#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (mar 16 de feb de 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314145.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_4314145
loop_
_publ_author_name
'Samuel Gautron'
'Robert Giordano'
'Carole Le Berre'
'Joël Jaud'
'Jean-Claude Daran'
'Philippe Serp'
'Philippe Kalck'
_publ_contact_author             'Jean-Claude Daran'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France
;
_publ_contact_author_email       ' daran@lcc-toulouse.fr '
_publ_contact_author_fax         ' (33) 5 61 55 30 03 '
_publ_contact_author_phone       ' (33) 5 61 33 31 74 '
_publ_section_title
;
 Isolation and Structural Characterization of Anionic and Neutral
 Compounds Resulting from the Oxidative Addition of HI or CH₃I to
 [IrI₂(CO)₂]⁻
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5523
_journal_page_last               5530
_journal_paper_doi               10.1021/ic0340938
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C3 H3 I2 Ir1 O2'
_chemical_formula_sum            'C3 H3 I2 Ir O2'
_chemical_formula_weight         517.05
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2003-01-27T13:58:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                102.94(2)
_cell_angle_beta                 110.72(3)
_cell_angle_gamma                90.52(2)
_cell_formula_units_Z            2
_cell_length_a                   6.6629(18)
_cell_length_b                   7.6766(19)
_cell_length_c                   8.710(2)
_cell_measurement_reflns_used    1936
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      4.07
_cell_measurement_wavelength     0.71073
_cell_volume                     404.2(2)
_computing_cell_refinement       'CRYSALIS 169 (Oxford-Diffraction, 2001)'
_computing_data_collection       'CRYSALIS 169 (Oxford-Diffraction, 2001)'
_computing_data_reduction        'CRYSALIS 169 (Oxford-Diffraction, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Oxfod-Diffraction Xcalibur'
_diffrn_measurement_method       ω-φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2468
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.07
_diffrn_standards_decay_%        0.01
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.078
_exptl_absorpt_correction_T_max  0.2578
_exptl_absorpt_correction_T_min  0.0726
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
         (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.875
_refine_diff_density_rms         0.293
_refine_ls_extinction_coef       0.0042(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0532P)²+1.1163P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.09
_reflns_number_gt                1365
_reflns_number_total             1541
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic0340938_1.cif
_cod_data_source_block           4
_cod_original_cell_volume        404.19(18)
_cod_original_formula_sum        'C3 H3 I2 Ir1 O2'
_cod_database_code               4314145
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 0.39123(6) 0.29420(5) 0.29104(4) 0.02450(18) Uani 1 1 d . . .
I2 I 0.76456(12) 0.14498(11) 0.39067(10) 0.0406(2) Uani 1 1 d . . .
I3 I 0.60332(12) 0.62599(9) 0.37736(8) 0.0326(2) Uani 1 1 d . . .
O2 O -0.0166(15) 0.4640(15) 0.1671(12) 0.052(2) Uani 1 1 d . . .
C1 C 0.2595(18) 0.0587(17) 0.2183(13) 0.036(3) Uani 1 1 d . . .
C2 C 0.1371(19) 0.4052(17) 0.2179(14) 0.037(3) Uani 1 1 d . . .
O1 O 0.1730(16) -0.0800(14) 0.1689(13) 0.058(3) Uani 1 1 d . . .
C3 C 0.4124(18) 0.2607(16) 0.0439(14) 0.034(2) Uani 1 1 d . . .
H3A H 0.458 0.3743 0.032 0.051 Uiso 1 1 calc R . .
H3B H 0.2737 0.2163 -0.0421 0.051 Uiso 1 1 calc R . .
H3C H 0.515 0.1766 0.0322 0.051 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.0242(3) 0.0254(2) 0.0235(2) 0.00471(16) 0.00894(16) 0.00291(15)
I2 0.0323(4) 0.0408(5) 0.0480(5) 0.0119(4) 0.0129(3) 0.0097(3)
I3 0.0431(4) 0.0291(4) 0.0309(4) 0.0067(3) 0.0204(3) -0.0020(3)
O2 0.034(5) 0.067(7) 0.059(6) 0.027(5) 0.016(4) 0.014(4)
C1 0.029(6) 0.043(7) 0.029(5) 0.009(5) 0.002(4) -0.005(5)
C2 0.034(7) 0.046(7) 0.035(6) 0.003(5) 0.020(5) 0.008(5)
O1 0.047(6) 0.048(6) 0.069(6) 0.016(5) 0.007(5) -0.015(5)
C3 0.035(6) 0.033(6) 0.034(6) 0.008(5) 0.012(5) 0.008(5)
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
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 96.3(5) . . ?
C1 Ir1 C3 87.7(5) . . ?
C2 Ir1 C3 89.6(4) . . ?
C1 Ir1 I2 85.6(4) . . ?
C2 Ir1 I2 177.4(4) . . ?
C3 Ir1 I2 88.7(3) . . ?
C1 Ir1 I3 174.7(4) . . ?
C2 Ir1 I3 86.4(4) . . ?
C3 Ir1 I3 87.7(3) . . ?
I2 Ir1 I3 91.50(4) . . ?
C1 Ir1 I3 98.8(3) . 2_666 ?
C2 Ir1 I3 91.1(3) . 2_666 ?
C3 Ir1 I3 173.3(3) . 2_666 ?
I2 Ir1 I3 90.38(4) . 2_666 ?
I3 Ir1 I3 85.70(3) . 2_666 ?
Ir1 I3 Ir1 94.30(3) . 2_666 ?
O1 C1 Ir1 176.7(10) . . ?
O2 C2 Ir1 176.4(11) . . ?
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 1.872(12) . ?
Ir1 C2 1.872(12) . ?
Ir1 C3 2.165(11) . ?
Ir1 I2 2.6874(11) . ?
Ir1 I3 2.7156(11) . ?
Ir1 I3 2.8021(11) 2_666 ?
I3 Ir1 2.8021(11) 2_666 ?
O2 C2 1.107(14) . ?
C1 O1 1.123(15) . ?
