#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:58:49 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179029 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/27/4122739.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4122739
loop_
_publ_author_name
'Henkelis, James J.'
'Carruthers, Christopher J.'
'Chambers, Scott E.'
'Clowes, Rob'
'Cooper, Andrew I.'
'Fisher, Julie'
'Hardie, Michaele J.'
_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            'C185 H174 B6 F24 N26 O34 Pd3'
_chemical_formula_weight         4145.56
_chemical_name_systematic
; 
di(tris(2-methyl-isonicotinoyl)-cyclotriguaiacylene}
tri[1,1'-methylenebis(3-(naphthalen-2-ylmethyl)-
imidazol-2-ylidene)]tripalladium(II) tetrafluoroborate 
;
_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                   25.2100(12)
_cell_length_b                   25.2100(12)
_cell_length_c                   20.5293(7)
_cell_measurement_temperature    100(2)
_cell_volume                     11299.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'station I19 Diamond Light Source'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1494
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            95207
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.9593
_exptl_absorpt_correction_T_min  0.9384
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4244
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
Eight nitromethane per formula unit (16 per cell) were
included in the formula in accordance with TGA
;
_refine_diff_density_max         1.422
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.927
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         8523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.927
_refine_ls_R_factor_all          0.1835
_refine_ls_R_factor_gt           0.1417
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3436
_refine_ls_wR_factor_ref         0.3647
_reflns_number_gt                5684
_reflns_number_total             8523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508502u_si_007.cif
_cod_data_source_block           c
_cod_depositor_comments
;Adding full bibliography for 4122738--4122744.cif.

The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Haxagonal' was replaced with
'hexagonal' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               4122739
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd1 Pd 0.95213(3) 0.19803(3) 0.2500 0.1020(4) Uani 1 2 d S .
F1 F 0.7481(10) -0.0296(12) 0.2500 0.219(8) Uiso 0.50 2 d SP 2
O1 O 0.8798(6) 0.4275(5) 0.4950(8) 0.323(9) Uani 1 1 d . .
N1 N 1.0594(3) 0.2026(3) 0.1923(3) 0.1138(16) Uani 1 1 d . .
C1 C 1.0927(4) 0.2381(4) 0.2500 0.109(3) Uani 1 2 d S .
H1A H 1.0948 0.2783 0.2500 0.131 Uiso 1 2 calc SR .
H1B H 1.1350 0.2450 0.2500 0.131 Uiso 1 2 calc SR .
B3 B 1.1322(7) 0.4476(7) 0.2500 0.127(4) Uiso 1 2 d S .
F2 F 0.8238(9) 0.0713(10) 0.2500 0.199(6) Uiso 0.50 2 d SP 1
O2 O 0.8381(3) 0.3099(3) 0.4921(3) 0.1479(19) Uani 1 1 d . .
N2 N 0.9833(3) 0.1428(2) 0.1342(3) 0.1084(15) Uani 1 1 d . .
C2 C 0.9999(3) 0.1801(3) 0.1864(3) 0.1064(18) Uani 1 1 d . .
B2 B 1.0000 0.0000 0.0000 0.115(6) Uiso 1 6 d S .
F3 F 0.8561(6) 0.0096(6) 0.2500 0.179(4) Uiso 0.67 2 d SP .
O3 O 0.7478(3) 0.2470(5) 0.4422(4) 0.204(4) Uani 1 1 d . .
N3 N 0.9055(3) 0.2199(2) 0.3216(2) 0.1029(14) Uani 1 1 d . .
C3 C 1.0831(4) 0.1795(4) 0.1456(4) 0.134(2) Uani 1 1 d . .
H3 H 1.1239 0.1874 0.1413 0.160 Uiso 1 1 calc R .
F9 F 0.7884(5) 0.0134(6) 0.3101(6) 0.179(4) Uiso 0.50 1 d P .
F4 F 1.0000 0.0000 0.0775(7) 0.120(4) Uiso 0.50 3 d SP .
C4 C 1.0350(5) 0.1440(4) 0.1089(4) 0.131(2) Uani 1 1 d . .
H4 H 1.0358 0.1227 0.0710 0.157 Uiso 1 1 calc R .
F5 F 1.0113(4) 0.0557(3) -0.0143(4) 0.115(2) Uiso 0.50 1 d P .
C5 C 0.9233(4) 0.1070(3) 0.1087(4) 0.129(2) Uani 1 1 d . .
H5A H 0.8931 0.0999 0.1433 0.155 Uiso 1 1 calc R .
H5B H 0.9172 0.0667 0.0949 0.155 Uiso 1 1 calc R .
F6 F 1.1963(5) 0.4718(5) 0.2500 0.208(3) Uiso 1 2 d S .
C6 C 0.9113(4) 0.1385(3) 0.0493(4) 0.122(2) Uani 1 1 d . .
F7 F 1.1080(4) 0.3861(4) 0.2500 0.172(3) Uiso 1 2 d S .
C7 C 0.9597(4) 0.1840(4) 0.0111(4) 0.130(2) Uani 1 1 d . .
H7 H 1.0007 0.1968 0.0233 0.156 Uiso 1 1 calc R .
F8 F 1.1149(3) 0.4675(3) 0.3020(4) 0.215(3) Uiso 1 1 d . .
C8 C 0.9501(4) 0.2091(4) -0.0404(5) 0.136(3) Uani 1 1 d . .
H8 H 0.9837 0.2394 -0.0647 0.164 Uiso 1 1 calc R .
C9 C 0.8901(5) 0.1908(4) -0.0590(4) 0.134(3) Uani 1 1 d . .
C10 C 0.8736(7) 0.2133(6) -0.1199(5) 0.170(4) Uani 1 1 d . .
H10 H 0.9058 0.2421 -0.1469 0.204 Uiso 1 1 calc R .
C11 C 0.8198(7) 0.1958(6) -0.1362(6) 0.159(4) Uani 1 1 d . .
H11 H 0.8117 0.2110 -0.1750 0.191 Uiso 1 1 calc R .
C12 C 0.7668(6) 0.1498(5) -0.0938(7) 0.168(4) Uani 1 1 d . .
H12 H 0.7255 0.1358 -0.1060 0.202 Uiso 1 1 calc R .
C13 C 0.7794(5) 0.1300(5) -0.0402(7) 0.172(4) Uani 1 1 d . .
H13 H 0.7466 0.1028 -0.0129 0.206 Uiso 1 1 calc R .
C14 C 0.8386(4) 0.1473(4) -0.0222(5) 0.137(3) Uani 1 1 d . .
C15 C 0.8552(4) 0.1228(3) 0.0340(4) 0.132(3) Uani 1 1 d . .
H15 H 0.8232 0.0937 0.0608 0.158 Uiso 1 1 calc R .
C16 C 0.7277(4) 0.4091(4) 0.6582(4) 0.151(3) Uani 1 1 d . .
H16A H 0.7056 0.3817 0.6952 0.181 Uiso 1 1 calc R .
H16B H 0.7598 0.4490 0.6756 0.181 Uiso 1 1 calc R .
C17 C 0.7358(4) 0.3178(4) 0.6139(4) 0.121(2) Uani 1 1 d . .
C18 C 0.7573(4) 0.3793(5) 0.6131(4) 0.133(3) Uani 1 1 d . .
C19 C 0.8043(5) 0.4165(4) 0.5707(6) 0.183(4) Uani 1 1 d . .
H19 H 0.8174 0.4589 0.5685 0.219 Uiso 1 1 calc R .
C20 C 0.8314(6) 0.3939(6) 0.5331(6) 0.185(5) Uani 1 1 d . .
C21 C 0.8089(5) 0.3320(5) 0.5341(5) 0.139(3) Uani 1 1 d . .
C22 C 0.7631(5) 0.2958(4) 0.5736(4) 0.124(2) Uani 1 1 d . .
H22 H 0.7490 0.2531 0.5737 0.149 Uiso 1 1 calc R .
C23 C 0.8022(6) 0.2707(6) 0.4477(4) 0.158(3) Uani 1 1 d . .
C24 C 0.8397(4) 0.2506(5) 0.4057(4) 0.134(3) Uani 1 1 d . .
C25 C 0.9029(4) 0.2851(4) 0.4022(4) 0.127(2) Uani 1 1 d . .
H25 H 0.9243 0.3194 0.4302 0.152 Uiso 1 1 calc R .
C26 C 0.9354(4) 0.2704(3) 0.3583(4) 0.118(2) Uani 1 1 d . .
C27 C 0.8450(3) 0.1840(4) 0.3273(4) 0.124(2) Uani 1 1 d . .
H27 H 0.8249 0.1469 0.3032 0.149 Uiso 1 1 calc R .
C28 C 0.8111(4) 0.1993(4) 0.3671(4) 0.131(2) Uani 1 1 d . .
H28 H 0.7678 0.1744 0.3681 0.157 Uiso 1 1 calc R .
C29 C 1.0023(4) 0.3084(4) 0.3539(4) 0.131(2) Uani 1 1 d . .
H29A H 1.0176 0.2920 0.3201 0.196 Uiso 1 1 calc R .
H29B H 1.0206 0.3082 0.3959 0.196 Uiso 1 1 calc R .
H29C H 1.0133 0.3505 0.3427 0.196 Uiso 1 1 calc R .
C30 C 0.9106(11) 0.4979(11) 0.5166(15) 0.41(2) Uani 1 1 d . .
H30A H 0.9459 0.5229 0.4885 0.610 Uiso 1 1 calc R .
H30B H 0.9242 0.5021 0.5620 0.610 Uiso 1 1 calc R .
H30C H 0.8806 0.5116 0.5124 0.610 Uiso 1 1 calc R .
B1 B 0.8035(12) 0.0189(13) 0.2500 0.145(7) Uiso 0.67 2 d SP .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 Pd1 C2 82.7(4) 10_556 .
C2 Pd1 N3 176.7(3) 10_556 10_556
C2 Pd1 N3 94.7(2) . 10_556
C2 Pd1 N3 94.7(2) 10_556 .
C2 Pd1 N3 176.7(3) . .
N3 Pd1 N3 87.8(3) 10_556 .
B1 F1 F9 50.2(8) . .
B1 F1 F9 50.2(8) . 10_556
F9 F1 F9 99.0(15) . 10_556
C20 O1 C30 108.9(11) . .
C2 N1 C3 112.8(7) . .
C2 N1 C1 121.2(6) . .
C3 N1 C1 124.9(7) . .
N1 C1 N1 107.5(7) . 10_556
F8 B3 F8 105.5(12) . 10_556
F8 B3 F7 112.5(9) . .
F8 B3 F7 112.5(9) 10_556 .
F8 B3 F6 110.7(8) . .
F8 B3 F6 110.7(8) 10_556 .
F7 B3 F6 104.9(11) . .
B1 F2 F9 46.0(7) . .
B1 F2 F9 46.0(7) . 10_556
F9 F2 F9 88.2(12) . 10_556
C23 O2 C21 114.8(8) . .
C2 N2 C4 108.7(6) . .
C2 N2 C5 126.9(7) . .
C4 N2 C5 124.5(7) . .
N1 C2 N2 105.4(6) . .
N1 C2 Pd1 122.2(5) . .
N2 C2 Pd1 132.2(5) . .
F5 B2 F5 115.2(2) 11_545 9_665
F5 B2 F5 115.2(2) 11_545 7_755
F5 B2 F5 115.2(2) 9_665 7_755
F5 B2 F5 64.8(2) 11_545 .
F5 B2 F5 64.8(2) 9_665 .
F5 B2 F5 179.997(1) 7_755 .
F5 B2 F5 179.998(2) 11_545 5_765
F5 B2 F5 64.8(2) 9_665 5_765
F5 B2 F5 64.8(2) 7_755 5_765
F5 B2 F5 115.2(2) . 5_765
F5 B2 F5 64.8(2) 11_545 3_645
F5 B2 F5 180.0(13) 9_665 3_645
F5 B2 F5 64.8(2) 7_755 3_645
F5 B2 F5 115.2(2) . 3_645
F5 B2 F5 115.2(2) 5_765 3_645
F5 B2 F4 102.8(3) 11_545 7_755
F5 B2 F4 102.8(3) 9_665 7_755
F5 B2 F4 102.8(3) 7_755 7_755
F5 B2 F4 77.2(3) . 7_755
F5 B2 F4 77.2(3) 5_765 7_755
F5 B2 F4 77.2(3) 3_645 7_755
F5 B2 F4 77.2(3) 11_545 .
F5 B2 F4 77.2(3) 9_665 .
F5 B2 F4 77.2(3) 7_755 .
F5 B2 F4 102.8(3) . .
F5 B2 F4 102.8(3) 5_765 .
F5 B2 F4 102.8(3) 3_645 .
F4 B2 F4 180.0 7_755 .
C27 N3 C26 120.3(6) . .
C27 N3 Pd1 118.6(5) . .
C26 N3 Pd1 120.9(5) . .
C4 C3 N1 103.5(8) . .
B1 F9 F1 52.5(13) . .
B1 F9 F2 40.5(12) . .
F1 F9 F2 84.9(10) . .
C3 C4 N2 109.5(8) . .
B2 F5 F5 57.60(12) . 9_665
B2 F5 F5 57.60(12) . 11_545
F5 F5 F5 104.0(7) 9_665 11_545
N2 C5 C6 112.4(6) . .
C15 C6 C7 118.5(9) . .
C15 C6 C5 119.3(8) . .
C7 C6 C5 122.3(8) . .
C8 C7 C6 122.8(9) . .
C7 C8 C9 119.3(9) . .
C8 C9 C14 121.9(9) . .
C8 C9 C10 123.7(10) . .
C14 C9 C10 114.3(10) . .
C11 C10 C9 122.8(13) . .
C10 C11 C12 120.1(12) . .
C13 C12 C11 118.6(10) . .
C12 C13 C14 122.4(13) . .
C13 C14 C9 121.7(11) . .
C13 C14 C15 124.8(11) . .
C9 C14 C15 113.4(8) . .
C6 C15 C14 123.9(8) . .
C17 C16 C18 106.2(5) 3_655 .
C22 C17 C18 117.6(9) . .
C22 C17 C16 119.4(8) . 5_665
C18 C17 C16 123.1(9) . 5_665
C17 C18 C19 119.7(9) . .
C17 C18 C16 121.0(9) . .
C19 C18 C16 119.3(9) . .
C20 C19 C18 121.5(10) . .
O1 C20 C19 124.8(12) . .
O1 C20 C21 117.3(9) . .
C19 C20 C21 118.0(11) . .
C22 C21 C20 120.9(8) . .
C22 C21 O2 123.1(10) . .
C20 C21 O2 116.0(10) . .
C21 C22 C17 122.3(8) . .
O3 C23 O2 128.8(8) . .
O3 C23 C24 121.5(9) . .
O2 C23 C24 109.3(9) . .
C28 C24 C25 117.3(8) . .
C28 C24 C23 120.9(9) . .
C25 C24 C23 121.7(9) . .
C24 C25 C26 120.9(7) . .
N3 C26 C25 119.5(7) . .
N3 C26 C29 120.2(7) . .
C25 C26 C29 120.2(7) . .
N3 C27 C28 121.6(7) . .
C27 C28 C24 120.1(8) . .
F2 B1 F9 93.5(15) . .
F2 B1 F9 93.5(15) . 10_556
F9 B1 F9 150(3) . 10_556
F2 B1 F1 136(3) . .
F9 B1 F1 77.3(14) . .
F9 B1 F1 77.3(14) 10_556 .
F2 B1 F3 105(2) . .
F9 B1 F3 103.1(13) . .
F9 B1 F3 103.1(13) 10_556 .
F1 B1 F3 118(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C2 1.977(7) 10_556
Pd1 C2 1.977(7) .
Pd1 N3 2.120(5) 10_556
Pd1 N3 2.120(5) .
F1 B1 1.32(3) .
F1 F9 1.622(19) .
F1 F9 1.622(19) 10_556
O1 C20 1.334(13) .
O1 C30 1.60(3) .
N1 C2 1.316(8) .
N1 C3 1.402(10) .
N1 C1 1.468(8) .
C1 N1 1.468(8) 10_556
B3 F8 1.340(10) .
B3 F8 1.340(10) 10_556
B3 F7 1.354(16) .
B3 F6 1.414(16) .
F2 B1 1.15(3) .
F2 F9 1.773(19) .
F2 F9 1.773(19) 10_556
O2 C23 1.315(11) .
O2 C21 1.416(9) .
N2 C2 1.346(8) .
N2 C4 1.391(10) .
N2 C5 1.418(9) .
B2 F5 1.319(7) 11_545
B2 F5 1.319(7) 9_665
B2 F5 1.319(7) 7_755
B2 F5 1.319(7) .
B2 F5 1.319(7) 5_765
B2 F5 1.319(7) 3_645
B2 F4 1.590(14) 7_755
B2 F4 1.590(14) .
F3 B1 1.46(3) .
O3 C23 1.198(12) .
N3 C27 1.333(9) .
N3 C26 1.340(8) .
C3 C4 1.324(11) .
F9 B1 1.278(14) .
F5 F5 1.413(9) 9_665
F5 F5 1.413(9) 11_545
C5 C6 1.564(11) .
C6 C15 1.301(11) .
C6 C7 1.421(11) .
C7 C8 1.315(13) .
C8 C9 1.398(12) .
C9 C14 1.427(12) .
C9 C10 1.515(14) .
C10 C11 1.244(14) .
C11 C12 1.530(16) .
C12 C13 1.310(15) .
C13 C14 1.379(13) .
C14 C15 1.466(12) .
C16 C17 1.564(12) 3_655
C16 C18 1.594(11) .
C17 C22 1.359(11) .
C17 C18 1.363(12) .
C17 C16 1.564(12) 5_665
C18 C19 1.388(13) .
C19 C20 1.333(14) .
C20 C21 1.370(14) .
C21 C22 1.331(12) .
C23 C24 1.539(12) .
C24 C28 1.374(11) .
C24 C25 1.384(11) .
C25 C26 1.388(11) .
C26 C29 1.468(10) .
C27 C28 1.370(10) .
B1 F9 1.278(14) 10_556
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.333 0.667 -0.250 1830 473 ' '
2 0.667 0.333 0.250 1830 476 ' '
3 0.000 1.000 0.250 92 10 ' '
4 0.000 0.000 0.750 92 10 ' '
