#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314147.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_4314147
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         'C38 H31 I3 Ir1 N1 O2 P2'
_chemical_formula_sum            'C38 H31 I3 Ir N O2 P2'
_chemical_formula_weight         1168.48
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-01-27T14:09:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.0000(10)
_cell_angle_beta                 94.713(2)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            4
_cell_length_a                   9.3661(3)
_cell_length_b                   16.4735(6)
_cell_length_c                   25.2247(5)
_cell_measurement_reflns_used    9171
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.6
_cell_measurement_wavelength     0.71073
_cell_volume                     3878.8(2)
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.063
_diffrn_reflns_av_unetI/netI     0.1049
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9607
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.945
_exptl_absorpt_correction_T_max  0.541
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
         multi-scan from symmetry-related measurements
  Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0401
_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)+(0.0293P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                5185
_reflns_number_total             8852
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic0340938_3.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C38 H31 I3 Ir1 N1 O2 P2'
_cod_database_code               4314147
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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 0.24390(3) 0.612412(17) 0.476104(10) 0.04592(9) Uani 1 1 d . . .
I1 I -0.03422(6) 0.63006(3) 0.49410(2) 0.07351(17) Uani 1 1 d . . .
I2 I 0.18317(6) 0.61795(4) 0.369960(18) 0.06632(16) Uani 1 1 d . . .
I3 I 0.30990(6) 0.78043(3) 0.479800(19) 0.05948(14) Uani 1 1 d . . .
C11 C 0.4387(11) 0.5908(6) 0.4622(3) 0.077(3) Uani 1 1 d . . .
O11 O 0.5455(6) 0.5810(4) 0.4560(2) 0.084(2) Uani 1 1 d . . .
C12 C 0.2713(9) 0.5937(5) 0.5488(3) 0.062(2) Uani 1 1 d . . .
O12 O 0.2857(8) 0.5804(4) 0.5928(2) 0.100(2) Uani 1 1 d . . .
N1 N 0.3661(5) 0.4516(3) 0.21381(18) 0.0384(12) Uani 1 1 d . . .
P1 P 0.45319(16) 0.37322(10) 0.23546(6) 0.0355(4) Uani 1 1 d . . .
P2 P 0.35452(16) 0.50054(10) 0.15960(6) 0.0361(4) Uani 1 1 d . . .
C111 C 0.6421(6) 0.3829(4) 0.2323(2) 0.0381(14) Uani 1 1 d . . .
C112 C 0.7094(7) 0.3603(4) 0.1871(3) 0.0501(17) Uani 1 1 d . . .
H112 H 0.6573 0.334 0.1592 0.06 Uiso 1 1 calc R . .
C113 C 0.8540(8) 0.3771(5) 0.1838(3) 0.063(2) Uani 1 1 d . . .
H113 H 0.8994 0.3606 0.1541 0.076 Uiso 1 1 calc R . .
C114 C 0.9293(8) 0.4178(5) 0.2243(3) 0.066(2) Uani 1 1 d . . .
H114 H 1.0252 0.4303 0.2214 0.08 Uiso 1 1 calc R . .
C115 C 0.8671(8) 0.4404(5) 0.2687(3) 0.061(2) Uani 1 1 d . . .
H115 H 0.92 0.4681 0.2958 0.073 Uiso 1 1 calc R . .
C116 C 0.7226(7) 0.4218(4) 0.2736(3) 0.0505(17) Uani 1 1 d . . .
H116 H 0.6806 0.4355 0.3045 0.061 Uiso 1 1 calc R . .
C121 C 0.4185(6) 0.3584(4) 0.3037(2) 0.0390(14) Uani 1 1 d . . .
C122 C 0.4843(7) 0.2951(4) 0.3324(2) 0.0498(17) Uani 1 1 d . . .
H122 H 0.5526 0.2636 0.3173 0.06 Uiso 1 1 calc R . .
C123 C 0.4490(8) 0.2786(5) 0.3832(3) 0.060(2) Uani 1 1 d . . .
H123 H 0.4938 0.2361 0.4023 0.072 Uiso 1 1 calc R . .
C124 C 0.3493(9) 0.3241(5) 0.4056(3) 0.066(2) Uani 1 1 d . . .
H124 H 0.327 0.3132 0.4401 0.079 Uiso 1 1 calc R . .
C125 C 0.2816(10) 0.3858(5) 0.3775(3) 0.077(2) Uani 1 1 d . . .
H125 H 0.2117 0.4158 0.3929 0.092 Uiso 1 1 calc R . .
C126 C 0.3152(9) 0.4043(4) 0.3267(3) 0.061(2) Uani 1 1 d . . .
H126 H 0.2694 0.4469 0.3081 0.073 Uiso 1 1 calc R . .
C131 C 0.3932(6) 0.2807(4) 0.2024(2) 0.0360(13) Uani 1 1 d . . .
C132 C 0.2498(7) 0.2752(5) 0.1843(3) 0.0572(19) Uani 1 1 d . . .
H132 H 0.1897 0.3194 0.1882 0.069 Uiso 1 1 calc R . .
C133 C 0.1953(9) 0.2058(6) 0.1609(3) 0.073(2) Uani 1 1 d . . .
H133 H 0.0996 0.2035 0.1479 0.088 Uiso 1 1 calc R . .
C134 C 0.2821(10) 0.1399(5) 0.1566(3) 0.072(2) Uani 1 1 d . . .
H134 H 0.2446 0.093 0.1403 0.086 Uiso 1 1 calc R . .
C135 C 0.4235(9) 0.1415(5) 0.1758(3) 0.062(2) Uani 1 1 d . . .
H135 H 0.4809 0.0957 0.1739 0.075 Uiso 1 1 calc R . .
C136 C 0.4790(8) 0.2132(4) 0.1981(3) 0.0532(17) Uani 1 1 d . . .
H136 H 0.5753 0.2158 0.2103 0.064 Uiso 1 1 calc R . .
C211 C 0.5229(6) 0.5348(4) 0.1396(2) 0.0413(15) Uani 1 1 d . . .
C212 C 0.5629(8) 0.5292(5) 0.0878(3) 0.069(2) Uani 1 1 d . . .
H212 H 0.5012 0.506 0.0612 0.082 Uiso 1 1 calc R . .
C213 C 0.6956(10) 0.5585(7) 0.0760(4) 0.092(3) Uani 1 1 d . . .
H213 H 0.7225 0.5534 0.0415 0.11 Uiso 1 1 calc R . .
C214 C 0.7866(10) 0.5941(6) 0.1132(5) 0.087(3) Uani 1 1 d . . .
H214 H 0.8743 0.6139 0.1041 0.105 Uiso 1 1 calc R . .
C215 C 0.7489(9) 0.6011(5) 0.1646(4) 0.079(3) Uani 1 1 d . . .
H215 H 0.8113 0.626 0.1902 0.095 Uiso 1 1 calc R . .
C216 C 0.6177(8) 0.5711(4) 0.1784(3) 0.0573(19) Uani 1 1 d . . .
H216 H 0.5933 0.5752 0.2133 0.069 Uiso 1 1 calc R . .
C221 C 0.2638(7) 0.4456(4) 0.1056(2) 0.0416(15) Uani 1 1 d . . .
C222 C 0.1186(7) 0.4611(4) 0.0905(3) 0.0522(17) Uani 1 1 d . . .
H222 H 0.0721 0.5039 0.1059 0.063 Uiso 1 1 calc R . .
C223 C 0.0460(9) 0.4131(5) 0.0533(3) 0.070(2) Uani 1 1 d . . .
H223 H -0.0506 0.4228 0.0438 0.084 Uiso 1 1 calc R . .
C224 C 0.1137(11) 0.3509(5) 0.0297(3) 0.071(2) Uani 1 1 d . . .
H224 H 0.0642 0.3205 0.0031 0.085 Uiso 1 1 calc R . .
C225 C 0.2538(10) 0.3332(5) 0.0448(3) 0.068(2) Uani 1 1 d . . .
H225 H 0.2971 0.2886 0.0302 0.082 Uiso 1 1 calc R . .
C226 C 0.3314(8) 0.3815(4) 0.0817(3) 0.0527(17) Uani 1 1 d . . .
H226 H 0.4281 0.3712 0.0905 0.063 Uiso 1 1 calc R . .
C231 C 0.2526(6) 0.5910(4) 0.1691(2) 0.0348(13) Uani 1 1 d . . .
C232 C 0.1960(7) 0.6089(4) 0.2165(3) 0.0491(16) Uani 1 1 d . . .
H232 H 0.211 0.5737 0.2452 0.059 Uiso 1 1 calc R . .
C233 C 0.1172(8) 0.6790(5) 0.2214(3) 0.059(2) Uani 1 1 d . . .
H233 H 0.0818 0.6915 0.2538 0.071 Uiso 1 1 calc R . .
C234 C 0.0912(8) 0.7294(5) 0.1795(3) 0.065(2) Uani 1 1 d . . .
H234 H 0.0369 0.776 0.1832 0.078 Uiso 1 1 calc R . .
C235 C 0.1441(8) 0.7125(4) 0.1314(3) 0.062(2) Uani 1 1 d . . .
H235 H 0.1245 0.7469 0.1024 0.075 Uiso 1 1 calc R . .
C236 C 0.2268(7) 0.6437(4) 0.1266(3) 0.0528(17) Uani 1 1 d . . .
H236 H 0.2655 0.6327 0.0946 0.063 Uiso 1 1 calc R . .
HY1 H 0.1991 0.5191 0.466 0.06 Uiso 1 1 d . . .
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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
C12 Ir1 C11 95.4(3) . . ?
C12 Ir1 I2 171.4(2) . . ?
C11 Ir1 I2 87.2(2) . . ?
C12 Ir1 I1 84.8(3) . . ?
C11 Ir1 I1 175.4(3) . . ?
I2 Ir1 I1 92.044(19) . . ?
C12 Ir1 I3 96.7(2) . . ?
C11 Ir1 I3 88.8(3) . . ?
I2 Ir1 I3 91.565(18) . . ?
I1 Ir1 I3 95.750(18) . . ?
O11 C11 Ir1 177.4(10) . . ?
O12 C12 Ir1 178.0(7) . . ?
P2 N1 P1 134.6(3) . . ?
N1 P1 C111 113.1(3) . . ?
N1 P1 C121 108.0(3) . . ?
C111 P1 C121 108.2(3) . . ?
N1 P1 C131 113.2(3) . . ?
C111 P1 C131 109.1(3) . . ?
C121 P1 C131 104.8(3) . . ?
N1 P2 C211 113.9(3) . . ?
N1 P2 C221 113.2(3) . . ?
C211 P2 C221 108.7(3) . . ?
N1 P2 C231 107.9(3) . . ?
C211 P2 C231 105.5(3) . . ?
C221 P2 C231 107.2(3) . . ?
C116 C111 C112 118.7(6) . . ?
C116 C111 P1 119.1(5) . . ?
C112 C111 P1 121.8(5) . . ?
C113 C112 C111 120.2(6) . . ?
C114 C113 C112 119.7(7) . . ?
C115 C114 C113 121.4(7) . . ?
C114 C115 C116 119.7(7) . . ?
C111 C116 C115 120.2(7) . . ?
C122 C121 C126 119.0(6) . . ?
C122 C121 P1 119.7(5) . . ?
C126 C121 P1 121.0(5) . . ?
C123 C122 C121 120.3(7) . . ?
C124 C123 C122 120.3(7) . . ?
C123 C124 C125 120.3(7) . . ?
C124 C125 C126 120.9(7) . . ?
C125 C126 C121 119.3(7) . . ?
C136 C131 C132 118.4(6) . . ?
C136 C131 P1 123.7(5) . . ?
C132 C131 P1 117.6(5) . . ?
C133 C132 C131 121.0(7) . . ?
C132 C133 C134 119.7(8) . . ?
C133 C134 C135 121.3(7) . . ?
C134 C135 C136 118.5(8) . . ?
C131 C136 C135 121.0(7) . . ?
C212 C211 C216 118.7(6) . . ?
C212 C211 P2 123.8(5) . . ?
C216 C211 P2 117.5(5) . . ?
C213 C212 C211 119.5(8) . . ?
C214 C213 C212 122.0(9) . . ?
C213 C214 C215 119.6(8) . . ?
C214 C215 C216 120.4(8) . . ?
C215 C216 C211 119.8(7) . . ?
C226 C221 C222 119.0(6) . . ?
C226 C221 P2 120.5(5) . . ?
C222 C221 P2 120.2(5) . . ?
C223 C222 C221 119.8(7) . . ?
C224 C223 C222 120.7(8) . . ?
C223 C224 C225 120.6(7) . . ?
C224 C225 C226 120.2(8) . . ?
C225 C226 C221 119.6(7) . . ?
C232 C231 C236 118.8(6) . . ?
C232 C231 P2 122.7(5) . . ?
C236 C231 P2 118.5(5) . . ?
C231 C232 C233 120.3(7) . . ?
C234 C233 C232 120.4(7) . . ?
C233 C234 C235 120.7(7) . . ?
C234 C235 C236 119.2(7) . . ?
C231 C236 C235 120.6(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 C12 1.857(8) . ?
Ir1 C11 1.920(10) . ?
Ir1 I2 2.6927(5) . ?
Ir1 I1 2.6964(6) . ?
Ir1 I3 2.8359(6) . ?
C11 O11 1.038(10) . ?
C12 O12 1.127(8) . ?
N1 P2 1.584(5) . ?
N1 P1 1.599(5) . ?
P1 C111 1.784(6) . ?
P1 C121 1.793(6) . ?
P1 C131 1.805(6) . ?
P2 C211 1.786(6) . ?
P2 C221 1.790(6) . ?
P2 C231 1.796(6) . ?
C111 C116 1.391(8) . ?
C111 C112 1.399(8) . ?
C112 C113 1.392(10) . ?
C113 C114 1.370(10) . ?
C114 C115 1.355(10) . ?
C115 C116 1.403(9) . ?
C121 C122 1.386(8) . ?
C121 C126 1.392(9) . ?
C122 C123 1.378(9) . ?
C123 C124 1.356(10) . ?
C124 C125 1.364(11) . ?
C125 C126 1.379(9) . ?
C131 C136 1.381(9) . ?
C131 C132 1.386(8) . ?
C132 C133 1.366(11) . ?
C133 C134 1.366(12) . ?
C134 C135 1.372(11) . ?
C135 C136 1.391(10) . ?
C211 C212 1.393(9) . ?
C211 C216 1.401(9) . ?
C212 C213 1.387(11) . ?
C213 C214 1.348(13) . ?
C214 C215 1.376(13) . ?
C215 C216 1.396(11) . ?
C221 C226 1.395(9) . ?
C221 C222 1.405(9) . ?
C222 C223 1.367(10) . ?
C223 C224 1.366(12) . ?
C224 C225 1.367(11) . ?
C225 C226 1.385(10) . ?
C231 C232 1.379(8) . ?
C231 C236 1.384(9) . ?
C232 C233 1.381(10) . ?
C233 C234 1.352(10) . ?
C234 C235 1.376(11) . ?
C235 C236 1.384(10) . ?
