#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:10:08 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178638 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/49/4074975.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_4074975
loop_
_publ_author_name
'Sykes, Alison Cartwright'
'White, Peter'
'Brookhart, Maurice'
_publ_section_title
;
 Reactions of Anilines and Benzamides with a Fourteen-Electron Iridium(I)
 Bis(Phosphinite) Complex: N-H Oxidative Addition versus Lewis Base
 Coordination.
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1664
_journal_page_last               1675
_journal_paper_doi               10.1021/om051070n
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C40 H54 Ir O2 P3'
_chemical_formula_sum            'C40 H54 Ir O2 P3'
_chemical_formula_weight         851.94
_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                 111.843(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2931(13)
_cell_length_b                   17.1006(15)
_cell_length_c                   17.8063(18)
_cell_measurement_reflns_used    1022
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.68
_cell_volume                     3757.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60305
_diffrn_reflns_theta_full        27.07
_diffrn_reflns_theta_max         27.07
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    3.714
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.464
_refine_diff_density_min         -1.918
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         8242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.323
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0507
_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)+(0.0000P)²+17.3679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                7479
_reflns_number_total             8242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om051070nsi20051215_121938.cif
_cod_data_source_block           c05225
_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               4074975
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 0.789564(15) 0.754910(10) 0.080058(12) 0.01404(7) Uani 1 1 d .
P1 P 0.95032(11) 0.78131(7) 0.06408(9) 0.0156(3) Uani 1 1 d .
P2 P 0.61920(11) 0.78370(7) 0.07869(9) 0.0156(3) Uani 1 1 d .
P3 P 0.80836(11) 0.62228(7) 0.11431(9) 0.0147(3) Uani 1 1 d .
C2 C 1.0804(4) 0.7881(3) 0.1559(3) 0.0181(11) Uani 1 1 d .
C3 C 1.0446(5) 0.8019(4) 0.2277(4) 0.0274(13) Uani 1 1 d .
H3A H 0.9904 0.7627 0.2267 0.041 Uiso 1 1 calc R
H3B H 1.0131 0.8543 0.2235 0.041 Uiso 1 1 calc R
H3C H 1.1075 0.7975 0.2785 0.041 Uiso 1 1 calc R
C4 C 1.1493(5) 0.7136(3) 0.1691(4) 0.0229(12) Uani 1 1 d .
H4A H 1.2051 0.7141 0.2238 0.034 Uiso 1 1 calc R
H4B H 1.1840 0.7116 0.1293 0.034 Uiso 1 1 calc R
H4C H 1.1028 0.6676 0.1627 0.034 Uiso 1 1 calc R
C5 C 1.1523(5) 0.8579(3) 0.1526(4) 0.0285(14) Uani 1 1 d .
H5A H 1.2174 0.8591 0.2021 0.043 Uiso 1 1 calc R
H5B H 1.1118 0.9067 0.1479 0.043 Uiso 1 1 calc R
H5C H 1.1733 0.8523 0.1056 0.043 Uiso 1 1 calc R
C6 C 0.9760(4) 0.7418(3) -0.0246(3) 0.0214(11) Uani 1 1 d .
C7 C 0.9892(5) 0.6522(3) -0.0207(4) 0.0256(13) Uani 1 1 d .
H7A H 1.0001 0.6336 -0.0692 0.038 Uiso 1 1 calc R
H7B H 0.9238 0.6280 -0.0179 0.038 Uiso 1 1 calc R
H7C H 1.0520 0.6379 0.0275 0.038 Uiso 1 1 calc R
C8 C 1.0747(5) 0.7791(4) -0.0366(4) 0.0283(14) Uani 1 1 d .
H8A H 1.1409 0.7660 0.0094 0.042 Uiso 1 1 calc R
H8B H 1.0658 0.8361 -0.0404 0.042 Uiso 1 1 calc R
H8C H 1.0801 0.7591 -0.0866 0.042 Uiso 1 1 calc R
C9 C 0.8740(5) 0.7621(4) -0.0995(4) 0.0342(15) Uani 1 1 d .
H9A H 0.8789 0.7374 -0.1476 0.051 Uiso 1 1 calc R
H9B H 0.8690 0.8190 -0.1070 0.051 Uiso 1 1 calc R
H9C H 0.8093 0.7430 -0.0913 0.051 Uiso 1 1 calc R
O10 O 0.9450(3) 0.8746(2) 0.0373(3) 0.0225(9) Uani 1 1 d .
C11 C 0.8484(4) 0.9115(3) 0.0254(3) 0.0175(11) Uani 1 1 d .
C12 C 0.8362(4) 0.9883(3) -0.0028(3) 0.0197(11) Uani 1 1 d .
H12 H 0.8927 1.0141 -0.0135 0.024 Uiso 1 1 calc R
C13 C 0.7392(5) 1.0257(3) -0.0148(3) 0.0206(12) Uani 1 1 d .
H13 H 0.7288 1.0779 -0.0344 0.025 Uiso 1 1 calc R
C14 C 0.6567(5) 0.9883(3) 0.0014(4) 0.0220(12) Uani 1 1 d .
H14 H 0.5900 1.0140 -0.0070 0.026 Uiso 1 1 calc R
C15 C 0.6750(4) 0.9124(3) 0.0301(3) 0.0180(11) Uani 1 1 d .
C16 C 0.7699(4) 0.8696(3) 0.0428(3) 0.0166(11) Uani 1 1 d .
O17 O 0.5936(3) 0.8756(2) 0.0475(3) 0.0228(9) Uani 1 1 d .
C18 C 0.4979(4) 0.7402(3) -0.0028(3) 0.0208(11) Uani 1 1 d .
C19 C 0.5127(5) 0.7602(4) -0.0822(3) 0.0294(13) Uani 1 1 d .
H19A H 0.5811 0.7380 -0.0813 0.044 Uiso 1 1 calc R
H19B H 0.5141 0.8172 -0.0881 0.044 Uiso 1 1 calc R
H19C H 0.4524 0.7383 -0.1280 0.044 Uiso 1 1 calc R
C20 C 0.3901(4) 0.7764(3) -0.0073(4) 0.0251(13) Uani 1 1 d .
H20A H 0.3313 0.7570 -0.0555 0.038 Uiso 1 1 calc R
H20B H 0.3944 0.8335 -0.0104 0.038 Uiso 1 1 calc R
H20C H 0.3760 0.7621 0.0411 0.038 Uiso 1 1 calc R
C21 C 0.4944(5) 0.6511(3) 0.0047(4) 0.0249(13) Uani 1 1 d .
H21A H 0.4830 0.6376 0.0544 0.037 Uiso 1 1 calc R
H21B H 0.5632 0.6287 0.0066 0.037 Uiso 1 1 calc R
H21C H 0.4349 0.6300 -0.0421 0.037 Uiso 1 1 calc R
C22 C 0.5931(5) 0.7959(3) 0.1750(4) 0.0238(12) Uani 1 1 d .
C23 C 0.5202(6) 0.8660(4) 0.1743(5) 0.0396(17) Uani 1 1 d .
H23A H 0.4503 0.8604 0.1293 0.059 Uiso 1 1 calc R
H23B H 0.5553 0.9145 0.1677 0.059 Uiso 1 1 calc R
H23C H 0.5085 0.8677 0.2254 0.059 Uiso 1 1 calc R
C24 C 0.5442(5) 0.7219(4) 0.1973(4) 0.0313(14) Uani 1 1 d .
H24A H 0.5532 0.7243 0.2545 0.047 Uiso 1 1 calc R
H24B H 0.5813 0.6756 0.1880 0.047 Uiso 1 1 calc R
H24C H 0.4668 0.7188 0.1637 0.047 Uiso 1 1 calc R
C25 C 0.7065(5) 0.8124(4) 0.2417(4) 0.0365(16) Uani 1 1 d .
H25A H 0.7358 0.8612 0.2292 0.055 Uiso 1 1 calc R
H25B H 0.7557 0.7691 0.2435 0.055 Uiso 1 1 calc R
H25C H 0.6994 0.8172 0.2943 0.055 Uiso 1 1 calc R
C26 C 0.7367(4) 0.5803(3) 0.1770(3) 0.0195(12) Uani 1 1 d .
C27 C 0.7664(5) 0.6043(4) 0.2579(4) 0.0318(15) Uani 1 1 d .
H27 H 0.8208 0.6431 0.2789 0.038 Uiso 1 1 calc R
C28 C 0.7179(6) 0.5724(5) 0.3078(4) 0.0401(17) Uani 1 1 d .
H28 H 0.7393 0.5893 0.3623 0.048 Uiso 1 1 calc R
C29 C 0.6386(6) 0.5163(4) 0.2781(5) 0.0436(19) Uani 1 1 d .
H29 H 0.6069 0.4933 0.3127 0.052 Uiso 1 1 calc R
C30 C 0.6052(5) 0.4934(4) 0.1982(5) 0.0380(17) Uani 1 1 d .
H30 H 0.5487 0.4560 0.1772 0.046 Uiso 1 1 calc R
C31 C 0.6545(5) 0.5252(3) 0.1479(4) 0.0243(13) Uani 1 1 d .
H31 H 0.6314 0.5088 0.0931 0.029 Uiso 1 1 calc R
C32 C 0.7618(4) 0.5550(3) 0.0265(3) 0.0166(11) Uani 1 1 d .
C33 C 0.7179(4) 0.5856(3) -0.0506(3) 0.0201(12) Uani 1 1 d .
H33 H 0.7116 0.6407 -0.0576 0.024 Uiso 1 1 calc R
C34 C 0.6827(5) 0.5370(3) -0.1183(4) 0.0257(13) Uani 1 1 d .
H34 H 0.6524 0.5589 -0.1711 0.031 Uiso 1 1 calc R
C35 C 0.6922(5) 0.4565(3) -0.1081(4) 0.0286(14) Uani 1 1 d .
H35 H 0.6688 0.4231 -0.1540 0.034 Uiso 1 1 calc R
C36 C 0.7353(5) 0.4251(3) -0.0315(4) 0.0255(14) Uani 1 1 d .
H36 H 0.7409 0.3700 -0.0246 0.031 Uiso 1 1 calc R
C37 C 0.7703(4) 0.4731(3) 0.0350(4) 0.0203(12) Uani 1 1 d .
H37 H 0.8006 0.4508 0.0876 0.024 Uiso 1 1 calc R
C38 C 0.9456(4) 0.5814(3) 0.1726(3) 0.0171(11) Uani 1 1 d .
C39 C 0.9979(4) 0.5291(3) 0.1400(4) 0.0225(12) Uani 1 1 d .
H39 H 0.9634 0.5126 0.0855 0.027 Uiso 1 1 calc R
C40 C 1.1007(5) 0.5004(3) 0.1863(4) 0.0312(15) Uani 1 1 d .
H40 H 1.1354 0.4646 0.1628 0.037 Uiso 1 1 calc R
C41 C 1.1525(5) 0.5235(3) 0.2660(4) 0.0286(14) Uani 1 1 d .
H41 H 1.2221 0.5034 0.2974 0.034 Uiso 1 1 calc R
C42 C 1.1017(5) 0.5764(4) 0.2999(4) 0.0297(14) Uani 1 1 d .
H42 H 1.1362 0.5926 0.3545 0.036 Uiso 1 1 calc R
C43 C 0.9996(5) 0.6051(3) 0.2526(4) 0.0223(12) Uani 1 1 d .
H43 H 0.9658 0.6420 0.2755 0.027 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'
O O 0.0106 0.0060 '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'
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
C16 Ir1 P1 77.63(15)
C16 Ir1 P2 77.67(15)
P1 Ir1 P2 155.30(4)
C16 Ir1 P3 176.59(15)
P1 Ir1 P3 102.02(5)
P2 Ir1 P3 102.64(5)
O10 P1 C6 96.2(2)
O10 P1 C2 96.7(2)
C6 P1 C2 111.0(2)
O10 P1 Ir1 106.36(14)
C6 P1 Ir1 120.33(18)
C2 P1 Ir1 119.83(18)
O17 P2 C18 96.1(2)
O17 P2 C22 96.6(2)
C18 P2 C22 110.6(3)
O17 P2 Ir1 106.50(14)
C18 P2 Ir1 118.76(18)
C22 P2 Ir1 121.76(19)
C32 P3 C26 100.5(3)
C32 P3 C38 100.8(2)
C26 P3 C38 97.8(2)
C32 P3 Ir1 114.39(18)
C26 P3 Ir1 120.12(18)
C38 P3 Ir1 119.71(17)
C4 C2 C3 110.6(5)
C4 C2 C5 107.7(4)
C3 C2 C5 107.4(5)
C4 C2 P1 112.6(4)
C3 C2 P1 105.2(4)
C5 C2 P1 113.2(4)
C7 C6 C8 109.3(5)
C7 C6 C9 108.2(5)
C8 C6 C9 107.8(5)
C7 C6 P1 112.1(4)
C8 C6 P1 113.6(4)
C9 C6 P1 105.7(4)
C11 O10 P1 115.1(3)
O10 C11 C16 117.6(4)
O10 C11 C12 117.7(5)
C16 C11 C12 124.6(5)
C13 C12 C11 117.9(5)
C12 C13 C14 121.2(5)
C15 C14 C13 117.7(5)
O17 C15 C14 117.7(5)
O17 C15 C16 117.4(5)
C14 C15 C16 124.9(5)
C11 C16 C15 113.6(4)
C11 C16 Ir1 123.1(4)
C15 C16 Ir1 123.3(4)
C15 O17 P2 115.1(3)
C21 C18 C20 110.4(4)
C21 C18 C19 108.7(5)
C20 C18 C19 107.4(5)
C21 C18 P2 111.9(4)
C20 C18 P2 113.4(4)
C19 C18 P2 104.8(4)
C23 C22 C24 108.5(5)
C23 C22 C25 107.1(5)
C24 C22 C25 109.4(5)
C23 C22 P2 114.1(4)
C24 C22 P2 112.4(4)
C25 C22 P2 105.0(4)
C31 C26 C27 117.5(5)
C31 C26 P3 123.0(5)
C27 C26 P3 119.4(4)
C28 C27 C26 121.4(6)
C29 C28 C27 120.0(7)
C28 C29 C30 120.0(6)
C29 C30 C31 120.0(6)
C26 C31 C30 121.0(6)
C33 C32 C37 118.2(5)
C33 C32 P3 119.2(4)
C37 C32 P3 122.6(4)
C32 C33 C34 121.1(5)
C35 C34 C33 119.5(6)
C36 C35 C34 120.1(5)
C37 C36 C35 120.3(5)
C36 C37 C32 120.9(5)
C39 C38 C43 117.8(5)
C39 C38 P3 123.2(4)
C43 C38 P3 118.9(4)
C38 C39 C40 121.0(6)
C41 C40 C39 120.5(6)
C40 C41 C42 119.5(5)
C43 C42 C41 119.2(6)
C42 C43 C38 122.0(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ir1 C16 2.056(5)
Ir1 P1 2.3030(14)
Ir1 P2 2.3088(14)
Ir1 P3 2.3378(13)
P1 O10 1.659(4)
P1 C6 1.863(6)
P1 C2 1.890(5)
P2 O17 1.660(4)
P2 C18 1.876(6)
P2 C22 1.884(6)
P3 C32 1.853(5)
P3 C26 1.861(6)
P3 C38 1.866(5)
C2 C4 1.535(7)
C2 C3 1.539(8)
C2 C5 1.544(7)
C6 C7 1.540(8)
C6 C8 1.544(7)
C6 C9 1.547(8)
O10 C11 1.374(6)
C11 C16 1.393(7)
C11 C12 1.394(7)
C12 C13 1.384(8)
C13 C14 1.388(8)
C14 C15 1.384(7)
C15 O17 1.383(6)
C15 C16 1.401(7)
C18 C21 1.531(7)
C18 C20 1.535(7)
C18 C19 1.538(8)
C22 C23 1.538(8)
C22 C24 1.541(8)
C22 C25 1.559(8)
C26 C31 1.388(8)
C26 C27 1.406(9)
C27 C28 1.388(9)
C28 C29 1.377(10)
C29 C30 1.381(11)
C30 C31 1.401(8)
C32 C33 1.380(8)
C32 C37 1.407(7)
C33 C34 1.394(8)
C34 C35 1.388(8)
C35 C36 1.377(9)
C36 C37 1.372(8)
C38 C39 1.385(7)
C38 C43 1.396(8)
C39 C40 1.396(8)
C40 C41 1.385(9)
C41 C42 1.394(9)
C42 C43 1.393(8)
