#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:46:09 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178611 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/22/4072243.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_4072243
loop_
_publ_author_name
'Jia, Wei-Guo'
'Han, Ying-Feng'
'Jin, Guo-Xin'
_publ_section_title
;
 Synthesis and Characterization of Binuclear Half-Sandwich Iridium and
 Rhodium Carbene Complexes Containing 1,2-Dichalcogenolato Carborane or
 Carbonato Ligands
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6035
_journal_paper_doi               10.1021/om800694h
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C36 H56 Cl8 Ir2 N4 O8'
_chemical_formula_weight         1340.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.541(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.514(4)
_cell_length_b                   11.847(4)
_cell_length_c                   17.498(6)
_cell_measurement_reflns_used    883
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.268
_cell_measurement_theta_min      2.830
_cell_volume                     2459.5(14)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13883
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        8.62
_exptl_absorpt_coefficient_mu    5.888
_exptl_absorpt_correction_T_max  0.6502
_exptl_absorpt_correction_T_min  0.4721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5368
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0329P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                4010
_reflns_number_total             5368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800694h_si_001.cif
_cod_data_source_block           f70422bm
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2459.6(15)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4072243
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
Ir1 Ir 0.274150(16) 0.817898(16) 0.547653(12) 0.03301(7) Uani 1 1 d .
N1 N 0.4223(4) 0.8767(4) 0.4436(3) 0.0402(11) Uani 1 1 d .
N2 N 0.3828(4) 0.7020(4) 0.4353(3) 0.0436(11) Uani 1 1 d .
O1 O 0.3740(3) 0.6918(3) 0.6205(2) 0.0409(9) Uani 1 1 d .
O2 O 0.4238(3) 0.8683(3) 0.6387(2) 0.0372(8) Uani 1 1 d .
O3 O 0.5313(3) 0.7361(3) 0.7207(2) 0.0519(10) Uani 1 1 d .
C1 C 0.4481(5) 0.7628(5) 0.6639(3) 0.0383(12) Uani 1 1 d .
C2 C 0.3686(4) 0.7965(4) 0.4730(3) 0.0353(12) Uani 1 1 d .
C3 C 0.4677(6) 0.8309(6) 0.3894(4) 0.0594(17) Uani 1 1 d .
H3 H 0.5085 0.8694 0.3616 0.071 Uiso 1 1 calc R
C4 C 0.4433(6) 0.7213(6) 0.3836(4) 0.0590(17) Uani 1 1 d .
H4 H 0.4632 0.6686 0.3511 0.071 Uiso 1 1 calc R
C5 C 0.4413(4) 0.9919(4) 0.4720(3) 0.0430(13) Uani 1 1 d .
H5A H 0.3879 1.0113 0.4998 0.052 Uiso 1 1 calc R
H5B H 0.4285 1.0423 0.4263 0.052 Uiso 1 1 calc R
C6 C 0.3442(6) 0.5902(5) 0.4484(4) 0.0642(19) Uani 1 1 d .
H6A H 0.3777 0.5694 0.5040 0.096 Uiso 1 1 calc R
H6B H 0.3657 0.5367 0.4148 0.096 Uiso 1 1 calc R
H6C H 0.2636 0.5906 0.4352 0.096 Uiso 1 1 calc R
C7 C 0.1085(5) 0.8038(6) 0.4622(4) 0.0530(16) Uani 1 1 d .
C8 C 0.1071(5) 0.7584(5) 0.5372(4) 0.0499(15) Uani 1 1 d .
C9 C 0.1353(5) 0.8446(5) 0.5970(3) 0.0454(14) Uani 1 1 d .
C10 C 0.1535(4) 0.9450(5) 0.5581(4) 0.0482(14) Uani 1 1 d .
C11 C 0.1381(5) 0.9213(6) 0.4761(4) 0.0535(16) Uani 1 1 d .
C12 C 0.0736(6) 0.7436(9) 0.3816(5) 0.098(3) Uani 1 1 d .
H12A H -0.0058 0.7539 0.3554 0.148 Uiso 1 1 calc R
H12B H 0.0898 0.6645 0.3899 0.148 Uiso 1 1 calc R
H12C H 0.1145 0.7743 0.3484 0.148 Uiso 1 1 calc R
C13 C 0.0791(6) 0.6375(6) 0.5500(5) 0.082(2) Uani 1 1 d .
H13A H 0.1247 0.6131 0.6026 0.124 Uiso 1 1 calc R
H13B H 0.0938 0.5905 0.5098 0.124 Uiso 1 1 calc R
H13C H 0.0009 0.6320 0.5459 0.124 Uiso 1 1 calc R
C14 C 0.1441(6) 0.8303(7) 0.6835(4) 0.076(2) Uani 1 1 d .
H14A H 0.1913 0.8886 0.7149 0.114 Uiso 1 1 calc R
H14B H 0.1764 0.7579 0.7021 0.114 Uiso 1 1 calc R
H14C H 0.0704 0.8352 0.6891 0.114 Uiso 1 1 calc R
C15 C 0.1841(6) 1.0577(6) 0.5961(5) 0.080(2) Uani 1 1 d .
H15A H 0.2285 1.0979 0.5694 0.120 Uiso 1 1 calc R
H15B H 0.2268 1.0483 0.6520 0.120 Uiso 1 1 calc R
H15C H 0.1167 1.0996 0.5916 0.120 Uiso 1 1 calc R
C16 C 0.1364(6) 1.0044(8) 0.4104(5) 0.109(4) Uani 1 1 d .
H16A H 0.0609 1.0117 0.3742 0.163 Uiso 1 1 calc R
H16B H 0.1848 0.9780 0.3813 0.163 Uiso 1 1 calc R
H16C H 0.1625 1.0766 0.4340 0.163 Uiso 1 1 calc R
C17 C 0.7536(8) 0.6866(7) 0.6697(5) 0.093(3) Uani 1 1 d .
H17A H 0.7669 0.7569 0.6997 0.112 Uiso 1 1 calc R
H17B H 0.7091 0.6383 0.6927 0.112 Uiso 1 1 calc R
Cl1 Cl 0.6770(3) 0.71485(19) 0.57043(16) 0.1156(9) Uani 1 1 d .
Cl2 Cl 0.8817(2) 0.6220(3) 0.68169(18) 0.1389(11) Uani 1 1 d .
C18 C 0.3120(6) 0.4416(6) 0.6848(4) 0.073(2) Uani 1 1 d .
H18A H 0.3417 0.5090 0.6673 0.087 Uiso 1 1 calc R
H18B H 0.3753 0.3970 0.7170 0.087 Uiso 1 1 calc R
Cl3 Cl 0.2304(3) 0.4800(3) 0.74301(17) 0.1597(14) Uani 1 1 d .
Cl4 Cl 0.2372(3) 0.3652(2) 0.60206(19) 0.1396(11) Uani 1 1 d .
O4 O 0.4138(5) 0.0060(4) 0.7723(3) 0.0655(13) Uani 1 1 d D
H4A H 0.440(7) 0.067(5) 0.774(6) 0.13(4) Uiso 1 1 d D
H4B H 0.436(7) -0.024(7) 0.741(4) 0.11(4) Uiso 1 1 d 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 0.0000 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'
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'
O O 0.0106 0.0060 '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_3
C2 Ir1 O1 86.91(17) .
C2 Ir1 O2 87.88(18) .
O1 Ir1 O2 62.08(13) .
C2 Ir1 C7 99.9(2) .
O1 Ir1 C7 128.7(2) .
O2 Ir1 C7 166.6(2) .
C2 Ir1 C11 102.2(2) .
O1 Ir1 C11 165.62(19) .
O2 Ir1 C11 128.6(2) .
C7 Ir1 C11 39.2(2) .
C2 Ir1 C8 130.4(2) .
O1 Ir1 C8 101.10(19) .
O2 Ir1 C8 139.1(2) .
C7 Ir1 C8 38.6(2) .
C11 Ir1 C8 64.5(2) .
C2 Ir1 C10 134.3(2) .
O1 Ir1 C10 137.31(19) .
O2 Ir1 C10 102.24(18) .
C7 Ir1 C10 64.5(2) .
C11 Ir1 C10 38.1(2) .
C8 Ir1 C10 63.6(2) .
C2 Ir1 C9 164.4(2) .
O1 Ir1 C9 104.88(18) .
O2 Ir1 C9 106.53(18) .
C7 Ir1 C9 64.8(2) .
C11 Ir1 C9 64.3(2) .
C8 Ir1 C9 38.2(2) .
C10 Ir1 C9 38.0(2) .
C2 N1 C3 110.5(5) .
C2 N1 C5 125.4(4) .
C3 N1 C5 123.7(5) .
C2 N2 C4 111.9(5) .
C2 N2 C6 125.6(5) .
C4 N2 C6 122.5(5) .
C1 O1 Ir1 94.0(3) .
C1 O2 Ir1 92.2(3) .
O3 C1 O1 124.6(5) .
O3 C1 O2 123.8(5) .
O1 C1 O2 111.6(5) .
N2 C2 N1 103.9(4) .
N2 C2 Ir1 127.9(4) .
N1 C2 Ir1 127.9(4) .
C4 C3 N1 107.8(5) .
C3 C4 N2 105.8(5) .
N1 C5 C5 111.4(6) 3_676
C8 C7 C11 106.8(5) .
C8 C7 C12 126.5(7) .
C11 C7 C12 126.4(7) .
C8 C7 Ir1 71.3(3) .
C11 C7 Ir1 70.6(3) .
C12 C7 Ir1 127.9(4) .
C7 C8 C9 109.4(5) .
C7 C8 C13 124.6(6) .
C9 C8 C13 125.9(6) .
C7 C8 Ir1 70.1(3) .
C9 C8 Ir1 72.3(3) .
C13 C8 Ir1 124.2(4) .
C10 C9 C8 106.7(5) .
C10 C9 C14 127.4(6) .
C8 C9 C14 125.8(6) .
C10 C9 Ir1 70.4(3) .
C8 C9 Ir1 69.5(3) .
C14 C9 Ir1 124.7(4) .
C11 C10 C9 109.2(5) .
C11 C10 C15 124.4(6) .
C9 C10 C15 126.4(6) .
C11 C10 Ir1 69.7(3) .
C9 C10 Ir1 71.6(3) .
C15 C10 Ir1 124.8(4) .
C10 C11 C7 107.9(5) .
C10 C11 C16 127.4(7) .
C7 C11 C16 124.2(7) .
C10 C11 Ir1 72.2(3) .
C7 C11 Ir1 70.2(3) .
C16 C11 Ir1 129.3(4) .
Cl2 C17 Cl1 113.8(5) .
Cl4 C18 Cl3 111.9(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 C2 2.037(5) .
Ir1 O1 2.099(3) .
Ir1 O2 2.122(3) .
Ir1 C7 2.142(6) .
Ir1 C11 2.147(5) .
Ir1 C8 2.159(5) .
Ir1 C10 2.180(5) .
Ir1 C9 2.195(5) .
N1 C2 1.356(6) .
N1 C3 1.363(7) .
N1 C5 1.446(6) .
N2 C2 1.339(6) .
N2 C4 1.372(8) .
N2 C6 1.453(7) .
O1 C1 1.303(6) .
O2 C1 1.328(6) .
O3 C1 1.230(6) .
C3 C4 1.330(8) .
C5 C5 1.497(10) 3_676
C7 C8 1.423(8) .
C7 C11 1.440(8) .
C7 C12 1.516(9) .
C8 C9 1.424(8) .
C8 C13 1.508(9) .
C9 C10 1.424(8) .
C9 C14 1.492(8) .
C10 C11 1.414(8) .
C10 C15 1.487(8) .
C11 C16 1.508(8) .
C17 Cl2 1.727(9) .
C17 Cl1 1.729(9) .
C18 Cl4 1.712(7) .
C18 Cl3 1.718(7) .
