#------------------------------------------------------------------------------
#$Date: 2015-09-08 11:27:23 +0300 (Tue, 08 Sep 2015) $
#$Revision: 155207 $
#$URL: svn://www.crystallography.net/cod/cif/1/52/12/1521275.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_1521275
loop_
_publ_author_name
'Rimoldi, M.'
'Fodor, D.'
'van Bokhoven, J. A.'
'Mezzetti, A.'
_publ_section_title
;
 Catalytic hydrogenation of liquid alkenes with a silica-grafted hydride
 pincer iridium(iii) complex: support for a heterogeneous mechanism
;
_journal_issue                   9
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              4575
_journal_paper_doi               10.1039/C5CY00837A
_journal_volume                  5
_journal_year                    2015
_chemical_formula_sum            'C24 H43 Ir O2 P2'
_chemical_formula_weight         617.72
_chemical_name_common            '[Ir(C2H4)(POCOP)] (6)'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-03-19 deposited with the CCDC.
2015-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                100.381(2)
_cell_angle_beta                 95.958(2)
_cell_angle_gamma                103.944(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5336(10)
_cell_length_b                   11.7835(14)
_cell_length_c                   13.3762(15)
_cell_measurement_reflns_used    6865
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.49
_cell_volume                     1268.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19459
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.153
_diffrn_reflns_theta_min         1.566
_exptl_absorpt_coefficient_mu    5.405
_exptl_absorpt_correction_T_max  0.8546
_exptl_absorpt_correction_T_min  0.7035
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2004/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.308
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         7478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0179P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6577
_reflns_number_total             7478
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cy00837a2.cif
_cod_data_source_block           final3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1521275--1521276.cif.
;
_cod_database_code               1521275
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.703
_shelx_estimated_absorpt_t_max   0.855
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ir1 Ir 0.96253(2) 0.77859(2) 0.22414(2) 0.00921(3) Uani 1 1 d . .
P1 P 1.17006(9) 0.94933(6) 0.25277(5) 0.01032(14) Uani 1 1 d . .
P2 P 0.80944(9) 0.60515(6) 0.25508(5) 0.01049(14) Uani 1 1 d . .
O2 O 0.9095(2) 0.58017(17) 0.35839(15) 0.0135(4) Uani 1 1 d . .
O1 O 1.2906(2) 0.94985(17) 0.35849(14) 0.0126(4) Uani 1 1 d . .
C1 C 1.0965(3) 0.7654(2) 0.3543(2) 0.0116(5) Uani 1 1 d . .
C2 C 1.2391(3) 0.8529(2) 0.4036(2) 0.0109(5) Uani 1 1 d . .
C3 C 1.3316(3) 0.8468(3) 0.4926(2) 0.0131(5) Uani 1 1 d . .
H3A H 1.4269 0.9089 0.5238 0.016 Uiso 1 1 calc R U
C4 C 1.2817(3) 0.7476(3) 0.5353(2) 0.0144(6) Uani 1 1 d . .
H4A H 1.3446 0.7414 0.5961 0.017 Uiso 1 1 calc R U
C5 C 1.1411(4) 0.6568(3) 0.4908(2) 0.0147(6) Uani 1 1 d . .
H5A H 1.1073 0.5889 0.5202 0.018 Uiso 1 1 calc R U
C6 C 1.0522(3) 0.6686(2) 0.4025(2) 0.0121(5) Uani 1 1 d . .
C7 C 1.3280(3) 0.9666(2) 0.1645(2) 0.0122(5) Uani 1 1 d . .
C8 C 1.3329(4) 0.8385(3) 0.1190(2) 0.0202(7) Uani 1 1 d . .
H8A H 1.4134 0.8406 0.0717 0.030 Uiso 1 1 calc R U
H8B H 1.2248 0.7925 0.0816 0.030 Uiso 1 1 calc R U
H8C H 1.3635 0.8004 0.1747 0.030 Uiso 1 1 calc R U
C9 C 1.4999(4) 1.0365(3) 0.2218(2) 0.0181(6) Uani 1 1 d . .
H9A H 1.5773 1.0430 0.1726 0.027 Uiso 1 1 calc R U
H9B H 1.5341 0.9941 0.2733 0.027 Uiso 1 1 calc R U
H9C H 1.4975 1.1167 0.2561 0.027 Uiso 1 1 calc R U
C10 C 1.2847(4) 1.0274(3) 0.0771(2) 0.0193(6) Uani 1 1 d . .
H10A H 1.3708 1.0341 0.0337 0.029 Uiso 1 1 calc R U
H10B H 1.2752 1.1075 0.1064 0.029 Uiso 1 1 calc R U
H10C H 1.1805 0.9796 0.0356 0.029 Uiso 1 1 calc R U
C11 C 1.1118(4) 1.0912(3) 0.2958(2) 0.0145(6) Uani 1 1 d . .
C12 C 1.2580(4) 1.2022(3) 0.3306(2) 0.0194(6) Uani 1 1 d . .
H12A H 1.2186 1.2730 0.3520 0.029 Uiso 1 1 calc R U
H12B H 1.3194 1.2127 0.2734 0.029 Uiso 1 1 calc R U
H12C H 1.3293 1.1916 0.3886 0.029 Uiso 1 1 calc R U
C13 C 0.9912(4) 1.1113(3) 0.2119(3) 0.0216(7) Uani 1 1 d . .
H13A H 0.9624 1.1861 0.2362 0.032 Uiso 1 1 calc R U
H13B H 0.8923 1.0444 0.1962 0.032 Uiso 1 1 calc R U
H13C H 1.0417 1.1161 0.1498 0.032 Uiso 1 1 calc R U
C14 C 1.0241(4) 1.0715(3) 0.3885(2) 0.0215(7) Uani 1 1 d . .
H14A H 0.9895 1.1431 0.4156 0.032 Uiso 1 1 calc R U
H14B H 1.0988 1.0564 0.4423 0.032 Uiso 1 1 calc R U
H14C H 0.9280 1.0026 0.3669 0.032 Uiso 1 1 calc R U
C15 C 0.8026(4) 0.4650(3) 0.1618(2) 0.0153(6) Uani 1 1 d . .
C16 C 0.9830(4) 0.4666(3) 0.1574(3) 0.0239(7) Uani 1 1 d . .
H16A H 0.9884 0.3948 0.1093 0.036 Uiso 1 1 calc R U
H16B H 1.0373 0.4680 0.2260 0.036 Uiso 1 1 calc R U
H16C H 1.0379 0.5379 0.1339 0.036 Uiso 1 1 calc R U
C17 C 0.7168(4) 0.3500(3) 0.1935(2) 0.0207(6) Uani 1 1 d . .
H17A H 0.7180 0.2806 0.1410 0.031 Uiso 1 1 calc R U
H17B H 0.6035 0.3500 0.2001 0.031 Uiso 1 1 calc R U
H17C H 0.7739 0.3459 0.2596 0.031 Uiso 1 1 calc R U
C18 C 0.7222(4) 0.4681(3) 0.0548(2) 0.0234(7) Uani 1 1 d . .
H18A H 0.7191 0.3942 0.0063 0.035 Uiso 1 1 calc R U
H18B H 0.7855 0.5369 0.0316 0.035 Uiso 1 1 calc R U
H18C H 0.6105 0.4750 0.0579 0.035 Uiso 1 1 calc R U
C19 C 0.6081(3) 0.6014(3) 0.3013(2) 0.0158(6) Uani 1 1 d . .
C20 C 0.5723(4) 0.5196(3) 0.3784(3) 0.0243(7) Uani 1 1 d . .
H20A H 0.4663 0.5209 0.3999 0.036 Uiso 1 1 calc R U
H20B H 0.6581 0.5481 0.4386 0.036 Uiso 1 1 calc R U
H20C H 0.5696 0.4376 0.3456 0.036 Uiso 1 1 calc R U
C21 C 0.4627(4) 0.5651(3) 0.2136(2) 0.0226(7) Uani 1 1 d . .
H21A H 0.3617 0.5648 0.2425 0.034 Uiso 1 1 calc R U
H21B H 0.4549 0.4849 0.1740 0.034 Uiso 1 1 calc R U
H21C H 0.4787 0.6224 0.1684 0.034 Uiso 1 1 calc R U
C22 C 0.6267(4) 0.7308(3) 0.3583(3) 0.0244(7) Uani 1 1 d . .
H22A H 0.5254 0.7362 0.3850 0.037 Uiso 1 1 calc R U
H22B H 0.6490 0.7848 0.3106 0.037 Uiso 1 1 calc R U
H22C H 0.7174 0.7537 0.4155 0.037 Uiso 1 1 calc R U
C23 C 0.8978(4) 0.8022(3) 0.0688(2) 0.0199(6) Uani 1 1 d . .
H23A H 0.9394 0.8836 0.0562 0.024 Uiso 1 1 calc R U
H23B H 0.9042 0.7378 0.0118 0.024 Uiso 1 1 calc R U
C24 C 0.7569(4) 0.7822(3) 0.1140(2) 0.0192(6) Uani 1 1 d . .
H24A H 0.6741 0.7050 0.0858 0.023 Uiso 1 1 calc R U
H24B H 0.7093 0.8508 0.1302 0.023 Uiso 1 1 calc R U
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'
Ir Ir -1.4442 7.9887 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 Ir1 C23 161.07(11)
C1 Ir1 C24 161.77(11)
C23 Ir1 C24 37.16(11)
C1 Ir1 P2 78.82(8)
C23 Ir1 P2 112.98(9)
C24 Ir1 P2 89.14(8)
C1 Ir1 P1 78.72(8)
C23 Ir1 P1 89.15(9)
C24 Ir1 P1 112.21(8)
P2 Ir1 P1 157.48(3)
O1 P1 C11 99.60(12)
O1 P1 C7 98.44(11)
C11 P1 C7 112.33(13)
O1 P1 Ir1 106.29(7)
C11 P1 Ir1 115.33(9)
C7 P1 Ir1 120.58(9)
O2 P2 C15 99.07(12)
O2 P2 C19 98.82(12)
C15 P2 C19 112.25(14)
O2 P2 Ir1 106.42(7)
C15 P2 Ir1 116.30(10)
C19 P2 Ir1 119.68(10)
C6 O2 P2 114.76(17)
C2 O1 P1 114.90(17)
C2 C1 C6 114.7(2)
C2 C1 Ir1 122.7(2)
C6 C1 Ir1 122.6(2)
C3 C2 O1 118.7(2)
C3 C2 C1 123.9(3)
O1 C2 C1 117.4(2)
C2 C3 C4 118.2(3)
C3 C4 C5 121.3(3)
C6 C5 C4 117.9(3)
C5 C6 O2 118.7(2)
C5 C6 C1 124.0(3)
O2 C6 C1 117.4(2)
C10 C7 C8 109.5(2)
C10 C7 C9 108.4(2)
C8 C7 C9 108.1(2)
C10 C7 P1 113.0(2)
C8 C7 P1 104.99(19)
C9 C7 P1 112.69(19)
C13 C11 C12 110.0(2)
C13 C11 C14 108.4(2)
C12 C11 C14 108.5(2)
C13 C11 P1 110.9(2)
C12 C11 P1 113.9(2)
C14 C11 P1 104.7(2)
C17 C15 C18 109.9(2)
C17 C15 C16 108.8(2)
C18 C15 C16 108.5(3)
C17 C15 P2 114.2(2)
C18 C15 P2 110.0(2)
C16 C15 P2 105.2(2)
C21 C19 C20 108.9(2)
C21 C19 C22 109.1(3)
C20 C19 C22 107.9(2)
C21 C19 P2 113.4(2)
C20 C19 P2 112.8(2)
C22 C19 P2 104.6(2)
C24 C23 Ir1 71.66(17)
C23 C24 Ir1 71.18(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ir1 C1 2.032(3)
Ir1 C23 2.178(3)
Ir1 C24 2.185(3)
Ir1 P2 2.2771(7)
Ir1 P1 2.2793(7)
P1 O1 1.658(2)
P1 C11 1.867(3)
P1 C7 1.881(3)
P2 O2 1.658(2)
P2 C15 1.866(3)
P2 C19 1.879(3)
O2 C6 1.391(3)
O1 C2 1.387(3)
C1 C2 1.401(4)
C1 C6 1.403(4)
C2 C3 1.383(4)
C3 C4 1.388(4)
C4 C5 1.394(4)
C5 C6 1.384(4)
C7 C10 1.534(4)
C7 C8 1.535(4)
C7 C9 1.541(4)
C11 C13 1.531(4)
C11 C12 1.535(4)
C11 C14 1.539(4)
C15 C17 1.531(4)
C15 C18 1.533(4)
C15 C16 1.543(4)
C19 C21 1.536(4)
C19 C20 1.539(4)
C19 C22 1.539(4)
C23 C24 1.390(4)
