#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:00:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178764 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/18/4101830.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_4101830
loop_
_publ_author_name
'Zhigang Xie'
'Liqing Ma'
'Kathryn E. deKrafft'
'Athena Jin'
'Wenbin Lin'
_publ_section_title
;
 Porous Phosphorescent Coordination Polymers for Oxygen Sensing
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              922
_journal_page_last               923
_journal_paper_doi               10.1021/ja909629f
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C90 H42 Ir2 N12 O20 Zn4'
_chemical_formula_weight         2257.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            3
_cell_length_a                   14.199
_cell_length_b                   14.199
_cell_length_c                   39.0767(5)
_cell_measurement_reflns_used    6826
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      66.00
_cell_measurement_theta_min      3.39
_cell_volume                     6822.82(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.985
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            8897
_diffrn_reflns_theta_full        66.38
_diffrn_reflns_theta_max         66.38
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    7.309
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.050
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3300
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.094
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2634
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_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+38.6822P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                2574
_reflns_number_total             2634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909629f_si_001_1.cif
_cod_data_source_block           IrZn-1
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4101830
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_assembly
_atom_site_disorder_group
Ir1 Ir 0.6667 0.3333 0.027660(7) 0.02646(18) Uani 1 3 d S . 1
Zn1 Zn 1.3333 0.6667 0.11903(5) 0.0301(5) Uani 0.50 3 d SP . 1
Zn2 Zn 1.48087(15) 0.74832(15) 0.14709(4) 0.0517(4) Uani 0.50 1 d P . 1
C1A C 0.8028(4) 0.3833(4) 0.05559(12) 0.0298(9) Uani 1 1 d . A 1
C2A C 0.8188(4) 0.3329(4) 0.08456(14) 0.0424(12) Uani 1 1 d . A 1
H2A H 0.7625 0.2645 0.0916 0.051 Uiso 1 1 calc R A 1
C3A C 0.9143(5) 0.3818(5) 0.10246(14) 0.0455(13) Uani 1 1 d . A 1
H3A H 0.9221 0.3455 0.1214 0.055 Uiso 1 1 calc R A 1
C4A C 1.0008(4) 0.4837(5) 0.09348(13) 0.0399(11) Uani 1 1 d . A 1
C5A C 0.9890(4) 0.5335(4) 0.06446(12) 0.0370(11) Uani 1 1 d . A 1
H5A H 1.0463 0.6014 0.0574 0.044 Uiso 1 1 calc R A 1
C6A C 0.8919(4) 0.4830(4) 0.04573(11) 0.0321(10) Uani 1 1 d . A 1
C7A C 0.7447(4) 0.2391(4) -0.03062(12) 0.0351(10) Uani 1 1 d . B 1
H7A H 0.7717 0.3079 -0.0408 0.042 Uiso 1 1 calc R B 1
C8A C 0.7603(5) 0.1632(5) -0.04731(13) 0.0418(12) Uani 1 1 d . B 1
H8A H 0.7966 0.1795 -0.0685 0.050 Uiso 1 1 calc R B 1
C9A C 0.7215(5) 0.0627(5) -0.03245(15) 0.0500(14) Uani 1 1 d . B 1
H9A H 0.7315 0.0091 -0.0432 0.060 Uiso 1 1 calc R B 1
C10A C 0.6681(5) 0.0418(5) -0.00169(14) 0.0455(13) Uani 1 1 d . B 1
H10A H 0.6415 -0.0264 0.0088 0.055 Uiso 1 1 calc R B 1
C11A C 0.6532(4) 0.1212(4) 0.01392(12) 0.0328(10) Uani 1 1 d . . 1
C12A C 1.1021(5) 0.5376(5) 0.11389(14) 0.0479(13) Uani 1 1 d . A 1
N1A N 0.6933(3) 0.2207(3) -0.00079(10) 0.0290(8) Uani 1 1 d . B 1
O1A O 1.1859(5) 0.6148(5) 0.10137(15) 0.034(2) Uiso 0.543(13) 1 d P A 1
O2A O 1.1034(6) 0.5050(7) 0.1441(2) 0.050(2) Uiso 0.543(13) 1 d P . 1
O2B O 1.1227(7) 0.4743(7) 0.1317(2) 0.043(3) Uiso 0.457(13) 1 d P A 2
O1B O 1.1541(8) 0.6429(8) 0.1109(3) 0.054(3) Uiso 0.457(13) 1 d P A 2
O3A O 1.3333 0.6667 0.1667 0.0367(18) Uani 1 6 d S . 1
N1D N 0.9860(17) 0.2107(16) 0.8830(5) 0.213(7) Uiso 1 1 d DU C 1
C2D C 1.038(2) 0.3131(19) 0.8642(6) 0.221(10) Uiso 1 1 d DU C 1
C3D C 0.887(2) 0.118(2) 0.8683(7) 0.260(13) Uiso 1 1 d DU C 1
C1D C 1.035(3) 0.201(3) 0.9135(8) 0.37(2) Uiso 1 1 d DU C 1
O1D O 0.980(3) 0.126(3) 0.9328(10) 0.55(3) Uiso 1 1 d DU C 1
O2H O 0.0000 0.0000 0.0000 0.52(5) Uiso 1 6 d S D 1
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'
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'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 '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
_geom_angle_publ_flag
C1A Ir1 C1A 93.42(18) 3_665 2_655 ?
C1A Ir1 C1A 93.42(18) 3_665 . ?
C1A Ir1 C1A 93.42(18) 2_655 . ?
C1A Ir1 N1A 79.23(18) 3_665 . ?
C1A Ir1 N1A 170.67(17) 2_655 . ?
C1A Ir1 N1A 92.76(18) . . ?
C1A Ir1 N1A 170.67(17) 3_665 2_655 ?
C1A Ir1 N1A 92.76(18) 2_655 2_655 ?
C1A Ir1 N1A 79.23(18) . 2_655 ?
N1A Ir1 N1A 95.26(14) . 2_655 ?
C1A Ir1 N1A 92.76(18) 3_665 3_665 ?
C1A Ir1 N1A 79.23(18) 2_655 3_665 ?
C1A Ir1 N1A 170.67(17) . 3_665 ?
N1A Ir1 N1A 95.26(14) . 3_665 ?
N1A Ir1 N1A 95.26(14) 2_655 3_665 ?
O3A Zn1 O1A 110.57(19) . . ?
O3A Zn1 O1A 110.57(19) . 3_775 ?
O1A Zn1 O1A 108.4(2) . 3_775 ?
O3A Zn1 O1A 110.57(19) . 2_755 ?
O1A Zn1 O1A 108.4(2) . 2_755 ?
O1A Zn1 O1A 108.4(2) 3_775 2_755 ?
O3A Zn1 Zn2 58.90(6) . 3_775 ?
O1A Zn1 Zn2 87.16(19) . 3_775 ?
O1A Zn1 Zn2 164.1(2) 3_775 3_775 ?
O1A Zn1 Zn2 68.4(2) 2_755 3_775 ?
O3A Zn1 Zn2 58.90(6) . . ?
O1A Zn1 Zn2 164.1(2) . . ?
O1A Zn1 Zn2 68.4(2) 3_775 . ?
O1A Zn1 Zn2 87.16(19) 2_755 . ?
Zn2 Zn1 Zn2 95.73(8) 3_775 . ?
O3A Zn1 Zn2 58.90(6) . 2_755 ?
O1A Zn1 Zn2 68.4(2) . 2_755 ?
O1A Zn1 Zn2 87.16(19) 3_775 2_755 ?
O1A Zn1 Zn2 164.1(2) 2_755 2_755 ?
Zn2 Zn1 Zn2 95.73(8) 3_775 2_755 ?
Zn2 Zn1 Zn2 95.73(8) . 2_755 ?
O3A Zn2 O2A 99.3(2) . 13_765 ?
O3A Zn2 Zn1 53.92(6) . . ?
O2A Zn2 Zn1 150.3(3) 13_765 . ?
O3A Zn2 O2A 92.0(2) . 2_755 ?
O2A Zn2 O2A 106.1(3) 13_765 2_755 ?
Zn1 Zn2 O2A 89.2(2) . 2_755 ?
O3A Zn2 O1A 94.47(18) . 3_775 ?
O2A Zn2 O1A 128.4(3) 13_765 3_775 ?
Zn1 Zn2 O1A 52.54(18) . 3_775 ?
O2A Zn2 O1A 123.0(3) 2_755 3_775 ?
O3A Zn2 Zn2 52.96(2) . 14_565 ?
O2A Zn2 Zn2 80.3(2) 13_765 14_565 ?
Zn1 Zn2 Zn2 90.29(5) . 14_565 ?
O2A Zn2 Zn2 51.6(2) 2_755 14_565 ?
O1A Zn2 Zn2 142.47(18) 3_775 14_565 ?
O3A Zn2 Zn2 52.96(2) . 15_545 ?
O2A Zn2 Zn2 60.7(3) 13_765 15_545 ?
Zn1 Zn2 Zn2 90.29(5) . 15_545 ?
O2A Zn2 Zn2 134.5(2) 2_755 15_545 ?
O1A Zn2 Zn2 91.24(16) 3_775 15_545 ?
Zn2 Zn2 Zn2 82.99(9) 14_565 15_545 ?
O3A Zn2 Zn2 37.04(2) . 3_775 ?
O2A Zn2 Zn2 124.8(2) 13_765 3_775 ?
Zn1 Zn2 Zn2 42.13(4) . 3_775 ?
O2A Zn2 Zn2 61.0(2) 2_755 3_775 ?
O1A Zn2 Zn2 94.67(18) 3_775 3_775 ?
Zn2 Zn2 Zn2 48.51(4) 14_565 3_775 ?
Zn2 Zn2 Zn2 90.000(1) 15_545 3_775 ?
O3A Zn2 Zn2 37.04(2) . 2_755 ?
O2A Zn2 Zn2 109.2(3) 13_765 2_755 ?
Zn1 Zn2 Zn2 42.14(4) . 2_755 ?
O2A Zn2 Zn2 120.9(2) 2_755 2_755 ?
O1A Zn2 Zn2 59.96(17) 3_775 2_755 ?
Zn2 Zn2 Zn2 90.0 14_565 2_755 ?
Zn2 Zn2 Zn2 48.51(4) 15_545 2_755 ?
Zn2 Zn2 Zn2 60.0 3_775 2_755 ?
C6A C1A C2A 116.0(4) . . ?
C6A C1A Ir1 115.4(3) . . ?
C2A C1A Ir1 128.5(4) . . ?
C3A C2A C1A 121.4(5) . . ?
C2A C3A C4A 122.2(5) . . ?
C5A C4A C3A 117.7(5) . . ?
C5A C4A C12A 120.7(5) . . ?
C3A C4A C12A 121.6(5) . . ?
C4A C5A C6A 120.3(5) . . ?
C1A C6A C5A 122.3(4) . . ?
C1A C6A C11A 116.3(4) . 2_655 ?
C5A C6A C11A 121.4(4) . 2_655 ?
N1A C7A C8A 123.5(5) . . ?
C7A C8A C9A 118.5(5) . . ?
C10A C9A C8A 119.0(5) . . ?
C9A C10A C11A 120.1(5) . . ?
N1A C11A C10A 120.3(4) . . ?
N1A C11A C6A 113.5(4) . 3_665 ?
C10A C11A C6A 126.2(5) . 3_665 ?
O1A C12A O2A 120.3(6) . . ?
O1A C12A C4A 119.8(5) . . ?
O2A C12A C4A 119.9(6) . . ?
C7A N1A C11A 118.6(4) . . ?
C7A N1A Ir1 126.6(3) . . ?
C11A N1A Ir1 114.8(3) . . ?
C12A O1A Zn1 124.1(5) . . ?
C12A O1A Zn2 101.3(5) . 2_755 ?
Zn1 O1A Zn2 59.05(17) . 2_755 ?
C12A O2A Zn2 131.7(6) . 13_765 ?
C12A O2A Zn2 102.7(6) . 3_775 ?
Zn2 O2A Zn2 67.7(2) 13_765 3_775 ?
Zn1 O3A Zn1 180.0 . 13_765 ?
Zn1 O3A Zn2 67.18(4) . 3_775 ?
Zn1 O3A Zn2 112.83(4) 13_765 3_775 ?
Zn1 O3A Zn2 67.18(4) . . ?
Zn1 O3A Zn2 112.82(4) 13_765 . ?
Zn2 O3A Zn2 105.92(5) 3_775 . ?
Zn1 O3A Zn2 112.83(4) . 15_545 ?
Zn1 O3A Zn2 67.17(4) 13_765 15_545 ?
Zn2 O3A Zn2 180.0 3_775 15_545 ?
Zn2 O3A Zn2 74.08(5) . 15_545 ?
Zn1 O3A Zn2 112.83(4) . 13_765 ?
Zn1 O3A Zn2 67.17(4) 13_765 13_765 ?
Zn2 O3A Zn2 74.08(5) 3_775 13_765 ?
Zn2 O3A Zn2 180.0 . 13_765 ?
Zn2 O3A Zn2 105.92(5) 15_545 13_765 ?
Zn1 O3A Zn2 67.18(4) . 2_755 ?
Zn1 O3A Zn2 112.82(4) 13_765 2_755 ?
Zn2 O3A Zn2 105.92(5) 3_775 2_755 ?
Zn2 O3A Zn2 105.92(5) . 2_755 ?
Zn2 O3A Zn2 74.08(5) 15_545 2_755 ?
Zn2 O3A Zn2 74.08(5) 13_765 2_755 ?
Zn1 O3A Zn2 112.83(4) . 14_565 ?
Zn1 O3A Zn2 67.18(4) 13_765 14_565 ?
Zn2 O3A Zn2 74.08(5) 3_775 14_565 ?
Zn2 O3A Zn2 74.08(5) . 14_565 ?
Zn2 O3A Zn2 105.92(5) 15_545 14_565 ?
Zn2 O3A Zn2 105.92(5) 13_765 14_565 ?
Zn2 O3A Zn2 179.996(1) 2_755 14_565 ?
C1D N1D C2D 120(2) . . ?
C1D N1D C3D 122(2) . . ?
C2D N1D C3D 118.1(19) . . ?
O1D C1D N1D 118(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C1A 2.014(5) 3_665 ?
Ir1 C1A 2.014(5) 2_655 ?
Ir1 C1A 2.015(5) . ?
Ir1 N1A 2.131(4) . ?
Ir1 N1A 2.131(4) 2_655 ?
Ir1 N1A 2.131(4) 3_665 ?
Zn1 O3A 1.8614(19) . ?
Zn1 O1A 1.965(6) . ?
Zn1 O1A 1.965(6) 3_775 ?
Zn1 O1A 1.965(6) 2_755 ?
Zn1 Zn2 2.123(2) 3_775 ?
Zn1 Zn2 2.123(2) . ?
Zn1 Zn2 2.123(2) 2_755 ?
Zn2 O3A 1.9721(17) . ?
Zn2 O2A 2.011(8) 13_765 ?
Zn2 O2A 2.239(9) 2_755 ?
Zn2 O1A 2.302(7) 3_775 ?
Zn2 Zn2 2.376(2) 14_565 ?
Zn2 Zn2 2.376(2) 15_545 ?
Zn2 Zn2 3.148(3) 3_775 ?
Zn2 Zn2 3.148(3) 2_755 ?
C1A C6A 1.401(7) . ?
C1A C2A 1.417(7) . ?
C2A C3A 1.368(8) . ?
C3A C4A 1.396(8) . ?
C4A C5A 1.390(7) . ?
C4A C12A 1.480(7) . ?
C5A C6A 1.401(7) . ?
C6A C11A 1.480(6) 2_655 ?
C7A N1A 1.330(6) . ?
C7A C8A 1.369(8) . ?
C8A C9A 1.376(9) . ?
C9A C10A 1.373(8) . ?
C10A C11A 1.388(7) . ?
C11A N1A 1.359(6) . ?
C11A C6A 1.480(6) 3_665 ?
C12A O1A 1.246(9) . ?
C12A O2A 1.271(9) . ?
O1A Zn2 2.302(7) 2_755 ?
O2A Zn2 2.011(8) 13_765 ?
O2A Zn2 2.239(9) 3_775 ?
O3A Zn1 1.8616(19) 13_765 ?
O3A Zn2 1.9721(18) 3_775 ?
O3A Zn2 1.9721(18) 15_545 ?
O3A Zn2 1.9721(18) 13_765 ?
O3A Zn2 1.9721(17) 2_755 ?
O3A Zn2 1.9721(18) 14_565 ?
N1D C1D 1.424(17) . ?
N1D C2D 1.458(16) . ?
N1D C3D 1.481(17) . ?
C1D O1D 1.21(2) . ?
