#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:58:49 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179029 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/27/4122738.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_4122738
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            'C171 H138 B6 F24 I2 N18 O18 Pd3'
_chemical_formula_weight         3826.85
_chemical_name_systematic
; 
di(tris(isonicotinoyl)-cyclotriguaiacylene}
tri[1,1'-methylenebis(3-(naphthalen-2-ylmethyl)-
imidazol-2-ylidene)]tripalladium(II) tetrafluoroborate 
iodine 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                   24.7255(18)
_cell_length_b                   24.7255(18)
_cell_length_c                   20.3293(11)
_cell_measurement_temperature    110(2)
_cell_volume                     10763.2(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Atlas'
_diffrn_measurement_method       'ω 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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16846
_diffrn_reflns_theta_full        44.98
_diffrn_reflns_theta_max         44.98
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    4.892
_exptl_absorpt_correction_T_max  0.5274
_exptl_absorpt_correction_T_min  0.3743
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3848
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.687
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         3022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.687
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.1292
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3670
_refine_ls_wR_factor_ref         0.3991
_reflns_number_gt                2181
_reflns_number_total             3022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja508502u_si_006.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_sg_symbol_H-M      P6(3)/m
_cod_database_code               4122738
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
Pd1 Pd 0.01643(8) 0.23740(8) 0.7500 0.0584(11) Uani 1 2 d S
F1 F 0.0000 0.0000 0.5746(13) 0.068(9) Uani 0.50 3 d SP
O1 O 0.1105(8) 0.5546(7) 0.5068(10) 0.140(6) Uani 1 1 d .
N1 N -0.0034(7) 0.1519(7) 0.8658(7) 0.062(4) Uani 1 1 d .
C1 C -0.1219(10) 0.1218(11) 0.7500 0.059(6) Uani 1 2 d S
H1A H -0.1285 0.1582 0.7500 0.071 Uiso 1 2 calc SR
H1B H -0.1633 0.0832 0.7500 0.071 Uiso 1 2 calc SR
B1 B 0.0000 0.0000 0.5000 0.069(17) Uani 1 6 d S
F2 F -0.0184(9) 0.0414(9) 0.4820(8) 0.066(5) Uani 0.50 1 d P
O2 O 0.1585(7) 0.4769(7) 0.5181(7) 0.090(4) Uani 1 1 d .
N2 N -0.0872(7) 0.1235(7) 0.8068(7) 0.062(4) Uani 1 1 d .
C2 C -0.0258(10) 0.1683(8) 0.8146(8) 0.060(5) Uani 1 1 d .
B2 B -0.1171(15) 0.3136(15) 0.7500 0.037(9) Uiso 0.67 2 d SP
F3 F -0.1002(7) 0.3465(8) 0.6951(9) 0.108(5) Uiso 0.67 1 d P
O3 O 0.0641(7) 0.4263(6) 0.4746(8) 0.102(4) Uani 1 1 d .
N3 N 0.0510(9) 0.3065(6) 0.6751(7) 0.064(4) Uani 1 1 d .
C3 C -0.1044(9) 0.0780(8) 0.8555(9) 0.065(5) Uani 1 1 d .
H3 H -0.1442 0.0419 0.8614 0.078 Uiso 1 1 calc R
B3 B 0.1828(9) 0.2356(9) 0.7500 0.021(5) Uiso 1 2 d S
F4 F -0.0994(8) 0.2662(9) 0.7500 0.071(5) Uiso 0.67 2 d SP
C4 C -0.0530(12) 0.0958(10) 0.8921(10) 0.081(6) Uani 1 1 d .
H4 H -0.0503 0.0742 0.9296 0.097 Uiso 1 1 calc R
F5 F -0.1829(12) 0.2796(12) 0.7500 0.121(8) Uiso 0.67 2 d SP
C5 C 0.0587(9) 0.1808(9) 0.8866(9) 0.073(5) Uani 1 1 d .
H5A H 0.0862 0.2060 0.8500 0.087 Uiso 1 1 calc R
H5B H 0.0694 0.1484 0.8978 0.087 Uiso 1 1 calc R
F6 F 0.2184(8) 0.2453(8) 0.6996(10) 0.195(7) Uiso 1 1 d .
C6 C 0.0716(10) 0.2241(9) 0.9478(11) 0.082(6) Uani 1 1 d .
F7 F 0.1635(13) 0.2693(13) 0.7500 0.204(10) Uiso 1 2 d S
C7 C 0.1358(11) 0.2678(10) 0.9628(10) 0.090(6) Uani 1 1 d .
H7 H 0.1687 0.2718 0.9353 0.108 Uiso 1 1 calc R
F8 F 0.1398(14) 0.1721(14) 0.7500 0.212(11) Uiso 1 2 d S
C8 C 0.1482(11) 0.3046(9) 1.0204(13) 0.085(6) Uani 1 1 d .
C9 C 0.2148(12) 0.3469(12) 1.0388(13) 0.111(8) Uani 1 1 d .
H9 H 0.2479 0.3501 1.0123 0.133 Uiso 1 1 calc R
C10 C 0.2255(13) 0.3790(10) 1.0922(16) 0.109(8) Uani 1 1 d .
H10 H 0.2673 0.4033 1.1073 0.131 Uiso 1 1 calc R
C11 C 0.1774(15) 0.3791(10) 1.1286(12) 0.102(7) Uani 1 1 d .
H11 H 0.1891 0.4068 1.1649 0.122 Uiso 1 1 calc R
C12 C 0.1149(15) 0.3422(12) 1.1158(13) 0.120(9) Uani 1 1 d .
H12 H 0.0833 0.3427 1.1421 0.144 Uiso 1 1 calc R
C13 C 0.1009(13) 0.3009(10) 1.0562(11) 0.083(6) Uani 1 1 d .
C14 C 0.0399(12) 0.2640(13) 1.0396(14) 0.108(8) Uani 1 1 d .
H14 H 0.0074 0.2645 1.0640 0.130 Uiso 1 1 calc R
C15 C 0.0269(10) 0.2247(10) 0.9839(12) 0.079(6) Uani 1 1 d .
H15 H -0.0155 0.1977 0.9718 0.095 Uiso 1 1 calc R
C16 C 0.2728(8) 0.6851(9) 0.3472(8) 0.077(5) Uani 1 1 d .
H16A H 0.2415 0.6959 0.3314 0.093 Uiso 1 1 calc R
H16B H 0.2932 0.6789 0.3083 0.093 Uiso 1 1 calc R
C17 C 0.2407(9) 0.6255(8) 0.3870(9) 0.067(5) Uani 1 1 d .
C18 C 0.2607(7) 0.5831(9) 0.3895(8) 0.057(4) Uani 1 1 d .
C19 C 0.2301(9) 0.5329(9) 0.4318(11) 0.068(5) Uani 1 1 d .
H19 H 0.2432 0.5027 0.4327 0.081 Uiso 1 1 calc R
C20 C 0.1829(10) 0.5242(9) 0.4717(10) 0.073(5) Uani 1 1 d .
C21 C 0.1610(11) 0.5686(11) 0.4657(11) 0.097(7) Uani 1 1 d .
C22 C 0.1910(10) 0.6175(8) 0.4253(12) 0.086(6) Uani 1 1 d .
H22 H 0.1777 0.6475 0.4229 0.103 Uiso 1 1 calc R
C23 C 0.1005(12) 0.4331(11) 0.5180(13) 0.095(8) Uani 1 1 d .
C24 C 0.0800(12) 0.3874(9) 0.5761(10) 0.085(6) Uani 1 1 d .
C25 C 0.1288(10) 0.3864(8) 0.6109(12) 0.098(7) Uani 1 1 d .
H25 H 0.1715 0.4134 0.6005 0.117 Uiso 1 1 calc R
C26 C 0.1091(11) 0.3416(9) 0.6630(9) 0.077(5) Uani 1 1 d .
H26 H 0.1393 0.3380 0.6886 0.092 Uiso 1 1 calc R
C27 C 0.0072(11) 0.3118(9) 0.6418(10) 0.082(6) Uani 1 1 d .
H27 H -0.0349 0.2872 0.6558 0.098 Uiso 1 1 calc R
C28 C 0.0190(10) 0.3499(10) 0.5895(12) 0.089(6) Uani 1 1 d .
H28 H -0.0132 0.3502 0.5643 0.107 Uiso 1 1 calc R
C29 C 0.0836(14) 0.5944(15) 0.493(2) 0.224(19) Uani 1 1 d .
H29A H 0.0477 0.5826 0.5220 0.337 Uiso 1 1 calc R
H29B H 0.0701 0.5892 0.4471 0.337 Uiso 1 1 calc R
H29C H 0.1151 0.6382 0.5010 0.337 Uiso 1 1 calc R
I1 I 0.0367(5) 0.0673(5) 0.7500 0.322(5) Uani 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 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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(10) 10_557 .
C2 Pd1 N3 92.6(6) 10_557 .
C2 Pd1 N3 173.1(8) . .
C2 Pd1 N3 173.1(8) 10_557 10_557
C2 Pd1 N3 92.6(6) . 10_557
N3 Pd1 N3 91.6(7) . 10_557
B1 F1 F2 48.7(9) . 9_556
B1 F1 F2 48.7(9) . 11_556
F2 F1 F2 81.2(14) 9_556 11_556
B1 F1 F2 48.7(9) . 7_556
F2 F1 F2 81.2(14) 9_556 7_556
F2 F1 F2 81.2(14) 11_556 7_556
C21 O1 C29 111.7(19) . .
C2 N1 C5 126.7(17) . .
C2 N1 C4 107.8(15) . .
C5 N1 C4 125.3(17) . .
N2 C1 N2 108.1(17) . 10_557
F2 B1 F2 179.997(5) 9_556 3
F2 B1 F2 113.1(6) 9_556 11_556
F2 B1 F2 66.9(6) 3 11_556
F2 B1 F2 66.9(6) 9_556 .
F2 B1 F2 113.1(6) 3 .
F2 B1 F2 66.9(6) 11_556 .
F2 B1 F2 113.1(6) 9_556 7_556
F2 B1 F2 66.9(6) 3 7_556
F2 B1 F2 113.1(6) 11_556 7_556
F2 B1 F2 179.998(5) . 7_556
F2 B1 F2 66.9(6) 9_556 5
F2 B1 F2 113.1(6) 3 5
F2 B1 F2 179.997(4) 11_556 5
F2 B1 F2 113.1(6) . 5
F2 B1 F2 66.9(6) 7_556 5
F2 B1 F1 105.6(7) 9_556 7_556
F2 B1 F1 74.4(7) 3 7_556
F2 B1 F1 105.6(7) 11_556 7_556
F2 B1 F1 74.4(7) . 7_556
F2 B1 F1 105.6(7) 7_556 7_556
F2 B1 F1 74.4(7) 5 7_556
F2 B1 F1 74.4(7) 9_556 .
F2 B1 F1 105.6(7) 3 .
F2 B1 F1 74.4(7) 11_556 .
F2 B1 F1 105.6(7) . .
F2 B1 F1 74.4(7) 7_556 .
F2 B1 F1 105.6(7) 5 .
F1 B1 F1 179.999(1) 7_556 .
B1 F2 F2 56.5(3) . 11_556
B1 F2 F2 56.5(3) . 9_556
F2 F2 F2 98.3(15) 11_556 9_556
B1 F2 F1 56.9(9) . 7_556
F2 F2 F1 89.6(9) 11_556 7_556
F2 F2 F1 89.6(9) 9_556 7_556
C23 O2 C20 122.6(17) . .
C2 N2 C3 109.7(14) . .
C2 N2 C1 121.6(16) . .
C3 N2 C1 128.0(16) . .
N1 C2 N2 107.7(14) . .
N1 C2 Pd1 131.2(16) . .
N2 C2 Pd1 120.8(13) . .
F3 B2 F3 116(3) . 10_557
F3 B2 F5 106.4(19) . .
F3 B2 F5 106.4(19) 10_557 .
F3 B2 F4 111.7(18) . .
F3 B2 F4 111.7(18) 10_557 .
F5 B2 F4 104(2) . .
C26 N3 C27 121.6(16) . .
C26 N3 Pd1 123.4(14) . .
C27 N3 Pd1 115.0(14) . .
C4 C3 N2 105.9(16) . .
F7 B3 F6 111.0(16) . 10_557
F7 B3 F6 111.0(16) . .
F6 B3 F6 105(2) 10_557 .
F7 B3 F8 117(2) . .
F6 B3 F8 105.9(15) 10_557 .
F6 B3 F8 105.9(15) . .
C3 C4 N1 108.9(16) . .
N1 C5 C6 112.8(15) . .
C15 C6 C7 119(2) . .
C15 C6 C5 123.8(19) . .
C7 C6 C5 117(2) . .
C8 C7 C6 117(2) . .
C13 C8 C7 120(2) . .
C13 C8 C9 122(2) . .
C7 C8 C9 118(3) . .
C10 C9 C8 117(3) . .
C9 C10 C11 122(3) . .
C12 C11 C10 125(2) . .
C11 C12 C13 114(3) . .
C8 C13 C14 123(2) . .
C8 C13 C12 119(2) . .
C14 C13 C12 117(3) . .
C13 C14 C15 117(2) . .
C6 C15 C14 123(2) . .
C17 C16 C18 110.4(13) . 5_565
C18 C17 C22 120.3(16) . .
C18 C17 C16 123.6(19) . .
C22 C17 C16 116.0(18) . .
C17 C18 C19 117.9(16) . .
C17 C18 C16 123.7(18) . 3_665
C19 C18 C16 118.3(17) . 3_665
C20 C19 C18 123.8(16) . .
C19 C20 O2 121.4(19) . .
C19 C20 C21 116.8(18) . .
O2 C20 C21 122(2) . .
C22 C21 O1 128(2) . .
C22 C21 C20 119.2(19) . .
O1 C21 C20 113(2) . .
C21 C22 C17 121.7(17) . .
O3 C23 O2 124(2) . .
O3 C23 C24 121(2) . .
O2 C23 C24 116(2) . .
C28 C24 C25 124.0(19) . .
C28 C24 C23 121(2) . .
C25 C24 C23 115(2) . .
C24 C25 C26 115.0(19) . .
N3 C26 C25 120.2(18) . .
N3 C27 C28 124(2) . .
C27 C28 C24 114.6(19) . .
I1 I1 I1 59.999(1) 8_557 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C2 1.987(17) 10_557
Pd1 C2 1.987(17) .
Pd1 N3 2.122(14) .
Pd1 N3 2.122(14) 10_557
F1 B1 1.52(3) .
F1 F2 1.74(2) 9_556
F1 F2 1.74(2) 11_556
F1 F2 1.74(2) 7_556
O1 C21 1.40(2) .
O1 C29 1.47(3) .
N1 C2 1.333(19) .
N1 C5 1.40(2) .
N1 C4 1.42(2) .
C1 N2 1.427(17) .
C1 N2 1.427(17) 10_557
B1 F2 1.361(18) 9_556
B1 F2 1.361(18) 3
B1 F2 1.361(18) 11_556
B1 F2 1.361(18) .
B1 F2 1.361(18) 7_556
B1 F2 1.361(18) 5
B1 F1 1.52(3) 7_556
F2 F2 1.50(2) 11_556
F2 F2 1.50(2) 9_556
F2 F1 1.74(2) 7_556
O2 C23 1.29(2) .
O2 C20 1.39(2) .
N2 C2 1.37(2) .
N2 C3 1.395(19) .
B2 F3 1.32(2) .
B2 F3 1.32(2) 10_557
B2 F5 1.41(4) .
B2 F4 1.44(4) .
O3 C23 1.21(2) .
N3 C26 1.28(2) .
N3 C27 1.34(2) .
C3 C4 1.34(2) .
B3 F7 1.15(3) .
B3 F6 1.29(2) 10_557
B3 F6 1.29(2) .
B3 F8 1.39(3) .
C5 C6 1.57(3) .
C6 C15 1.33(3) .
C6 C7 1.44(3) .
C7 C8 1.42(3) .
C8 C13 1.34(3) .
C8 C9 1.49(3) .
C9 C10 1.29(3) .
C10 C11 1.40(3) .
C11 C12 1.37(3) .
C12 C13 1.51(3) .
C13 C14 1.36(3) .
C14 C15 1.42(3) .
C16 C17 1.51(2) .
C16 C18 1.55(2) 5_565
C17 C18 1.37(2) .
C17 C22 1.38(2) .
C18 C19 1.38(2) .
C18 C16 1.55(2) 3_665
C19 C20 1.35(2) .
C20 C21 1.45(3) .
C21 C22 1.34(3) .
C23 C24 1.53(3) .
C24 C28 1.35(3) .
C24 C25 1.41(3) .
C25 C26 1.43(3) .
C27 C28 1.35(2) .
I1 I1 2.50(2) 8_557
I1 I1 2.50(2) 3
