#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:54:05 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180280 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/66/7116637.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_7116637
loop_
_publ_author_name
'Nem Singh'
'Jae-Ho Jo'
'Young Ho Song'
'Hyunuk Kim'
'Dongwook Kim'
'Myoung Soo Lah'
'Ki-Whan Chi'
_publ_section_title
;
 Coordination-driven self-assembly of an iridium-cornered prismatic cage
 and encapsulation of three heteroguests in its large cavity
;
_journal_name_full               Chem.Commun.
_journal_page_first              4492
_journal_paper_doi               10.1039/C4cc09494H
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C44 H46 Cl2 Ir2 N4, 2(C H2 Cl2)'
_chemical_formula_sum            'C46 H50 Cl6 Ir2 N4'
_chemical_formula_weight         1256.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-26 deposited with the CCDC.
2015-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                100.26(3)
_cell_angle_beta                 102.15(3)
_cell_angle_gamma                103.55(3)
_cell_formula_units_Z            1
_cell_length_a                   7.9910(16)
_cell_length_b                   9.776(2)
_cell_length_c                   15.449(3)
_cell_measurement_reflns_used    21535
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.27
_cell_volume                     1113.7(5)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Diamond 3'
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXTL-XL
_computing_structure_solution    SHELXTL-XS
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7504
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    6.367
_exptl_absorpt_correction_T_max  0.5685
_exptl_absorpt_correction_T_min  0.4485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.213
_refine_diff_density_min         -2.413
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0317
_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/[σ²(Fo²)+(0.0654P)²+2.9039P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                3820
_reflns_number_total             3838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc09494h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1113.7(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7116637
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ir1 Ir -0.027114(18) 0.535941(15) 0.287166(10) 0.01665(11) Uani 1 1 d U
Cl1 Cl -0.24992(15) 0.47696(12) 0.36862(9) 0.0250(2) Uani 1 1 d U
N1 N -0.2101(5) 0.4018(4) 0.1698(3) 0.0195(7) Uani 1 1 d U
N2 N 0.0442(5) 0.3488(4) 0.3003(3) 0.0192(7) Uani 1 1 d U
C1 C -0.3532(6) 0.4338(5) 0.1245(4) 0.0227(10) Uani 1 1 d .
H1 H -0.4043 0.5046 0.1498 0.027 Uiso 1 1 calc R
C2 C -0.4174(6) 0.3483(6) 0.0344(4) 0.0249(10) Uani 1 1 d .
H2 H -0.5178 0.3496 -0.0107 0.030 Uiso 1 1 calc R
C3 C -0.3040(7) 0.2615(6) 0.0248(4) 0.0224(10) Uani 1 1 d .
H3 H -0.3101 0.1938 -0.0289 0.027 Uiso 1 1 calc R
C4 C -0.1775(6) 0.2930(5) 0.1104(4) 0.0195(9) Uani 1 1 d .
C5 C 0.1355(7) 0.3261(5) 0.3771(3) 0.0232(9) Uani 1 1 d U
H5 H 0.1546 0.3841 0.4365 0.028 Uiso 1 1 calc R
C6 C 0.1991(7) 0.2047(6) 0.3578(4) 0.0267(10) Uani 1 1 d U
H6 H 0.2667 0.1669 0.4010 0.032 Uiso 1 1 calc R
C7 C 0.1453(7) 0.1509(5) 0.2649(4) 0.0242(9) Uani 1 1 d U
H7 H 0.1690 0.0692 0.2318 0.029 Uiso 1 1 calc R
C8 C 0.0474(6) 0.2406(5) 0.2278(3) 0.0185(9) Uani 1 1 d U
C9 C -0.0523(6) 0.2180(5) 0.1376(3) 0.0194(9) Uani 1 1 d U
C10 C -0.0276(6) 0.1047(5) 0.0674(3) 0.0178(8) Uani 1 1 d U
C11 C 0.1418(6) 0.1186(5) 0.0511(3) 0.0203(9) Uani 1 1 d U
H11 H 0.2393 0.1992 0.0860 0.024 Uiso 1 1 calc R
C12 C 0.1677(6) 0.0155(5) -0.0157(3) 0.0191(8) Uani 1 1 d U
H12 H 0.2827 0.0272 -0.0261 0.023 Uiso 1 1 calc R
C13 C 0.2070(6) 0.6553(5) 0.2591(4) 0.0219(8) Uani 1 1 d U
C14 C 0.2333(6) 0.6881(5) 0.3575(4) 0.0229(8) Uani 1 1 d U
C15 C 0.0982(7) 0.7512(5) 0.3774(4) 0.0255(8) Uani 1 1 d U
C16 C -0.0109(7) 0.7611(5) 0.2925(4) 0.0264(9) Uani 1 1 d U
C17 C 0.0605(7) 0.7069(6) 0.2208(4) 0.0251(8) Uani 1 1 d U
C18 C -0.1615(8) 0.8290(7) 0.2858(6) 0.0459(17) Uani 1 1 d .
H18A H -0.1133 0.9348 0.3021 0.069 Uiso 1 1 calc R
H18B H -0.2316 0.7994 0.3277 0.069 Uiso 1 1 calc R
H18C H -0.2381 0.7973 0.2233 0.069 Uiso 1 1 calc R
C19 C -0.0055(8) 0.7010(8) 0.1230(4) 0.0405(15) Uani 1 1 d .
H19A H -0.1342 0.6892 0.1080 0.061 Uiso 1 1 calc R
H19B H 0.0185 0.6188 0.0862 0.061 Uiso 1 1 calc R
H19C H 0.0557 0.7912 0.1098 0.061 Uiso 1 1 calc R
C20 C 0.3271(7) 0.5960(6) 0.2097(4) 0.0318(12) Uani 1 1 d .
H20A H 0.2573 0.5380 0.1487 0.048 Uiso 1 1 calc R
H20B H 0.3814 0.5349 0.2439 0.048 Uiso 1 1 calc R
H20C H 0.4211 0.6763 0.2043 0.048 Uiso 1 1 calc R
C21 C 0.3818(8) 0.6659(7) 0.4253(4) 0.0354(14) Uani 1 1 d .
H21A H 0.4855 0.7514 0.4419 0.053 Uiso 1 1 calc R
H21B H 0.4143 0.5804 0.3985 0.053 Uiso 1 1 calc R
H21C H 0.3431 0.6512 0.4799 0.053 Uiso 1 1 calc R
C22 C 0.0725(9) 0.8022(7) 0.4691(5) 0.0413(15) Uani 1 1 d .
H22A H 0.1131 0.7431 0.5095 0.062 Uiso 1 1 calc R
H22B H -0.0542 0.7931 0.4636 0.062 Uiso 1 1 calc R
H22C H 0.1419 0.9039 0.4944 0.062 Uiso 1 1 calc R
Cl1C Cl 0.5239(2) 0.02613(19) 0.17555(11) 0.0435(4) Uani 1 1 d .
Cl2C Cl 0.5133(2) -0.00192(16) 0.35822(11) 0.0384(3) Uani 1 1 d .
C1C C 0.6022(8) 0.1121(6) 0.2925(4) 0.0362(13) Uani 1 1 d .
H1C1 H 0.5674 0.2030 0.3037 0.043 Uiso 1 1 calc R
H1C2 H 0.7341 0.1371 0.3111 0.043 Uiso 1 1 calc R
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 '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
N1 Ir1 N2 83.50(16) . .
N1 Ir1 C13 111.95(18) . .
N2 Ir1 C13 99.41(18) . .
N1 Ir1 C16 111.37(19) . .
N2 Ir1 C16 161.6(2) . .
C13 Ir1 C16 65.54(19) . .
N1 Ir1 C17 94.07(19) . .
N2 Ir1 C17 133.53(19) . .
C13 Ir1 C17 39.04(19) . .
C16 Ir1 C17 38.5(2) . .
N1 Ir1 C14 151.24(18) . .
N2 Ir1 C14 96.88(18) . .
C13 Ir1 C14 39.45(19) . .
C16 Ir1 C14 64.8(2) . .
C17 Ir1 C14 64.85(19) . .
N1 Ir1 C15 149.97(19) . .
N2 Ir1 C15 126.43(19) . .
C13 Ir1 C15 65.28(19) . .
C16 Ir1 C15 38.9(2) . .
C17 Ir1 C15 64.5(2) . .
C14 Ir1 C15 38.10(19) . .
N1 Ir1 Cl1 88.28(12) . .
N2 Ir1 Cl1 90.42(12) . .
C13 Ir1 Cl1 158.27(15) . .
C16 Ir1 Cl1 100.49(15) . .
C17 Ir1 Cl1 136.01(16) . .
C14 Ir1 Cl1 120.44(14) . .
C15 Ir1 Cl1 93.29(14) . .
C1 N1 C4 107.3(4) . .
C1 N1 Ir1 124.4(3) . .
C4 N1 Ir1 125.2(3) . .
C5 N2 C8 107.0(4) . .
C5 N2 Ir1 125.9(3) . .
C8 N2 Ir1 125.3(3) . .
N1 C1 C2 110.9(4) . .
C3 C2 C1 106.1(4) . .
C2 C3 C4 107.1(5) . .
N1 C4 C9 123.5(4) . .
N1 C4 C3 108.5(4) . .
C9 C4 C3 127.6(5) . .
N2 C5 C6 110.8(5) . .
C7 C6 C5 107.2(5) . .
C6 C7 C8 107.1(5) . .
C9 C8 N2 123.6(4) . .
C9 C8 C7 127.8(4) . .
N2 C8 C7 108.0(4) . .
C8 C9 C4 124.0(5) . .
C8 C9 C10 117.4(4) . .
C4 C9 C10 118.5(4) . .
C12 C10 C11 118.3(4) 2 .
C12 C10 C9 122.2(4) 2 .
C11 C10 C9 119.5(4) . .
C12 C11 C10 120.7(4) . .
C11 C12 C10 121.0(4) . 2
C17 C13 C14 107.3(4) . .
C17 C13 C20 127.0(5) . .
C14 C13 C20 125.2(5) . .
C17 C13 Ir1 71.8(3) . .
C14 C13 Ir1 72.0(3) . .
C20 C13 Ir1 127.4(4) . .
C15 C14 C13 107.9(4) . .
C15 C14 C21 126.4(5) . .
C13 C14 C21 125.6(5) . .
C15 C14 Ir1 71.0(3) . .
C13 C14 Ir1 68.6(3) . .
C21 C14 Ir1 128.2(4) . .
C14 C15 C16 108.3(5) . .
C14 C15 C22 126.9(6) . .
C16 C15 C22 124.7(5) . .
C14 C15 Ir1 70.9(3) . .
C16 C15 Ir1 69.8(3) . .
C22 C15 Ir1 126.0(4) . .
C17 C16 C15 107.8(5) . .
C17 C16 C18 127.8(6) . .
C15 C16 C18 124.2(6) . .
C17 C16 Ir1 71.0(3) . .
C15 C16 Ir1 71.3(3) . .
C18 C16 Ir1 127.1(4) . .
C16 C17 C13 108.5(5) . .
C16 C17 C19 126.4(5) . .
C13 C17 C19 125.0(5) . .
C16 C17 Ir1 70.5(3) . .
C13 C17 Ir1 69.2(3) . .
C19 C17 Ir1 125.3(4) . .
Cl1C C1C Cl2C 110.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 N1 2.069(4) .
Ir1 N2 2.070(4) .
Ir1 C13 2.133(5) .
Ir1 C16 2.160(5) .
Ir1 C17 2.167(5) .
Ir1 C14 2.178(5) .
Ir1 C15 2.180(5) .
Ir1 Cl1 2.4097(13) .
N1 C1 1.344(6) .
N1 C4 1.387(6) .
N2 C5 1.340(6) .
N2 C8 1.406(6) .
C1 C2 1.408(7) .
C2 C3 1.391(7) .
C3 C4 1.418(7) .
C4 C9 1.412(7) .
C5 C6 1.406(7) .
C6 C7 1.374(7) .
C7 C8 1.422(7) .
C8 C9 1.402(7) .
C9 C10 1.486(7) .
C10 C12 1.395(6) 2
C10 C11 1.408(6) .
C11 C12 1.393(7) .
C12 C10 1.395(6) 2
C13 C17 1.437(7) .
C13 C14 1.456(7) .
C13 C20 1.501(7) .
C14 C15 1.422(7) .
C14 C21 1.494(8) .
C15 C16 1.446(8) .
C15 C22 1.489(9) .
C16 C17 1.426(8) .
C16 C18 1.499(8) .
C17 C19 1.479(8) .
Cl1C C1C 1.760(6) .
Cl2C C1C 1.764(6) .
