#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:37:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179757 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/53/7005331.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_7005331
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 H28 I2 Ir N6 O4 Rh'
_chemical_formula_sum            'C32 H28 I2 Ir N6 O4 Rh'
_chemical_formula_weight         1109.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 110.566(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.513(5)
_cell_length_b                   8.4782(15)
_cell_length_c                   21.624(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3521.0(12)
_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 0.992
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10979
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    6.042
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2088
_refine_diff_density_max         1.409
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.00023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0305
_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)+(0.0430P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                2958
_reflns_number_total             4051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b700736a.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      C2/c
_cod_database_code               7005331
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Rh1 Rh -0.010965(11) 0.31576(2) 0.306442(9) 0.02080(8) Uani 0.50 1 d P . .
Ir1 Ir -0.010965(11) 0.31576(2) 0.306442(9) 0.02080(8) Uani 0.50 1 d P . .
I1 I -0.033456(17) 0.32569(4) 0.424584(14) 0.03697(11) Uani 1 1 d . . .
C1 C -0.0972(3) 0.2072(5) 0.2740(2) 0.0313(10) Uani 1 1 d . . .
O1 O -0.14781(18) 0.1442(4) 0.25587(16) 0.0444(8) Uani 1 1 d . . .
C2 C 0.0382(2) 0.1235(5) 0.3369(2) 0.0321(10) Uani 1 1 d . . .
O2 O 0.06515(19) 0.0115(3) 0.35282(17) 0.0470(9) Uani 1 1 d . . .
N1 N 0.06765(17) 0.5235(3) 0.23461(15) 0.0219(7) Uani 1 1 d . . .
N2 N 0.09816(18) 0.5413(4) 0.29804(15) 0.0247(7) Uani 1 1 d . . .
N3 N 0.08059(17) 0.4500(4) 0.33741(15) 0.0232(7) Uani 1 1 d . . .
C11 C 0.0946(2) 0.6355(5) 0.19970(18) 0.0243(9) Uani 1 1 d . . .
C12 C 0.1647(2) 0.6754(5) 0.2220(2) 0.0330(10) Uani 1 1 d . . .
H12A H 0.1961 0.6259 0.2602 0.040 Uiso 1 1 calc R . .
C13 C 0.1888(3) 0.7869(5) 0.1887(2) 0.0369(11) Uani 1 1 d . . .
H13A H 0.2366 0.8154 0.2053 0.044 Uiso 1 1 calc R . .
C14 C 0.1447(2) 0.8586(5) 0.1314(2) 0.0319(10) Uani 1 1 d . . .
C15 C 0.0754(3) 0.8160(5) 0.1097(2) 0.0348(11) Uani 1 1 d . . .
H15A H 0.0440 0.8639 0.0710 0.042 Uiso 1 1 calc R . .
C16 C 0.0506(2) 0.7062(5) 0.1426(2) 0.0335(10) Uani 1 1 d . . .
H16A H 0.0027 0.6784 0.1260 0.040 Uiso 1 1 calc R . .
C17 C 0.1714(3) 0.9784(5) 0.0951(2) 0.0447(13) Uani 1 1 d . . .
H17A H 0.1499 0.9606 0.0474 0.067 Uiso 1 1 calc R . .
H17B H 0.2221 0.9682 0.1083 0.067 Uiso 1 1 calc R . .
H17C H 0.1598 1.0846 0.1059 0.067 Uiso 1 1 calc R . .
C18 C 0.1218(2) 0.4835(4) 0.40560(18) 0.0238(9) Uani 1 1 d . . .
C19 C 0.1347(2) 0.6377(5) 0.42839(19) 0.0258(9) Uani 1 1 d . . .
H19A H 0.1164 0.7230 0.3989 0.031 Uiso 1 1 calc R . .
C20 C 0.1738(2) 0.6676(5) 0.4934(2) 0.0291(10) Uani 1 1 d . . .
H20A H 0.1822 0.7737 0.5082 0.035 Uiso 1 1 calc R . .
C21 C 0.2012(2) 0.5458(5) 0.53795(19) 0.0299(9) Uani 1 1 d . . .
C22 C 0.1894(2) 0.3925(5) 0.5144(2) 0.0341(10) Uani 1 1 d . . .
H22A H 0.2087 0.3074 0.5437 0.041 Uiso 1 1 calc R . .
C23 C 0.1499(2) 0.3607(5) 0.4488(2) 0.0311(10) Uani 1 1 d . . .
H23A H 0.1423 0.2548 0.4336 0.037 Uiso 1 1 calc R . .
C24 C 0.2425(3) 0.5774(6) 0.61005(19) 0.0437(12) Uani 1 1 d . . .
H24A H 0.2736 0.4882 0.6286 0.066 Uiso 1 1 calc R . .
H24B H 0.2104 0.5909 0.6342 0.066 Uiso 1 1 calc R . .
H24C H 0.2701 0.6736 0.6140 0.066 Uiso 1 1 calc R . .
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'
Rh Rh -1.1178 0.9187 '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 Rh1 C2 91.43(17) . . ?
C1 Rh1 N3 175.59(14) . . ?
C2 Rh1 N3 92.72(16) . . ?
C1 Rh1 N1 86.85(15) . 2 ?
C2 Rh1 N1 175.83(15) . 2 ?
N3 Rh1 N1 88.91(12) . 2 ?
C1 Rh1 Ir1 95.64(13) . 2 ?
C2 Rh1 Ir1 94.48(13) . 2 ?
N3 Rh1 Ir1 82.55(9) . 2 ?
N1 Rh1 Ir1 81.92(8) 2 2 ?
C1 Rh1 Rh1 95.64(13) . 2 ?
C2 Rh1 Rh1 94.48(13) . 2 ?
N3 Rh1 Rh1 82.55(9) . 2 ?
N1 Rh1 Rh1 81.92(8) 2 2 ?
Ir1 Rh1 Rh1 0.000(8) 2 2 ?
C1 Rh1 I1 85.36(13) . . ?
C2 Rh1 I1 86.93(13) . . ?
N3 Rh1 I1 96.34(9) . . ?
N1 Rh1 I1 96.71(8) 2 . ?
Ir1 Rh1 I1 178.238(7) 2 . ?
Rh1 Rh1 I1 178.238(7) 2 . ?
O1 C1 Rh1 179.0(4) . . ?
O2 C2 Rh1 178.0(4) . . ?
N2 N1 C11 110.2(3) . . ?
N2 N1 Ir1 121.8(2) . 2 ?
C11 N1 Ir1 125.6(2) . 2 ?
N2 N1 Rh1 121.8(2) . 2 ?
C11 N1 Rh1 125.6(2) . 2 ?
Ir1 N1 Rh1 0.000(18) 2 2 ?
N3 N2 N1 118.9(3) . . ?
N2 N3 C18 110.8(3) . . ?
N2 N3 Rh1 122.8(2) . . ?
C18 N3 Rh1 124.7(2) . . ?
C16 C11 C12 118.4(4) . . ?
C16 C11 N1 120.2(4) . . ?
C12 C11 N1 121.4(4) . . ?
C13 C12 C11 120.2(4) . . ?
C12 C13 C14 121.5(5) . . ?
C15 C14 C13 117.3(4) . . ?
C15 C14 C17 121.5(4) . . ?
C13 C14 C17 121.2(4) . . ?
C16 C15 C14 121.7(4) . . ?
C15 C16 C11 120.8(4) . . ?
C23 C18 C19 119.1(4) . . ?
C23 C18 N3 119.8(3) . . ?
C19 C18 N3 121.1(3) . . ?
C20 C19 C18 120.4(4) . . ?
C19 C20 C21 121.3(4) . . ?
C22 C21 C20 117.8(4) . . ?
C22 C21 C24 120.5(4) . . ?
C20 C21 C24 121.7(4) . . ?
C21 C22 C23 121.4(4) . . ?
C18 C23 C22 119.9(4) . . ?
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
Rh1 C1 1.897(5) . ?
Rh1 C2 1.908(5) . ?
Rh1 N3 2.094(3) . ?
Rh1 N1 2.125(3) 2 ?
Rh1 Ir1 2.6329(5) 2 ?
Rh1 Rh1 2.6329(5) 2 ?
Rh1 I1 2.7522(5) . ?
C1 O1 1.109(5) . ?
C2 O2 1.092(5) . ?
N1 N2 1.301(4) . ?
N1 C11 1.439(5) . ?
N1 Ir1 2.125(3) 2 ?
N1 Rh1 2.125(3) 2 ?
N2 N3 1.292(4) . ?
N3 C18 1.447(5) . ?
C11 C16 1.383(5) . ?
C11 C12 1.388(6) . ?
C12 C13 1.381(6) . ?
C13 C14 1.391(6) . ?
C14 C15 1.379(6) . ?
C14 C17 1.500(6) . ?
C15 C16 1.374(6) . ?
C18 C23 1.382(5) . ?
C18 C19 1.389(5) . ?
C19 C20 1.376(5) . ?
C20 C21 1.389(5) . ?
C21 C22 1.386(6) . ?
C21 C24 1.514(5) . ?
C22 C23 1.391(5) . ?
