#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:37:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179757 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/53/7005333.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_7005333
loop_
_publ_author_name
'Adams, Christopher J.'
'Baber, R. Angharad'
'Connelly, Neil G.'
'Harding, Phimphaka'
'Hayward, Owen D.'
'Kandiah, Mathivathani'
'Orpen, A. Guy'
_publ_section_title
;
 Iodination of triazenide-bridged rhodium and iridium complexes:
 oxidative addition vs. one-electron oxidation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1325
_journal_page_last               1333
_journal_paper_doi               10.1039/b700736a
_journal_year                    2007
_chemical_formula_moiety         'C32 H30 I4 Ir2 N6 O4, C H2 Cl2'
_chemical_formula_sum            'C33 H32 Cl2 I4 Ir2 N6 O4'
_chemical_formula_weight         1539.55
_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
_cell_angle_alpha                94.177(18)
_cell_angle_beta                 100.254(14)
_cell_angle_gamma                98.35(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9001(15)
_cell_length_b                   9.642(2)
_cell_length_c                   13.510(5)
_cell_measurement_temperature    173(2)
_cell_volume                     1122.9(5)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11700
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.827
_exptl_absorpt_correction_T_max  .492
_exptl_absorpt_correction_T_min  .257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.892
_refine_diff_density_min         -2.963
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0330
_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)+(0.0612P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                3926
_reflns_number_total             5076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b700736a.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1123.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7005333
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.58645(2) 0.99800(2) 0.871547(15) 0.02392(8) Uani 1 1 d . . .
I1 I 0.31885(4) 1.04379(4) 0.92230(3) 0.02698(11) Uani 1 1 d . . .
I2 I 0.85549(5) 0.95767(4) 0.82484(3) 0.03522(12) Uani 1 1 d . . .
O1 O 0.4776(6) 0.6877(5) 0.8207(4) 0.0469(12) Uani 1 1 d . . .
O2 O 0.4377(5) 0.9562(4) 0.6586(3) 0.0385(11) Uani 1 1 d . . .
N1 N 0.5284(6) 1.1847(5) 0.7231(3) 0.0296(11) Uani 1 1 d . . .
N2 N 0.6075(5) 1.2727(5) 0.8018(3) 0.0262(10) Uani 1 1 d . . .
H2A H 0.6263 1.3644 0.7994 0.031 Uiso 1 1 calc R . .
N3 N 0.6541(5) 1.2141(5) 0.8814(3) 0.0243(10) Uani 1 1 d . . .
C1 C 0.5174(7) 0.8009(7) 0.8417(5) 0.0320(13) Uani 1 1 d . . .
C2 C 0.5047(6) 1.0331(6) 0.7310(4) 0.0283(12) Uani 1 1 d . . .
C11 C 0.4590(7) 1.2489(6) 0.6372(4) 0.0309(13) Uani 1 1 d . . .
C12 C 0.3726(8) 1.3565(7) 0.6535(5) 0.0381(15) Uani 1 1 d . . .
H12A H 0.3604 1.3864 0.7198 0.046 Uiso 1 1 calc R . .
C13 C 0.3068(8) 1.4167(8) 0.5722(5) 0.0475(18) Uani 1 1 d . . .
H13A H 0.2468 1.4884 0.5825 0.057 Uiso 1 1 calc R . .
C14 C 0.3244(8) 1.3766(7) 0.4739(5) 0.0453(17) Uani 1 1 d . . .
C15 C 0.4101(9) 1.2700(7) 0.4615(5) 0.0452(17) Uani 1 1 d . . .
H15A H 0.4214 1.2389 0.3952 0.054 Uiso 1 1 calc R . .
C16 C 0.4790(8) 1.2078(7) 0.5415(5) 0.0386(15) Uani 1 1 d . . .
H16A H 0.5401 1.1370 0.5310 0.046 Uiso 1 1 calc R . .
C17 C 0.2536(10) 1.4484(9) 0.3834(6) 0.060(2) Uani 1 1 d . . .
H17A H 0.3173 1.4455 0.3314 0.091 Uiso 1 1 calc R . .
H17B H 0.2494 1.5466 0.4055 0.091 Uiso 1 1 calc R . .
H17C H 0.1487 1.3989 0.3556 0.091 Uiso 1 1 calc R . .
C18 C 0.7339(6) 1.3153(6) 0.9640(4) 0.0261(12) Uani 1 1 d . . .
C19 C 0.6802(7) 1.4393(6) 0.9823(4) 0.0301(13) Uani 1 1 d . . .
H19A H 0.5886 1.4577 0.9409 0.036 Uiso 1 1 calc R . .
C20 C 0.7598(7) 1.5384(6) 1.0616(4) 0.0322(13) Uani 1 1 d . . .
H20A H 0.7219 1.6239 1.0740 0.039 Uiso 1 1 calc R . .
C21 C 0.8945(7) 1.5130(6) 1.1226(4) 0.0308(13) Uani 1 1 d . . .
C22 C 0.9480(7) 1.3871(6) 1.1029(4) 0.0286(12) Uani 1 1 d . . .
H22A H 1.0401 1.3686 1.1437 0.034 Uiso 1 1 calc R . .
C23 C 0.8678(6) 1.2879(6) 1.0240(4) 0.0285(12) Uani 1 1 d . . .
H23A H 0.9046 1.2019 1.0113 0.034 Uiso 1 1 calc R . .
C24 C 0.9797(8) 1.6190(7) 1.2108(5) 0.0402(15) Uani 1 1 d . . .
H24A H 1.0908 1.6333 1.2100 0.060 Uiso 1 1 calc R . .
H24B H 0.9621 1.5832 1.2745 0.060 Uiso 1 1 calc R . .
H24C H 0.9413 1.7088 1.2047 0.060 Uiso 1 1 calc R . .
C99 C 0.0637(13) 0.8684(13) 0.5922(8) 0.031(3) Uani 0.50 1 d P . .
H99A H 0.1221 0.9640 0.6157 0.038 Uiso 0.50 1 calc PR . .
H99B H -0.0472 0.8706 0.5922 0.038 Uiso 0.50 1 calc PR . .
Cl1 Cl 0.1317(5) 0.7455(5) 0.6745(4) 0.0803(14) Uani 0.50 1 d P . .
Cl2 Cl 0.0897(6) 0.8163(7) 0.4660(4) 0.103(2) Uani 0.50 1 d P . .
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'
I I -0.4742 1.8119 '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'
Cl Cl 0.1484 0.1585 '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
C1 Ir1 C2 91.7(2) . . ?
C1 Ir1 N3 171.6(2) . . ?
C2 Ir1 N3 80.0(2) . . ?
C1 Ir1 I2 88.29(19) . . ?
C2 Ir1 I2 91.58(16) . . ?
N3 Ir1 I2 90.34(12) . . ?
C1 Ir1 I1 92.89(19) . . ?
C2 Ir1 I1 89.22(16) . . ?
N3 Ir1 I1 88.61(12) . . ?
I2 Ir1 I1 178.558(15) . . ?
C1 Ir1 I1 89.35(18) . 2_677 ?
C2 Ir1 I1 175.08(15) . 2_677 ?
N3 Ir1 I1 98.98(12) . 2_677 ?
I2 Ir1 I1 93.25(2) . 2_677 ?
I1 Ir1 I1 85.93(2) . 2_677 ?
Ir1 I1 Ir1 94.07(2) . 2_677 ?
N2 N1 C11 116.1(5) . . ?
N2 N1 C2 119.8(4) . . ?
C11 N1 C2 123.8(5) . . ?
N3 N2 N1 115.2(5) . . ?
N2 N3 C18 112.2(4) . . ?
N2 N3 Ir1 115.5(4) . . ?
C18 N3 Ir1 132.1(3) . . ?
O1 C1 Ir1 177.3(6) . . ?
O2 C2 N1 118.6(5) . . ?
O2 C2 Ir1 132.2(5) . . ?
N1 C2 Ir1 109.2(4) . . ?
C16 C11 C12 120.6(5) . . ?
C16 C11 N1 120.8(5) . . ?
C12 C11 N1 118.5(5) . . ?
C13 C12 C11 118.4(6) . . ?
C12 C13 C14 122.3(6) . . ?
C15 C14 C13 117.3(6) . . ?
C15 C14 C17 121.1(7) . . ?
C13 C14 C17 121.6(7) . . ?
C16 C15 C14 122.1(7) . . ?
C15 C16 C11 119.3(6) . . ?
C19 C18 C23 120.3(5) . . ?
C19 C18 N3 120.4(5) . . ?
C23 C18 N3 119.3(5) . . ?
C18 C19 C20 120.1(5) . . ?
C21 C20 C19 120.5(5) . . ?
C22 C21 C20 118.7(5) . . ?
C22 C21 C24 120.4(5) . . ?
C20 C21 C24 120.8(5) . . ?
C21 C22 C23 120.7(5) . . ?
C18 C23 C22 119.7(5) . . ?
Cl1 C99 Cl2 108.9(7) . . ?
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 C1 1.901(7) . ?
Ir1 C2 1.980(6) . ?
Ir1 N3 2.071(5) . ?
Ir1 I2 2.6562(6) . ?
Ir1 I1 2.6795(6) . ?
Ir1 I1 2.8384(11) 2_677 ?
I1 Ir1 2.8384(11) 2_677 ?
O1 C1 1.097(7) . ?
O2 C2 1.193(6) . ?
N1 N2 1.331(6) . ?
N1 C11 1.439(7) . ?
N1 C2 1.461(7) . ?
N2 N3 1.283(6) . ?
N3 C18 1.435(7) . ?
C11 C16 1.375(8) . ?
C11 C12 1.405(8) . ?
C12 C13 1.361(9) . ?
C13 C14 1.398(10) . ?
C14 C15 1.384(9) . ?
C14 C17 1.531(9) . ?
C15 C16 1.367(8) . ?
C18 C19 1.372(8) . ?
C18 C23 1.388(7) . ?
C19 C20 1.396(8) . ?
C20 C21 1.393(8) . ?
C21 C22 1.392(7) . ?
C21 C24 1.522(8) . ?
C22 C23 1.395(8) . ?
C99 Cl1 1.780(12) . ?
C99 Cl2 1.805(13) . ?
