#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:03:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179229 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/49/4314986.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_4314986
loop_
_publ_author_name
'Guo-Liang Wang'
'Yue-Jian Lin'
'Heinz Berke'
'Guo-Xin Jin'
_publ_section_title
;
 Two-Step Assembly of Multinuclear Metallacycles with Half-Sandwich Ir,
 Rh, and Ru Fragments for Counteranion Encapsulation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2193
_journal_page_last               2201
_journal_paper_doi               10.1021/ic902011v
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C80 H92 F12 Ir4 N4 O20 S4'
_chemical_formula_weight         2554.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.715(12)
_cell_length_b                   19.715(12)
_cell_length_c                   12.650(11)
_cell_measurement_reflns_used    788
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.056
_cell_measurement_theta_min      2.816
_cell_volume                     4917(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_sigmaI/netI    0.1250
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22974
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        6.76
_exptl_absorpt_coefficient_mu    5.567
_exptl_absorpt_correction_T_max  0.6060
_exptl_absorpt_correction_T_min  0.4023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.489
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5324
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.0483
_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)+(0.0569P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                2112
_reflns_number_total             5324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902011v_si_001_3.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4314986
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -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_assembly
_atom_site_disorder_group
Ir1 Ir 0.963458(18) 0.344671(18) 0.11568(3) 0.06183(16) Uani 1 1 d . . .
N1 N 1.2626(4) 0.4908(4) 0.3020(7) 0.066(2) Uani 1 1 d . . .
O1 O 1.0198(4) 0.3063(4) -0.0120(5) 0.091(2) Uani 1 1 d . . .
O2 O 1.0506(3) 0.3952(3) 0.1657(6) 0.075(2) Uani 1 1 d . . .
O3 O 0.9166(8) 0.2859(6) 0.6983(10) 0.241(7) Uani 1 1 d . . .
O4 O 0.9244(6) 0.2831(5) 0.5051(8) 0.167(4) Uani 1 1 d . . .
O5 O 1.0169(8) 0.2563(7) 0.6149(10) 0.223(7) Uani 1 1 d . . .
S1 S 0.9513(3) 0.2949(2) 0.6040(4) 0.1307(14) Uani 1 1 d . . .
F1 F 1.0160(7) 0.3955(6) 0.6845(9) 0.247(6) Uani 1 1 d . . .
F2 F 1.0242(7) 0.3892(6) 0.5212(11) 0.256(7) Uani 1 1 d . . .
F3 F 0.9302(10) 0.4204(7) 0.5918(12) 0.280(8) Uani 1 1 d . . .
C1 C 1.1056(7) 0.2758(8) -0.1261(9) 0.161(7) Uani 1 1 d . . .
H1A H 1.1284 0.2344 -0.1079 0.242 Uiso 1 1 calc R . .
H1B H 1.1368 0.3059 -0.1608 0.242 Uiso 1 1 calc R . .
H1C H 1.0684 0.2660 -0.1726 0.242 Uiso 1 1 calc R . .
C2 C 1.0799(7) 0.3083(7) -0.0297(9) 0.091(4) Uani 1 1 d . . .
C3 C 1.1268(6) 0.3433(6) 0.0383(9) 0.094(4) Uani 1 1 d . . .
H3 H 1.1726 0.3369 0.0241 0.113 Uiso 1 1 calc R . .
C4 C 1.1106(5) 0.3873(5) 0.1260(9) 0.070(3) Uani 1 1 d . . .
C5 C 1.2757(6) 0.4700(6) 0.2005(10) 0.089(4) Uani 1 1 d . . .
H5 H 1.3185 0.4775 0.1718 0.107 Uiso 1 1 calc R . .
C6 C 1.2255(6) 0.4373(5) 0.1385(8) 0.084(3) Uani 1 1 d . . .
H6 H 1.2342 0.4250 0.0688 0.101 Uiso 1 1 calc R . .
C7 C 1.1638(5) 0.4244(5) 0.1842(8) 0.064(3) Uani 1 1 d . . .
C8 C 1.1513(5) 0.4461(5) 0.2862(9) 0.076(3) Uani 1 1 d . . .
H8 H 1.1095 0.4380 0.3180 0.092 Uiso 1 1 calc R . .
C9 C 1.2013(6) 0.4796(6) 0.3394(9) 0.093(4) Uani 1 1 d . . .
H9 H 1.1914 0.4957 0.4068 0.111 Uiso 1 1 calc R . .
C10 C 0.8971(5) 0.4315(5) 0.1073(10) 0.068(3) Uani 1 1 d . . .
C11 C 0.8844(5) 0.3902(6) 0.0205(10) 0.076(3) Uani 1 1 d . . .
C12 C 0.8642(5) 0.3258(6) 0.0566(11) 0.081(3) Uani 1 1 d . . .
C13 C 0.8632(5) 0.3293(6) 0.1721(11) 0.084(3) Uani 1 1 d . . .
C14 C 0.8855(5) 0.3940(6) 0.2027(9) 0.070(3) Uani 1 1 d . . .
C15 C 0.9192(6) 0.5041(5) 0.1069(9) 0.102(4) Uani 1 1 d . . .
H15A H 0.9376 0.5153 0.0389 0.153 Uiso 1 1 calc R . .
H15B H 0.9532 0.5108 0.1602 0.153 Uiso 1 1 calc R . .
H15C H 0.8809 0.5328 0.1215 0.153 Uiso 1 1 calc R . .
C16 C 0.8908(6) 0.4112(6) -0.0939(8) 0.103(4) Uani 1 1 d . . .
H16A H 0.8464 0.4193 -0.1227 0.154 Uiso 1 1 calc R . .
H16B H 0.9126 0.3757 -0.1332 0.154 Uiso 1 1 calc R . .
H16C H 0.9173 0.4520 -0.0986 0.154 Uiso 1 1 calc R . .
C17 C 0.8447(6) 0.2651(6) -0.0118(11) 0.130(5) Uani 1 1 d . . .
H17A H 0.8051 0.2760 -0.0525 0.195 Uiso 1 1 calc R . .
H17B H 0.8353 0.2268 0.0326 0.195 Uiso 1 1 calc R . .
H17C H 0.8815 0.2543 -0.0586 0.195 Uiso 1 1 calc R . .
C18 C 0.8425(6) 0.2740(6) 0.2474(10) 0.119(5) Uani 1 1 d . . .
H18A H 0.8722 0.2741 0.3075 0.178 Uiso 1 1 calc R . .
H18B H 0.8453 0.2309 0.2123 0.178 Uiso 1 1 calc R . .
H18C H 0.7967 0.2816 0.2704 0.178 Uiso 1 1 calc R . .
C19 C 0.8851(6) 0.4216(6) 0.3119(9) 0.102(4) Uani 1 1 d . . .
H19A H 0.8441 0.4468 0.3233 0.153 Uiso 1 1 calc R . .
H19B H 0.9235 0.4509 0.3214 0.153 Uiso 1 1 calc R . .
H19C H 0.8875 0.3849 0.3617 0.153 Uiso 1 1 calc R . .
C20 C 0.9823(13) 0.3740(11) 0.5952(14) 0.149(6) Uani 1 1 d U . .
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'
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'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
O2 Ir1 O1 88.2(3) . . ?
O2 Ir1 C13 137.2(5) . . ?
O1 Ir1 C13 134.4(5) . . ?
O2 Ir1 C14 102.7(3) . . ?
O1 Ir1 C14 160.9(4) . . ?
C13 Ir1 C14 38.6(4) . . ?
O2 Ir1 N1 82.3(3) . 8_746 ?
O1 Ir1 N1 83.0(3) . 8_746 ?
C13 Ir1 N1 97.0(3) . 8_746 ?
C14 Ir1 N1 113.7(4) . 8_746 ?
O2 Ir1 C12 161.5(4) . . ?
O1 Ir1 C12 98.8(4) . . ?
C13 Ir1 C12 40.2(4) . . ?
C14 Ir1 C12 66.2(4) . . ?
N1 Ir1 C12 115.4(4) 8_746 . ?
O2 Ir1 C10 97.8(3) . . ?
O1 Ir1 C10 124.7(4) . . ?
C13 Ir1 C10 64.2(4) . . ?
C14 Ir1 C10 39.1(4) . . ?
N1 Ir1 C10 152.3(4) 8_746 . ?
C12 Ir1 C10 64.1(4) . . ?
O2 Ir1 C11 124.4(4) . . ?
O1 Ir1 C11 95.9(4) . . ?
C13 Ir1 C11 64.9(4) . . ?
C14 Ir1 C11 65.0(4) . . ?
N1 Ir1 C11 153.4(4) 8_746 . ?
C12 Ir1 C11 38.3(4) . . ?
C10 Ir1 C11 37.5(4) . . ?
C9 N1 C5 117.3(10) . . ?
C9 N1 Ir1 126.4(8) . 7_676 ?
C5 N1 Ir1 116.2(8) . 7_676 ?
C2 O1 Ir1 130.6(8) . . ?
C4 O2 Ir1 125.4(7) . . ?
O4 S1 O3 124.6(9) . . ?
O4 S1 O5 109.2(7) . . ?
O3 S1 O5 106.4(9) . . ?
O4 S1 C20 103.7(8) . . ?
O3 S1 C20 110.8(9) . . ?
O5 S1 C20 99.3(11) . . ?
O1 C2 C3 122.4(11) . . ?
O1 C2 C1 118.7(12) . . ?
C3 C2 C1 118.9(12) . . ?
C2 C3 C4 127.3(11) . . ?
O2 C4 C3 124.9(10) . . ?
O2 C4 C7 113.4(10) . . ?
C3 C4 C7 121.6(10) . . ?
N1 C5 C6 121.5(11) . . ?
C7 C6 C5 118.0(10) . . ?
C6 C7 C8 119.7(10) . . ?
C6 C7 C4 120.8(10) . . ?
C8 C7 C4 119.5(10) . . ?
C9 C8 C7 118.8(10) . . ?
N1 C9 C8 124.5(11) . . ?
C11 C10 C14 109.6(9) . . ?
C11 C10 C15 127.6(11) . . ?
C14 C10 C15 122.9(11) . . ?
C11 C10 Ir1 71.6(6) . . ?
C14 C10 Ir1 69.3(5) . . ?
C15 C10 Ir1 125.6(7) . . ?
C10 C11 C12 108.8(10) . . ?
C10 C11 C16 125.6(11) . . ?
C12 C11 C16 125.6(12) . . ?
C10 C11 Ir1 70.9(6) . . ?
C12 C11 Ir1 69.4(6) . . ?
C16 C11 Ir1 125.9(8) . . ?
C11 C12 C13 106.6(11) . . ?
C11 C12 C17 126.4(13) . . ?
C13 C12 C17 126.9(13) . . ?
C11 C12 Ir1 72.3(6) . . ?
C13 C12 Ir1 69.7(6) . . ?
C17 C12 Ir1 124.6(8) . . ?
C14 C13 C12 108.3(10) . . ?
C14 C13 C18 124.7(13) . . ?
C12 C13 C18 126.9(13) . . ?
C14 C13 Ir1 70.8(6) . . ?
C12 C13 Ir1 70.0(6) . . ?
C18 C13 Ir1 124.7(8) . . ?
C13 C14 C10 106.6(10) . . ?
C13 C14 C19 126.0(12) . . ?
C10 C14 C19 126.5(11) . . ?
C13 C14 Ir1 70.6(6) . . ?
C10 C14 Ir1 71.6(6) . . ?
C19 C14 Ir1 130.8(7) . . ?
F2 C20 F3 107.5(19) . . ?
F2 C20 F1 102.5(19) . . ?
F3 C20 F1 100.4(15) . . ?
F2 C20 S1 120.0(15) . . ?
F3 C20 S1 110.3(19) . . ?
F1 C20 S1 114.0(14) . . ?
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 O2 2.084(6) . ?
Ir1 O1 2.101(8) . ?
Ir1 C13 2.123(10) . ?
Ir1 C14 2.125(10) . ?
Ir1 N1 2.126(8) 8_746 ?
Ir1 C12 2.127(10) . ?
Ir1 C10 2.157(9) . ?
Ir1 C11 2.165(11) . ?
N1 C9 1.316(12) . ?
N1 C5 1.372(12) . ?
N1 Ir1 2.126(8) 7_676 ?
O1 C2 1.205(12) . ?
O2 C4 1.295(11) . ?
O3 S1 1.387(10) . ?
O4 S1 1.380(10) . ?
O5 S1 1.506(11) . ?
S1 C20 1.68(2) . ?
F1 C20 1.377(19) . ?
F2 C20 1.28(2) . ?
F3 C20 1.38(2) . ?
C1 C2 1.467(14) . ?
C2 C3 1.440(14) . ?
C3 C4 1.444(14) . ?
C4 C7 1.476(12) . ?
C5 C6 1.417(13) . ?
C6 C7 1.371(12) . ?
C7 C8 1.381(12) . ?
C8 C9 1.364(13) . ?
C10 C11 1.390(13) . ?
C10 C14 1.433(13) . ?
C10 C15 1.497(13) . ?
C11 C12 1.407(14) . ?
C11 C16 1.510(13) . ?
C12 C13 1.462(15) . ?
C12 C17 1.526(14) . ?
C13 C14 1.403(14) . ?
C13 C18 1.505(14) . ?
C14 C19 1.485(13) . ?
