#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:39:49 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178626 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/37/4073779.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_4073779
loop_
_publ_author_name
'Sau, Yiu-Keung'
'Chan, Ka-Wang'
'Zhang, Qian-Feng'
'Williams, Ian D.'
'Leung, Wa-Hung'
_publ_section_title
;
 Alkyl and Aryl Compounds of Rhodium(III) and Iridium(III) Supported by
 4,4‘-Di-tert-butyl-2,2‘-bipyridyl
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              6338
_journal_paper_doi               10.1021/om7006216
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C45 H54 Ir N2'
_chemical_formula_weight         815.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                115.7260(10)
_cell_angle_beta                 106.2750(10)
_cell_angle_gamma                91.4960(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9687(9)
_cell_length_b                   13.7906(10)
_cell_length_c                   13.8682(10)
_cell_measurement_reflns_used    5717
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.8197
_cell_measurement_theta_min      2.3135
_cell_volume                     1950.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12313
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    3.455
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.944
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6771
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0359
_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)+(0.0584P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                6072
_reflns_number_total             6771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7006216-file004.cif
_cod_data_source_block           kevin48
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P-1
_cod_database_code               4073779
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
Ir1 Ir 0.623583(15) 0.229583(14) 0.222516(15) 0.01972(8) Uani 1 1 d .
N1 N 0.4915(4) 0.2823(3) 0.1249(3) 0.0228(9) Uani 1 1 d .
N2 N 0.4608(4) 0.1694(3) 0.2292(3) 0.0218(9) Uani 1 1 d .
C1 C 0.5080(5) 0.3274(5) 0.0601(5) 0.0306(12) Uani 1 1 d .
H1A H 0.5851 0.3364 0.0556 0.037 Uiso 1 1 calc R
C2 C 0.4210(5) 0.3607(5) 0.0006(5) 0.0348(13) Uani 1 1 d .
H2A H 0.4384 0.3917 -0.0439 0.042 Uiso 1 1 calc R
C3 C 0.3063(5) 0.3497(4) 0.0046(4) 0.0302(12) Uani 1 1 d .
C4 C 0.2893(4) 0.3010(4) 0.0701(4) 0.0262(11) Uani 1 1 d .
H4A H 0.2131 0.2919 0.0763 0.031 Uiso 1 1 calc R
C5 C 0.3796(4) 0.2659(4) 0.1257(4) 0.0219(10) Uani 1 1 d .
C6 C 0.3632(4) 0.2031(4) 0.1861(4) 0.0220(10) Uani 1 1 d .
C7 C 0.2542(4) 0.1766(4) 0.1946(4) 0.0255(11) Uani 1 1 d .
H7A H 0.1870 0.2018 0.1637 0.031 Uiso 1 1 calc R
C8 C 0.2436(5) 0.1133(5) 0.2481(5) 0.0330(13) Uani 1 1 d .
C9 C 0.3450(5) 0.0785(4) 0.2904(5) 0.0288(12) Uani 1 1 d .
H9A H 0.3421 0.0345 0.3270 0.035 Uiso 1 1 calc R
C10 C 0.4498(5) 0.1079(4) 0.2793(4) 0.0251(11) Uani 1 1 d .
H10A H 0.5180 0.0830 0.3090 0.030 Uiso 1 1 calc R
C11 C 0.2061(5) 0.3931(5) -0.0531(5) 0.0380(14) Uani 1 1 d .
C12 C 0.2281(7) 0.4056(9) -0.1491(8) 0.077(3) Uani 1 1 d .
H12A H 0.2347 0.3344 -0.2061 0.116 Uiso 1 1 calc R
H12B H 0.3017 0.4568 -0.1203 0.116 Uiso 1 1 calc R
H12C H 0.1623 0.4336 -0.1833 0.116 Uiso 1 1 calc R
C13 C 0.0879(6) 0.3181(6) -0.1001(6) 0.0529(18) Uani 1 1 d .
H13A H 0.0917 0.2462 -0.1579 0.079 Uiso 1 1 calc R
H13B H 0.0256 0.3495 -0.1340 0.079 Uiso 1 1 calc R
H13C H 0.0702 0.3103 -0.0387 0.079 Uiso 1 1 calc R
C14 C 0.1939(9) 0.5034(7) 0.0360(8) 0.083(3) Uani 1 1 d .
H14A H 0.2686 0.5542 0.0691 0.124 Uiso 1 1 calc R
H14B H 0.1743 0.4935 0.0956 0.124 Uiso 1 1 calc R
H14C H 0.1309 0.5330 0.0005 0.124 Uiso 1 1 calc R
C15 C 0.1260(6) 0.0845(5) 0.2602(7) 0.054(2) Uani 1 1 d D
C16A C 0.1226(11) -0.0022(10) 0.2961(11) 0.039(3) Uiso 0.50 1 d PD
C17A C 0.0787(14) 0.1857(12) 0.3208(14) 0.062(4) Uiso 0.50 1 d PD
C18A C 0.0287(14) 0.0229(13) 0.1263(12) 0.062(4) Uiso 0.50 1 d PD
C16B C 0.1617(14) 0.1346(13) 0.4026(12) 0.064(4) Uiso 0.50 1 d PD
C17B C 0.0382(14) 0.1507(12) 0.2462(14) 0.060(4) Uiso 0.50 1 d PD
C18B C 0.1027(13) -0.0311(11) 0.2314(13) 0.051(3) Uiso 0.50 1 d PD
C21 C 0.7294(4) 0.1541(4) 0.2995(4) 0.0233(11) Uani 1 1 d .
C22 C 0.7186(5) 0.0386(4) 0.2370(5) 0.0296(12) Uani 1 1 d .
C23 C 0.7835(5) -0.0197(5) 0.2863(5) 0.0383(14) Uani 1 1 d .
H23A H 0.7759 -0.0965 0.2429 0.046 Uiso 1 1 calc R
C24 C 0.8590(5) 0.0309(5) 0.3969(5) 0.0399(14) Uani 1 1 d .
H24A H 0.9004 -0.0112 0.4295 0.048 Uiso 1 1 calc R
C25 C 0.8737(5) 0.1418(5) 0.4589(5) 0.0353(13) Uani 1 1 d .
C26 C 0.8123(5) 0.2023(5) 0.4097(4) 0.0277(12) Uani 1 1 d .
H26A H 0.8269 0.2796 0.4525 0.033 Uiso 1 1 calc R
C27 C 0.6383(5) -0.0206(5) 0.1168(5) 0.0448(16) Uani 1 1 d .
H27A H 0.6415 -0.0989 0.0868 0.067 Uiso 1 1 calc R
H27B H 0.6637 0.0076 0.0712 0.067 Uiso 1 1 calc R
H27C H 0.5571 -0.0093 0.1140 0.067 Uiso 1 1 calc R
C28 C 0.9564(6) 0.2006(6) 0.5797(5) 0.0546(18) Uani 1 1 d .
H28A H 0.9929 0.1474 0.6017 0.082 Uiso 1 1 calc R
H28B H 0.9118 0.2396 0.6301 0.082 Uiso 1 1 calc R
H28C H 1.0181 0.2530 0.5856 0.082 Uiso 1 1 calc R
C31 C 0.6329(5) 0.3642(5) 0.3620(5) 0.0381(14) Uani 1 1 d .
C32 C 0.6470(6) 0.4719(5) 0.3809(7) 0.055(2) Uani 1 1 d .
C33 C 0.6544(6) 0.5600(7) 0.4982(7) 0.066(2) Uani 1 1 d .
H33A H 0.6651 0.6353 0.5167 0.080 Uiso 1 1 calc R
C34 C 0.6454(7) 0.5277(6) 0.5737(7) 0.060(2) Uani 1 1 d .
H34A H 0.6475 0.5842 0.6450 0.072 Uiso 1 1 calc R
C35 C 0.6337(7) 0.4254(7) 0.5625(6) 0.062(2) Uani 1 1 d .
C36 C 0.6242(6) 0.3479(7) 0.4600(5) 0.062(2) Uani 1 1 d .
H36A H 0.6104 0.2745 0.4473 0.074 Uiso 1 1 calc R
C37 C 0.6529(8) 0.5076(7) 0.3020(8) 0.071(2) Uani 1 1 d .
H37A H 0.6475 0.4445 0.2303 0.107 Uiso 1 1 calc R
H37B H 0.7281 0.5567 0.3306 0.107 Uiso 1 1 calc R
H37C H 0.5874 0.5466 0.2899 0.107 Uiso 1 1 calc R
C38 C 0.6285(9) 0.3980(8) 0.6561(7) 0.084(3) Uani 1 1 d .
H38A H 0.6197 0.3187 0.6280 0.126 Uiso 1 1 calc R
H38B H 0.5609 0.4242 0.6803 0.126 Uiso 1 1 calc R
H38C H 0.7015 0.4335 0.7204 0.126 Uiso 1 1 calc R
C41 C 0.7687(4) 0.2834(4) 0.1980(4) 0.0237(11) Uani 1 1 d .
C42 C 0.7820(5) 0.2388(4) 0.0911(4) 0.0304(12) Uani 1 1 d .
C43 C 0.8811(5) 0.2813(5) 0.0767(5) 0.0366(13) Uani 1 1 d .
H43A H 0.8889 0.2518 0.0034 0.044 Uiso 1 1 calc R
C44 C 0.9662(5) 0.3638(5) 0.1654(5) 0.0344(13) Uani 1 1 d .
H44A H 1.0319 0.3910 0.1531 0.041 Uiso 1 1 calc R
C45 C 0.9571(5) 0.4079(4) 0.2730(5) 0.0326(13) Uani 1 1 d .
C46 C 0.8615(4) 0.3654(4) 0.2867(5) 0.0284(12) Uani 1 1 d .
H46A H 0.8573 0.3933 0.3611 0.034 Uiso 1 1 calc R
C47 C 0.6968(6) 0.1436(5) -0.0086(5) 0.0454(16) Uani 1 1 d .
H47A H 0.7213 0.1250 -0.0754 0.068 Uiso 1 1 calc R
H47B H 0.6176 0.1627 -0.0225 0.068 Uiso 1 1 calc R
H47C H 0.6958 0.0808 0.0070 0.068 Uiso 1 1 calc R
C48 C 1.0496(6) 0.4988(6) 0.3725(6) 0.0516(18) Uani 1 1 d .
H48A H 1.1110 0.5188 0.3470 0.077 Uiso 1 1 calc R
H48B H 1.0850 0.4743 0.4291 0.077 Uiso 1 1 calc R
H48C H 1.0128 0.5624 0.4061 0.077 Uiso 1 1 calc R
C1S C 0.5921(9) 0.0036(13) 0.4651(12) 0.092(4) Uani 1 1 d .
H1SA H 0.6587 0.0056 0.4411 0.111 Uiso 1 1 calc R
C2S C 0.5040(13) -0.0908(11) 0.4008(11) 0.106(4) Uani 1 1 d .
H2SA H 0.5070 -0.1508 0.3338 0.127 Uiso 1 1 calc R
C3S C 0.4120(11) -0.0875(11) 0.4451(12) 0.098(4) Uani 1 1 d .
H3SA H 0.3504 -0.1489 0.4081 0.118 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'
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
C31 Ir1 C21 97.0(2) .
C31 Ir1 C41 96.4(2) .
C21 Ir1 C41 87.3(2) .
C31 Ir1 N1 89.9(2) .
C21 Ir1 N1 169.96(17) .
C41 Ir1 N1 99.21(18) .
C31 Ir1 N2 87.39(19) .
C21 Ir1 N2 97.38(18) .
C41 Ir1 N2 173.58(17) .
N1 Ir1 N2 75.56(15) .
C1 N1 C5 116.7(4) .
C1 N1 Ir1 126.3(3) .
C5 N1 Ir1 117.0(3) .
C10 N2 C6 117.7(4) .
C10 N2 Ir1 125.2(3) .
C6 N2 Ir1 116.9(3) .
N1 C1 C2 123.9(5) .
C1 C2 C3 120.4(5) .
C4 C3 C2 115.4(5) .
C4 C3 C11 121.3(5) .
C2 C3 C11 123.2(5) .
C5 C4 C3 121.7(5) .
N1 C5 C4 121.7(5) .
N1 C5 C6 114.6(4) .
C4 C5 C6 123.7(4) .
N2 C6 C7 121.8(5) .
N2 C6 C5 115.1(4) .
C7 C6 C5 123.0(5) .
C8 C7 C6 120.2(5) .
C9 C8 C7 116.8(5) .
C9 C8 C15 121.8(5) .
C7 C8 C15 121.4(5) .
C10 C9 C8 119.9(5) .
N2 C10 C9 123.5(5) .
C12 C11 C13 107.8(6) .
C12 C11 C14 110.1(7) .
C13 C11 C14 106.8(6) .
C12 C11 C3 112.2(5) .
C13 C11 C3 111.7(5) .
C14 C11 C3 108.2(5) .
C17B C15 C18B 125.8(10) .
C17B C15 C16A 128.6(9) .
C18B C15 C16A 30.1(6) .
C17B C15 C17A 35.6(7) .
C18B C15 C17A 136.3(9) .
C16A C15 C17A 117.2(9) .
C17B C15 C8 116.6(8) .
C18B C15 C8 111.0(7) .
C16A C15 C8 114.5(7) .
C17A C15 C8 111.2(8) .
C17B C15 C16B 97.4(9) .
C18B C15 C16B 96.9(9) .
C16A C15 C16B 66.8(8) .
C17A C15 C16B 63.5(9) .
C8 C15 C16B 101.9(7) .
C17B C15 C18A 69.2(9) .
C18B C15 C18A 74.6(9) .
C16A C15 C18A 102.3(8) .
C17A C15 C18A 104.6(10) .
C8 C15 C18A 105.3(7) .
C16B C15 C18A 152.8(9) .
C18B C16A C15 73.4(14) .
C18B C16A C16B 135.7(18) .
C15 C16A C16B 62.4(7) .
C17B C17A C15 68.1(13) .
C17B C17A C16B 128.5(18) .
C15 C17A C16B 63.9(8) .
C15 C18A C17B 48.4(6) .
C15 C18A C18B 47.0(6) .
C17B C18A C18B 87.7(9) .
C17A C16B C15 52.6(7) .
C17A C16B C16A 95.1(9) .
C15 C16B C16A 50.7(6) .
C17A C17B C15 76.3(15) .
C17A C17B C18A 138.0(18) .
C15 C17B C18A 62.3(8) .
C16A C18B C15 76.5(14) .
C16A C18B C18A 129.4(18) .
C15 C18B C18A 58.3(7) .
C26 C21 C22 115.4(5) .
C26 C21 Ir1 127.6(4) .
C22 C21 Ir1 117.0(4) .
C23 C22 C21 120.3(5) .
C23 C22 C27 119.5(5) .
C21 C22 C27 120.2(5) .
C24 C23 C22 121.9(5) .
C25 C24 C23 119.5(6) .
C24 C25 C26 119.5(5) .
C24 C25 C28 121.3(6) .
C26 C25 C28 119.2(6) .
C25 C26 C21 123.2(5) .
C32 C31 C36 115.6(7) .
C32 C31 Ir1 128.4(5) .
C36 C31 Ir1 116.1(5) .
C31 C32 C37 126.3(7) .
C31 C32 C33 117.2(8) .
C37 C32 C33 116.5(7) .
C34 C33 C32 117.6(8) .
C33 C34 C35 128.7(8) .
C36 C35 C34 114.2(8) .
C36 C35 C38 121.5(8) .
C34 C35 C38 124.3(8) .
C35 C36 C31 126.6(8) .
C42 C41 C46 116.1(5) .
C42 C41 Ir1 121.1(4) .
C46 C41 Ir1 122.7(4) .
C41 C42 C43 119.4(5) .
C41 C42 C47 122.0(5) .
C43 C42 C47 118.5(5) .
C44 C43 C42 121.7(5) .
C43 C44 C45 120.3(5) .
C46 C45 C44 117.8(5) .
C46 C45 C48 120.8(5) .
C44 C45 C48 121.5(5) .
C45 C46 C41 124.6(5) .
C3S C1S C2S 124.1(10) 2_656
C3S C2S C1S 113.6(12) .
C1S C3S C2S 122.2(12) 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 C31 1.988(6) .
Ir1 C21 2.026(5) .
Ir1 C41 2.041(5) .
Ir1 N1 2.138(4) .
Ir1 N2 2.139(4) .
N1 C1 1.347(7) .
N1 C5 1.356(6) .
N2 C10 1.334(6) .
N2 C6 1.347(6) .
C1 C2 1.360(8) .
C2 C3 1.397(8) .
C3 C4 1.394(7) .
C3 C11 1.533(8) .
C4 C5 1.372(7) .
C5 C6 1.485(7) .
C6 C7 1.395(7) .
C7 C8 1.392(8) .
C8 C9 1.386(8) .
C8 C15 1.526(7) .
C9 C10 1.378(7) .
C11 C12 1.504(9) .
C11 C13 1.523(9) .
C11 C14 1.531(10) .
C15 C17B 1.437(15) .
C15 C18B 1.463(14) .
C15 C16A 1.484(13) .
C15 C17A 1.504(15) .
C15 C16B 1.699(15) .
C15 C18A 1.701(15) .
C16A C18B 0.765(15) .
C16A C16B 1.763(19) .
C17A C17B 0.901(18) .
C17A C16B 1.69(2) .
C18A C17B 1.80(2) .
C18A C18B 1.93(2) .
C21 C26 1.413(7) .
C21 C22 1.426(7) .
C22 C23 1.390(8) .
C22 C27 1.499(8) .
C23 C24 1.384(9) .
C24 C25 1.368(9) .
C25 C26 1.394(8) .
C25 C28 1.515(8) .
C31 C32 1.387(9) .
C31 C36 1.501(10) .
C32 C37 1.398(12) .
C32 C33 1.526(11) .
C33 C34 1.332(11) .
C34 C35 1.349(11) .
C35 C36 1.327(9) .
C35 C38 1.517(12) .
C41 C42 1.396(7) .
C41 C46 1.409(7) .
C42 C43 1.411(8) .
C42 C47 1.496(8) .
C43 C44 1.367(8) .
C44 C45 1.385(8) .
C45 C46 1.368(7) .
C45 C48 1.507(8) .
C1S C3S 1.296(16) 2_656
C1S C2S 1.412(16) .
C2S C3S 1.395(16) .
C3S C1S 1.296(16) 2_656
