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_1518254
_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
'2(C264 H312 B24 Fe12 N96 O72 Pd6), 11(B F4), 3(C4 H10 O)'
_chemical_formula_sum            'C270 H327 B29.5 F22 Fe12 N96 O73.5 Pd6'
_chemical_formula_weight         8138.75
_space_group_crystal_system      cubic
_space_group_IT_number           209
_space_group_name_Hall           'F 4 2 3'
_space_group_name_H-M_alt        'F 4 3 2'
_symmetry_space_group_name_Hall  'F 4 2 3'
_symmetry_space_group_name_H-M   'F 4 3 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   77.18120(10)
_cell_length_b                   77.18120(10)
_cell_length_c                   77.18120(10)
_cell_measurement_reflns_used    795832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0699
_cell_measurement_theta_min      1.4534
_cell_volume                     459763.6(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       'Pylatus software, SNBL@ESRF (Dyadkin 2013)'
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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
;
Palatinus L., Chapuis G. (2007): Superflip - a computer program for
the solution of crystal structures by charge flipping in
arbitrary dimensions. J. Appl. Cryst. 40, 786-790
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       83
_diffrn_reflns_limit_h_min       -90
_diffrn_reflns_limit_k_max       85
_diffrn_reflns_limit_k_min       -90
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_number            795832
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.077
_diffrn_reflns_theta_max         25.076
_diffrn_reflns_theta_min         1.570
_diffrn_source
'Swiss Norwegian beamline @ ESRF, Grenoble, France'
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    0.941
_exptl_crystal_description       pyramidal
_exptl_crystal_F_000             132496
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_refine_diff_density_max         3.178
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.300
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1526
_refine_ls_number_reflns         32544
_refine_ls_number_restraints     4154
_refine_ls_restrained_S_all      1.300
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0810
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2584
_refine_ls_wR_factor_ref         0.2646
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                31295
_reflns_number_total             32544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03046j2.cif
_cod_data_source_block           cage3
_cod_depositor_comments
'Adding full bibliography for 1518252--1518257.cif.'
_cod_original_cell_volume        459763.6(18)
_cod_original_formula_sum        'C270 H327 B29.50 F22 Fe12 N96 O73.50 Pd6'
_cod_database_code               1518254
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.958
_computing_refinement_gui        'shelXle (Huebschle, 2014)'