Metallo-cryptophanes decorated with bis-N-heterocyclic carbene ligands: self-assembly and guest uptake into a nonporous crystalline lattice.
Henkelis, James J.; Carruthers, Christopher J.; Chambers, Scott E.; Clowes, Rob; Cooper, Andrew I.; Fisher, Julie; Hardie, Michaele J.; Journal of the American Chemical Society 136 (2014) 14393–14396; doi:10.1021/ja508502u

data_4122741
_publ_section_title
;
 Metallo-cryptophanes decorated with bis-N-heterocyclic carbene ligands:
 self-assembly and guest uptake into a nonporous crystalline lattice.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14393
_journal_page_last               14396
_journal_paper_doi               10.1021/ja508502u
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C191 H186 B6 F24 N26 O34 Pd3'
_chemical_formula_weight         4229.72
_chemical_name_systematic
; 
di(tris(isonicotinoyl)-tris(propyl)-cyclotricatechylene}
tri[1,1'-methylenebis(3-(naphthalen-2-ylmethyl)-
imidazol-2-ylidene)]tripalladium(II) tetrafluoroborate 
nitromethane clathrate
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   24.6118(19)
_cell_length_b                   24.6118(19)
_cell_length_c                   20.272(3)
_cell_measurement_temperature    100(2)
_cell_volume                     10634(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10244
_diffrn_reflns_theta_full        45.00
_diffrn_reflns_theta_max         45.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    2.820
_exptl_absorpt_correction_T_max  0.7284
_exptl_absorpt_correction_T_min  0.5510
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4340
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
Thermogravimetric analysis indicates that there are an additional
eight molecules of nitromethane present in the unit cell that were
not located and whose contributions to diffraction were removed by
SQUEEZE. These have been included in the molecular formula and 
resultant parameters. 
;
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         2988
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0960
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2723
_refine_ls_wR_factor_ref         0.2935
_reflns_number_gt                2172
_reflns_number_total             2988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508502u_si_002.cif
_cod_data_source_block           c:
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4122738--4122744.cif.
;
_cod_original_cell_volume        10634.4(18)
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               4122741