#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:11:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178772 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/26/4102622.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_4102622
loop_
_publ_author_name
'Eduardo Sola'
'Alba García-Camprubí'
'José L. Andrés'
'Marta Martín'
'Pablo Plou'
_publ_contact_author_address
;
  Dr. Marta Martín
  Departamento de Química Inorgánica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       martam@unizar.es
_publ_contact_author_fax         '+34 956 761187'
_publ_contact_author_name        'Dr. Marta Martín'
_publ_contact_author_phone       '+34 976 762026'
_publ_section_title
;
 Iridium Compounds with κ-P,P,Si(biPSi) Pincer Ligands: Favoring Reactive
 Structures in Unsaturated Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9111
_journal_page_last               9121
_journal_paper_doi               10.1021/ja102479h
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C31 H36 I Ir P2 Si'
_chemical_formula_weight         817.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 111.8960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8913(3)
_cell_length_b                   22.2515(8)
_cell_length_c                   9.1239(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1486.52(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.936
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17640
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.85
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    5.696
_exptl_absorpt_correction_T_max  0.4270
_exptl_absorpt_correction_T_min  0.3954
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0186
_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)+(0.0192P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0419
_reflns_number_gt                3574
_reflns_number_total             3737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja102479h_si_002_4.cif
_cod_data_source_block           marta62s
_cod_database_code               4102622
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
H1 H 0.249(6) 0.2500 -0.010(5) 0.038(12) Uiso 1 2 d S
Ir1 Ir 0.405572(17) 0.2500 0.111407(14) 0.01196(4) Uani 1 2 d S
I1 I 0.70976(3) 0.2500 0.38232(3) 0.02142(6) Uani 1 2 d S
P1 P 0.38991(8) 0.35256(3) 0.10966(7) 0.01328(13) Uani 1 1 d .
Si1 Si 0.53229(13) 0.2500 -0.07871(11) 0.01486(19) Uani 1 2 d S
C1 C 0.3672(5) 0.2500 -0.2896(4) 0.0220(8) Uani 1 2 d S
H1A H 0.2796 0.2829 -0.3055 0.033 Uiso 0.50 1 calc PR
H1B H 0.3016 0.2116 -0.3133 0.033 Uiso 0.50 1 calc PR
H1C H 0.4342 0.2555 -0.3600 0.033 Uiso 0.50 1 calc PR
C2 C 0.6937(3) 0.31550(11) -0.0498(3) 0.0199(5) Uani 1 1 d .
H2A H 0.8009 0.3076 0.0481 0.024 Uiso 1 1 calc R
H2B H 0.7378 0.3146 -0.1381 0.024 Uiso 1 1 calc R
C3 C 0.6310(3) 0.37975(11) -0.0386(3) 0.0197(5) Uani 1 1 d .
H3A H 0.5182 0.3878 -0.1314 0.024 Uiso 1 1 calc R
H3B H 0.7260 0.4080 -0.0427 0.024 Uiso 1 1 calc R
C4 C 0.5936(3) 0.39200(11) 0.1124(3) 0.0158(5) Uani 1 1 d .
H4A H 0.5774 0.4357 0.1223 0.019 Uiso 1 1 calc R
H4B H 0.7000 0.3789 0.2054 0.019 Uiso 1 1 calc R
C5 C 0.3473(3) 0.37846(10) 0.2818(3) 0.0135(5) Uani 1 1 d .
C6 C 0.4707(3) 0.41197(11) 0.4027(3) 0.0175(5) Uani 1 1 d .
H6 H 0.5832 0.4240 0.3962 0.021 Uiso 1 1 calc R
C7 C 0.4304(3) 0.42807(11) 0.5340(3) 0.0195(5) Uani 1 1 d .
H7 H 0.5158 0.4509 0.6167 0.023 Uiso 1 1 calc R
C8 C 0.2669(3) 0.41095(11) 0.5440(3) 0.0193(5) Uani 1 1 d .
H8 H 0.2392 0.4225 0.6328 0.023 Uiso 1 1 calc R
C9 C 0.1433(3) 0.37687(12) 0.4245(3) 0.0217(6) Uani 1 1 d .
H9 H 0.0314 0.3646 0.4318 0.026 Uiso 1 1 calc R
C10 C 0.1835(3) 0.36076(12) 0.2950(3) 0.0208(5) Uani 1 1 d .
H10 H 0.0986 0.3373 0.2135 0.025 Uiso 1 1 calc R
C11 C 0.2069(3) 0.39130(11) -0.0492(3) 0.0147(5) Uani 1 1 d .
C12 C 0.0721(3) 0.36016(11) -0.1687(3) 0.0160(5) Uani 1 1 d .
H12 H 0.0748 0.3175 -0.1707 0.019 Uiso 1 1 calc R
C13 C -0.0670(3) 0.39123(12) -0.2857(3) 0.0179(5) Uani 1 1 d .
H13 H -0.1596 0.3696 -0.3660 0.021 Uiso 1 1 calc R
C14 C -0.0707(3) 0.45321(12) -0.2852(3) 0.0191(5) Uani 1 1 d .
H14 H -0.1642 0.4742 -0.3661 0.023 Uiso 1 1 calc R
C15 C 0.0631(3) 0.48497(11) -0.1657(3) 0.0208(5) Uani 1 1 d .
H15 H 0.0606 0.5276 -0.1646 0.025 Uiso 1 1 calc R
C16 C 0.1996(3) 0.45408(11) -0.0489(3) 0.0195(5) Uani 1 1 d .
H16 H 0.2898 0.4759 0.0329 0.023 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'
Si Si 0.0817 0.0704 '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'
I I -0.4742 1.8119 '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
P1 Ir1 P1 174.05(3) 4_565 .
P1 Ir1 Si1 91.850(15) 4_565 .
P1 Ir1 Si1 91.850(15) . .
P1 Ir1 I1 91.910(15) 4_565 .
P1 Ir1 I1 91.910(15) . .
Si1 Ir1 I1 101.53(2) . .
P1 Ir1 H1 87.86(7) 4_565 .
P1 Ir1 H1 87.86(7) . .
Si1 Ir1 H1 84.6(18) . .
I1 Ir1 H1 173.9(18) . .
C5 P1 C4 106.38(11) . .
C5 P1 C11 100.87(10) . .
C4 P1 C11 102.39(11) . .
C5 P1 Ir1 109.72(8) . .
C4 P1 Ir1 115.81(8) . .
C11 P1 Ir1 119.95(8) . .
C1 Si1 C2 108.49(11) . .
C1 Si1 C2 108.49(11) . 4_565
C2 Si1 C2 101.05(16) . 4_565
C1 Si1 Ir1 116.19(12) . .
C2 Si1 Ir1 110.76(8) . .
C2 Si1 Ir1 110.76(8) 4_565 .
Si1 C1 H1A 109.5 . .
Si1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Si1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 Si1 120.86(18) . .
C3 C2 H2A 107.1 . .
Si1 C2 H2A 107.1 . .
C3 C2 H2B 107.1 . .
Si1 C2 H2B 107.1 . .
H2A C2 H2B 106.8 . .
C2 C3 C4 113.6(2) . .
C2 C3 H3A 108.8 . .
C4 C3 H3A 108.8 . .
C2 C3 H3B 108.8 . .
C4 C3 H3B 108.8 . .
H3A C3 H3B 107.7 . .
C3 C4 P1 111.44(16) . .
C3 C4 H4A 109.3 . .
P1 C4 H4A 109.3 . .
C3 C4 H4B 109.3 . .
P1 C4 H4B 109.3 . .
H4A C4 H4B 108.0 . .
C6 C5 C10 118.8(2) . .
C6 C5 P1 123.80(19) . .
C10 C5 P1 117.36(18) . .
C5 C6 C7 120.2(2) . .
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 . .
C8 C7 C6 120.3(2) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
C7 C8 C9 120.0(2) . .
C7 C8 H8 120.0 . .
C9 C8 H8 120.0 . .
C10 C9 C8 119.8(2) . .
C10 C9 H9 120.1 . .
C8 C9 H9 120.1 . .
C9 C10 C5 121.0(2) . .
C9 C10 H10 119.5 . .
C5 C10 H10 119.5 . .
C12 C11 C16 118.6(2) . .
C12 C11 P1 122.10(18) . .
C16 C11 P1 119.28(18) . .
C11 C12 C13 120.4(2) . .
C11 C12 H12 119.8 . .
C13 C12 H12 119.8 . .
C14 C13 C12 120.2(2) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C13 C14 C15 119.9(2) . .
C13 C14 H14 120.0 . .
C15 C14 H14 120.0 . .
C16 C15 C14 119.7(2) . .
C16 C15 H15 120.1 . .
C14 C15 H15 120.1 . .
C15 C16 C11 121.1(2) . .
C15 C16 H16 119.5 . .
C11 C16 H16 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ir1 P1 2.2852(6) 4_565
Ir1 P1 2.2852(6) .
Ir1 Si1 2.3027(9) .
Ir1 I1 2.7288(3) .
Ir1 H1 1.32(4) .
P1 C5 1.819(2) .
P1 C4 1.823(2) .
P1 C11 1.835(2) .
Si1 C1 1.879(4) .
Si1 C2 1.888(2) .
Si1 C2 1.888(2) 4_565
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.528(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.537(3) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.386(3) .
C5 C10 1.398(3) .
C6 C7 1.396(3) .
C6 H6 0.9500 .
C7 C8 1.381(3) .
C7 H7 0.9500 .
C8 C9 1.386(3) .
C8 H8 0.9500 .
C9 C10 1.380(3) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 C12 1.391(3) .
C11 C16 1.398(3) .
C12 C13 1.396(3) .
C12 H12 0.9500 .
C13 C14 1.380(4) .
C13 H13 0.9500 .
C14 C15 1.394(3) .
C14 H14 0.9500 .
C15 C16 1.383(3) .
C15 H15 0.9500 .
C16 H16 0.9500 .
