#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:20:56 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178560 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/68/4066803.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_4066803
loop_
_publ_author_name
'Adams, Richard D.'
'Trufan, Eszter'
_publ_section_title
;
 Iridium−Germanium and −Tin Carbonyl Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4346
_journal_paper_doi               10.1021/om1006424
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C52 H44 Ge4 Ir2 O4'
_chemical_formula_weight         1407.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.470(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3589(7)
_cell_length_b                   20.6075(14)
_cell_length_c                   12.0951(8)
_cell_measurement_reflns_used    5080
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.24
_cell_volume                     2521.0(3)
_computing_cell_refinement       'SAINT+  V6.45 (Bruker, 2003)'
_computing_data_collection       'SMART V5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT+  V6.45'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34007
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    7.654
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            paleyellow
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.950
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0448
_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)+(0.0419P)²+5.1864P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                4415
_reflns_number_total             5150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1006424_si_001.cif
_cod_data_source_block           H2Ir2(CO)4(GePh2)2(GePh2H)2
_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_sg_symbol_H-M      P2(1)/n
_cod_database_code               4066803
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ir1 Ir 1.00110(3) 0.945591(12) 0.07979(2) 0.04226(10) Uani 1 1 d .
Ge1 Ge 0.94074(8) 0.93240(4) 0.26891(6) 0.0514(2) Uani 1 1 d .
Ge2 Ge 0.95470(7) 1.05851(3) 0.12061(6) 0.04394(17) Uani 1 1 d .
O11 O 1.2939(7) 0.9610(4) 0.1915(6) 0.093(2) Uani 1 1 d .
O12 O 1.0050(8) 0.7998(3) 0.0443(7) 0.106(2) Uani 1 1 d .
C11 C 1.1865(7) 0.9554(4) 0.1498(7) 0.0564(18) Uani 1 1 d .
C12 C 1.0059(10) 0.8549(4) 0.0551(8) 0.075(2) Uani 1 1 d .
C13 C 1.0902(8) 0.8911(4) 0.3726(6) 0.0568(18) Uani 1 1 d .
C14 C 1.1633(11) 0.9258(5) 0.4606(8) 0.088(3) Uani 1 1 d .
H14 H 1.1407 0.9687 0.4709 0.106 Uiso 1 1 calc R
C15 C 1.2714(12) 0.8981(7) 0.5356(9) 0.112(4) Uani 1 1 d .
H15 H 1.3201 0.9224 0.5950 0.134 Uiso 1 1 calc R
C16 C 1.3046(11) 0.8350(6) 0.5207(9) 0.091(3) Uani 1 1 d .
H16 H 1.3749 0.8157 0.5708 0.109 Uiso 1 1 calc R
C17 C 1.2351(11) 0.8010(5) 0.4333(9) 0.094(3) Uani 1 1 d .
H17 H 1.2596 0.7586 0.4216 0.112 Uiso 1 1 calc R
C18 C 1.1278(11) 0.8282(4) 0.3606(8) 0.086(3) Uani 1 1 d .
H18 H 1.0796 0.8033 0.3018 0.104 Uiso 1 1 calc R
C19 C 0.7763(8) 0.8838(4) 0.2588(6) 0.0581(19) Uani 1 1 d .
C20 C 0.6862(10) 0.9043(6) 0.3183(9) 0.088(3) Uani 1 1 d .
H20 H 0.7048 0.9413 0.3629 0.105 Uiso 1 1 calc R
C21 C 0.5652(11) 0.8714(7) 0.3147(11) 0.109(4) Uani 1 1 d .
H21 H 0.5050 0.8864 0.3558 0.131 Uiso 1 1 calc R
C22 C 0.5397(11) 0.8178(7) 0.2499(11) 0.104(4) Uani 1 1 d .
H22 H 0.4617 0.7949 0.2475 0.125 Uiso 1 1 calc R
C23 C 0.6258(14) 0.7967(6) 0.1885(12) 0.130(5) Uani 1 1 d .
H23 H 0.6055 0.7607 0.1415 0.156 Uiso 1 1 calc R
C24 C 0.7441(11) 0.8288(5) 0.1960(10) 0.098(3) Uani 1 1 d .
H24 H 0.8046 0.8123 0.1565 0.118 Uiso 1 1 calc R
C25 C 1.0780(7) 1.1093(3) 0.2326(6) 0.0504(17) Uani 1 1 d .
C26 C 1.0415(9) 1.1295(4) 0.3305(7) 0.066(2) Uani 1 1 d .
H26 H 0.9566 1.1209 0.3403 0.079 Uiso 1 1 calc R
C27 C 1.1298(12) 1.1626(5) 0.4148(7) 0.089(3) Uani 1 1 d .
H27 H 1.1043 1.1754 0.4807 0.106 Uiso 1 1 calc R
C28 C 1.2530(12) 1.1760(6) 0.4003(9) 0.102(4) Uani 1 1 d .
H28 H 1.3118 1.1982 0.4566 0.122 Uiso 1 1 calc R
C29 C 1.2916(11) 1.1576(6) 0.3054(9) 0.111(4) Uani 1 1 d .
H29 H 1.3758 1.1678 0.2956 0.133 Uiso 1 1 calc R
C30 C 1.2043(9) 1.1231(5) 0.2221(8) 0.082(3) Uani 1 1 d .
H30 H 1.2323 1.1093 0.1580 0.099 Uiso 1 1 calc R
C31 C 0.7776(7) 1.0899(4) 0.1203(6) 0.0526(17) Uani 1 1 d .
C32 C 0.7563(10) 1.1560(4) 0.1261(8) 0.078(3) Uani 1 1 d .
H32 H 0.8277 1.1843 0.1353 0.094 Uiso 1 1 calc R
C33 C 0.6308(11) 1.1804(5) 0.1186(10) 0.097(3) Uani 1 1 d .
H33 H 0.6179 1.2250 0.1221 0.116 Uiso 1 1 calc R
C34 C 0.5261(11) 1.1395(6) 0.1062(11) 0.108(4) Uani 1 1 d .
H34 H 0.4414 1.1563 0.0988 0.130 Uiso 1 1 calc R
C35 C 0.5439(10) 1.0731(6) 0.1043(11) 0.098(3) Uani 1 1 d .
H35 H 0.4723 1.0452 0.0988 0.118 Uiso 1 1 calc R
C36 C 0.6699(9) 1.0487(4) 0.1109(8) 0.076(2) Uani 1 1 d .
H36 H 0.6824 1.0040 0.1089 0.091 Uiso 1 1 calc R
H1 H 0.834(6) 0.938(2) 0.035(5) 0.030(15) Uiso 1 1 d .
H2 H 0.918(7) 0.996(3) 0.330(5) 0.06(2) 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 0.0000 0.0000 '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'
Ge Ge 0.1547 1.8001 '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
C12 Ir1 C11 96.6(4) . .
C12 Ir1 Ge2 169.2(3) . .
C11 Ir1 Ge2 91.9(2) . .
C12 Ir1 Ge1 93.3(3) . .
C11 Ir1 Ge1 91.8(2) . .
Ge2 Ir1 Ge1 79.69(2) . .
C12 Ir1 Ge2 78.6(3) . 3_775
C11 Ir1 Ge2 93.1(2) . 3_775
Ge2 Ir1 Ge2 107.76(2) . 3_775
Ge1 Ir1 Ge2 170.93(3) . 3_775
C12 Ir1 Ir1 129.9(3) . 3_775
C11 Ir1 Ir1 94.2(2) . 3_775
Ge2 Ir1 Ir1 55.690(18) . 3_775
Ge1 Ir1 Ir1 135.09(2) . 3_775
Ge2 Ir1 Ir1 52.067(17) 3_775 3_775
C12 Ir1 H1 85.1(17) . .
C11 Ir1 H1 172.8(19) . .
Ge2 Ir1 H1 85.7(17) . .
Ge1 Ir1 H1 81.1(19) . .
Ge2 Ir1 H1 94.1(19) 3_775 .
Ir1 Ir1 H1 90.0(18) 3_775 .
C19 Ge1 C13 111.9(3) . .
C19 Ge1 Ir1 112.5(2) . .
C13 Ge1 Ir1 108.1(2) . .
C19 Ge1 H2 104(3) . .
C13 Ge1 H2 104(2) . .
Ir1 Ge1 H2 116(2) . .
C31 Ge2 C25 107.4(3) . .
C31 Ge2 Ir1 122.8(2) . .
C25 Ge2 Ir1 121.4(2) . .
C31 Ge2 Ir1 111.7(2) . 3_775
C25 Ge2 Ir1 116.7(2) . 3_775
Ir1 Ge2 Ir1 72.24(2) . 3_775
O11 C11 Ir1 179.4(8) . .
O12 C12 Ir1 176.4(8) . .
C14 C13 C18 117.1(8) . .
C14 C13 Ge1 119.9(7) . .
C18 C13 Ge1 123.0(6) . .
C13 C14 C15 121.5(10) . .
C13 C14 H14 119.3 . .
C15 C14 H14 119.3 . .
C16 C15 C14 119.3(10) . .
C16 C15 H15 120.3 . .
C14 C15 H15 120.3 . .
C17 C16 C15 119.6(10) . .
C17 C16 H16 120.2 . .
C15 C16 H16 120.2 . .
C16 C17 C18 120.8(10) . .
C16 C17 H17 119.6 . .
C18 C17 H17 119.6 . .
C13 C18 C17 121.7(9) . .
C13 C18 H18 119.2 . .
C17 C18 H18 119.2 . .
C20 C19 C24 116.0(9) . .
C20 C19 Ge1 119.6(7) . .
C24 C19 Ge1 124.4(7) . .
C19 C20 C21 122.4(11) . .
C19 C20 H20 118.8 . .
C21 C20 H20 118.8 . .
C22 C21 C20 118.1(11) . .
C22 C21 H21 120.9 . .
C20 C21 H21 120.9 . .
C21 C22 C23 120.9(11) . .
C21 C22 H22 119.5 . .
C23 C22 H22 119.5 . .
C22 C23 C24 119.6(12) . .
C22 C23 H23 120.2 . .
C24 C23 H23 120.2 . .
C19 C24 C23 122.8(11) . .
C19 C24 H24 118.6 . .
C23 C24 H24 118.6 . .
C30 C25 C26 117.3(7) . .
C30 C25 Ge2 122.8(6) . .
C26 C25 Ge2 119.8(6) . .
C25 C26 C27 121.2(9) . .
C25 C26 H26 119.4 . .
C27 C26 H26 119.4 . .
C28 C27 C26 119.6(9) . .
C28 C27 H27 120.2 . .
C26 C27 H27 120.2 . .
C29 C28 C27 120.9(9) . .
C29 C28 H28 119.5 . .
C27 C28 H28 119.5 . .
C28 C29 C30 119.6(10) . .
C28 C29 H29 120.2 . .
C30 C29 H29 120.2 . .
C25 C30 C29 121.5(9) . .
C25 C30 H30 119.3 . .
C29 C30 H30 119.3 . .
C32 C31 C36 118.2(8) . .
C32 C31 Ge2 119.2(6) . .
C36 C31 Ge2 122.6(6) . .
C33 C32 C31 121.0(9) . .
C33 C32 H32 119.5 . .
C31 C32 H32 119.5 . .
C34 C33 C32 120.0(10) . .
C34 C33 H33 120.0 . .
C32 C33 H33 120.0 . .
C33 C34 C35 120.8(10) . .
C33 C34 H34 119.6 . .
C35 C34 H34 119.6 . .
C34 C35 C36 119.1(10) . .
C34 C35 H35 120.4 . .
C36 C35 H35 120.4 . .
C35 C36 C31 120.9(9) . .
C35 C36 H36 119.6 . .
C31 C36 H36 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 C12 1.895(9) .
Ir1 C11 1.935(8) .
Ir1 Ge2 2.4478(7) .
Ir1 Ge1 2.5129(8) .
Ir1 Ge2 2.5634(7) 3_775
Ir1 Ir1 2.9556(5) 3_775
Ir1 H1 1.71(6) .
Ge1 C19 1.957(8) .
Ge1 C13 1.964(8) .
Ge1 H2 1.55(7) .
Ge2 C31 1.944(7) .
Ge2 C25 1.953(7) .
Ge2 Ir1 2.5634(7) 3_775
O11 C11 1.124(9) .
O12 C12 1.143(10) .
C13 C14 1.367(12) .
C13 C18 1.369(12) .
C14 C15 1.402(15) .
C14 H14 0.9300 .
C15 C16 1.367(15) .
C15 H15 0.9300 .
C16 C17 1.340(14) .
C16 H16 0.9300 .
C17 C18 1.380(13) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 C20 1.364(12) .
C19 C24 1.365(12) .
C20 C21 1.418(15) .
C20 H20 0.9300 .
C21 C22 1.348(17) .
C21 H21 0.9300 .
C22 C23 1.350(17) .
C22 H22 0.9300 .
C23 C24 1.378(14) .
C23 H23 0.9300 .
C24 H24 0.9300 .
C25 C30 1.372(11) .
C25 C26 1.383(10) .
C26 C27 1.392(12) .
C26 H26 0.9300 .
C27 C28 1.353(14) .
C27 H27 0.9300 .
C28 C29 1.349(15) .
C28 H28 0.9300 .
C29 C30 1.394(12) .
C29 H29 0.9300 .
C30 H30 0.9300 .
C31 C32 1.384(11) .
C31 C36 1.387(11) .
C32 C33 1.379(13) .
C32 H32 0.9300 .
C33 C34 1.356(15) .
C33 H33 0.9300 .
C34 C35 1.381(15) .
C34 H34 0.9300 .
C35 C36 1.385(12) .
C35 H35 0.9300 .
C36 H36 0.9300 .
