_journal_paper_doi               10.1039/C4SC03046J
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety
'C264 H312 B24 Fe12 N96 O72 Pd6, 14(C7 H8), 10(N O3), 12(C2 H3 N), 4(O)'
_chemical_formula_sum            'C193 H230 B12 Fe6 N59 O53 Pd3'
_chemical_formula_weight         5008.37
_chemical_properties_physical    Air-sensitive
_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-2014/6
_cell_angle_alpha                111.25(3)
_cell_angle_beta                 101.84(3)
_cell_angle_gamma                110.60(3)
_cell_formula_units_Z            2
_cell_length_a                   24.070(5)
_cell_length_b                   25.090(5)
_cell_length_c                   26.260(5)
_cell_measurement_reflns_used    877170
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.755
_cell_measurement_theta_min      0.905
_cell_volume                     12790(8)
_computing_cell_refinement
'XDS (Kabsch 2013) and autoPROC (Vonrhein 2013)'
_computing_data_collection       'Pylatus software (Dyadkin 2013)'
_computing_data_reduction
'XDS (Kabsch 2013) and autoPROC (Vonrhein 2013)'
_computing_molecular_graphics    'shelXle (Huebschle, 2014)'
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type
'Pilatus 2M, Dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.715
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            877170
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.077
_diffrn_reflns_theta_max         28.755
_diffrn_reflns_theta_min         0.905
_diffrn_source
'Swiss Norwegian beamline @ ESRF, Grenoble, France'
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5158
_exptl_crystal_recrystallization_method
'by layering a solution of complex 5 in MeCN onto toluene'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.523
_refine_diff_density_min         -1.249
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3304
_refine_ls_number_reflns         60736
_refine_ls_number_restraints     9072
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+26.2909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                57514
_reflns_number_total             60736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03046j2.cif
_cod_data_source_block           cage5
_cod_depositor_comments
'Adding full bibliography for 1518252--1518257.cif.'
_cod_original_cell_volume        12790(6)
_cod_database_code               1518255
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.970
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_shelxl_version_number           2014/6
_shelx_res_checksum              8593
_shelx_fab_checksum              43238