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_1518256
_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, 7.5(C24 H20 B), 2.25(B F4), 4.25(C2 H3 N), 0.5(C2 H4 N), 11.5(O)'
_chemical_formula_sum         'C453.5 H476.75 B33.75 F9 Fe12 N100.75 O83.5 Pd6'
_chemical_formula_weight         10519.01
_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                109.87(3)
_cell_angle_beta                 111.57(4)
_cell_angle_gamma                90.72(4)
_cell_formula_units_Z            4
_cell_length_a                   37.76(2)
_cell_length_b                   37.914(15)
_cell_length_c                   49.64(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     61382(6)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1885
_diffrn_reflns_av_unetI/netI     0.2789
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            222504
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        17.000
_diffrn_reflns_theta_max         17.200
_diffrn_reflns_theta_min         1.075
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.6993
_exptl_absorpt_correction_T_min  0.5760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       plate
_exptl_crystal_F_000             21635
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN:H2O, 2:1'
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.086
_refine_diff_density_max         3.608
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.394
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5610
_refine_ls_number_reflns         72139
_refine_ls_number_restraints     42737
_refine_ls_restrained_S_all      1.824
_refine_ls_R_factor_all          0.2907
_refine_ls_R_factor_gt           0.1670
_refine_ls_shift/su_max          0.000
_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          0.3795
_refine_ls_wR_factor_ref         0.4645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32996
_reflns_number_total             72139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03046j2.cif
_cod_data_source_block           cage5_BPh4
_cod_depositor_comments
;
Adding full bibliography for 1518252--1518257.cif.

2019-08-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         21038.03
_cod_original_formula_moiety
'2(C264 H312 B24 Fe12 N96 O72 Pd6), 15(C24 H20 B), 4.5(B F4), 8.5(C2 H3 N), (C2 H4 N), 23(O)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        61382(56)
_cod_original_formula_sum
'C907 H953.50 B67.50 F18 Fe24 N201.50 O167 Pd12'
_cod_database_code               1518256
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.957
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_shelxl_version_number           2014/6
_shelx_res_checksum              83403
_shelx_fab_checksum              21588