#------------------------------------------------------------------------------
#$Date: 2019-11-09 07:53:59 +0200 (Sat, 09 Nov 2019) $
#$Revision: 225417 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/31/2243182.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243182
loop_
_publ_author_name
'Taullaj, Fioralba'
'Lough, Alan J.'
'Fekl, Ulrich'
_publ_section_title
;
 An iridium complex with an unsupported Ir---Zn bond:
 diiodido(η⁵-pentamethylcyclopentadienyl)bis(trimethylphosphane)iridiumzinc(Ir---Zn)
 benzene hemisolvate
;
_journal_coeditor_code           ZL2763
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1824
_journal_page_last               1827
_journal_paper_doi               10.1107/S2056989019014622
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ir Zn I2 (C10 H15) (C3 H9 P1)2], 0.5C6 H6'
_chemical_formula_moiety         'C16 H33 I2 Ir P2 Zn, 0.5(C6 H6)'
_chemical_formula_sum            'C19 H36 I2 Ir P2 Zn'
_chemical_formula_weight         837.79
_chemical_name_systematic
;
Diiodido(η⁵-pentamethylcyclopentadienyl)bis(trimethylphosphane)\
iridiumzinc(Ir---Zn) benzene hemisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                95.975(2)
_cell_angle_beta                 91.255(2)
_cell_angle_gamma                114.847(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5353(7)
_cell_length_b                   10.1962(8)
_cell_length_c                   14.6331(10)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.22
_cell_volume                     1280.58(16)
_computing_cell_refinement
;
APEX2 (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Kappa APEX DUO CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            56694
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.546
_diffrn_reflns_theta_min         1.403
_diffrn_source
'sealed tube with Bruker Triumph monochromator'
_exptl_absorpt_coefficient_mu    8.665
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(TWINABS; Bruker, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.173
_exptl_crystal_description       needle
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.662
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5865
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0542P)²+11.6185P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                4967
_reflns_number_total             5865
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            zl2763sup1.cif
_cod_data_source_block           I
_cod_database_code               2243182
_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   0.252
_shelx_estimated_absorpt_t_max   0.846
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Ir Ir1 0.64620(4) 0.30438(4) 0.23280(2) 0.01416(10) Uani d 1
Zn Zn1 0.85316(12) 0.54793(12) 0.22619(7) 0.0182(2) Uani d 1
I I1 1.13849(8) 0.64673(8) 0.29085(5) 0.03107(17) Uani d 1
I I2 0.84656(9) 0.74030(8) 0.12668(5) 0.03387(18) Uani d 1
P P1 0.4792(3) 0.4076(3) 0.25762(17) 0.0184(5) Uani d 1
P P2 0.7072(3) 0.3167(3) 0.38389(16) 0.0184(5) Uani d 1
C C1 0.5046(12) 0.1007(11) 0.1315(7) 0.028(2) Uani d 1
C C2 0.6108(11) 0.0698(10) 0.1844(7) 0.0216(18) Uani d 1
C C3 0.7631(12) 0.1679(11) 0.1690(7) 0.0224(18) Uani d 1
C C4 0.7521(13) 0.2568(12) 0.1035(7) 0.027(2) Uani d 1
C C5 0.5942(13) 0.2200(11) 0.0809(6) 0.0260(19) Uani d 1
C C6 0.3309(13) 0.0135(13) 0.1213(9) 0.039(3) Uani d 1
H H6A 0.302415 -0.058383 0.066236 0.059 Uiso calc 1
H H6B 0.280848 0.079058 0.115315 0.059 Uiso calc 1
H H6C 0.296607 -0.036785 0.175766 0.059 Uiso calc 1
C C7 0.5730(14) -0.0549(12) 0.2404(9) 0.036(3) Uani d 1
H H7A 0.587149 -0.134379 0.204256 0.054 Uiso calc 1
H H7B 0.465243 -0.089402 0.256554 0.054 Uiso calc 1
H H7C 0.642101 -0.022047 0.296775 0.054 Uiso calc 1
C C8 0.9134(13) 0.1610(14) 0.1988(9) 0.038(3) Uani d 1
H H8A 0.951864 0.122296 0.145845 0.056 Uiso calc 1
H H8B 0.894569 0.097313 0.247218 0.056 Uiso calc 1
H H8C 0.990738 0.259090 0.222445 0.056 Uiso calc 1
C C9 0.8854(16) 0.3580(13) 0.0514(8) 0.042(3) Uani d 1
H H9A 0.891465 0.304718 -0.007005 0.064 Uiso calc 1
H H9B 0.983291 0.391807 0.088981 0.064 Uiso calc 1
H H9C 0.866425 0.442011 0.038967 0.064 Uiso calc 1
C C10 0.5338(18) 0.2725(17) 0.0030(8) 0.049(4) Uani d 1
H H10A 0.561866 0.237987 -0.055749 0.074 Uiso calc 1
H H10B 0.579434 0.379230 0.011319 0.074 Uiso calc 1
H H10C 0.420718 0.234441 0.002733 0.074 Uiso calc 1
C C11 0.3809(14) 0.4250(14) 0.1551(8) 0.035(3) Uani d 1
H H11A 0.305145 0.462747 0.173110 0.053 Uiso calc 1
H H11B 0.327569 0.329362 0.118423 0.053 Uiso calc 1
H H11C 0.457013 0.492346 0.118469 0.053 Uiso calc 1
C C12 0.3114(11) 0.3065(12) 0.3218(8) 0.026(2) Uani d 1
H H12A 0.237710 0.350330 0.319995 0.040 Uiso calc 1
H H12B 0.346343 0.310499 0.385961 0.040 Uiso calc 1
H H12C 0.260818 0.204706 0.293688 0.040 Uiso calc 1
C C13 0.5420(12) 0.5912(11) 0.3179(8) 0.028(2) Uani d 1
H H13A 0.451169 0.609824 0.330705 0.042 Uiso calc 1
H H13B 0.608472 0.662236 0.279284 0.042 Uiso calc 1
H H13C 0.600217 0.600006 0.375988 0.042 Uiso calc 1
C C14 0.8854(12) 0.2999(13) 0.4124(7) 0.027(2) Uani d 1
H H14A 0.905137 0.313444 0.479545 0.041 Uiso calc 1
H H14B 0.972012 0.374360 0.385704 0.041 Uiso calc 1
H H14C 0.874887 0.203020 0.387452 0.041 Uiso calc 1
C C15 0.5697(13) 0.1720(12) 0.4447(7) 0.034(3) Uani d 1
H H15A 0.609739 0.184805 0.508784 0.051 Uiso calc 1
H H15B 0.556651 0.076787 0.414398 0.051 Uiso calc 1
H H15C 0.469393 0.177272 0.443155 0.051 Uiso calc 1
C C16 0.7304(13) 0.4736(11) 0.4657(7) 0.029(2) Uani d 1
H H16A 0.772321 0.465670 0.525593 0.043 Uiso calc 1
H H16B 0.629520 0.476117 0.472535 0.043 Uiso calc 1
H H16C 0.801849 0.563231 0.442954 0.043 Uiso calc 1
C C1S 1.1540(14) 1.0646(12) 0.5329(8) 0.033(3) Uani d 1
H H1S 1.259917 1.108754 0.555309 0.040 Uiso calc 1
C C2S 1.1106(14) 0.9857(13) 0.4464(9) 0.037(3) Uani d 1
H H2S 1.186666 0.975586 0.409107 0.045 Uiso calc 1
C C3S 0.9552(14) 0.9211(13) 0.4139(8) 0.037(3) Uani d 1
H H3S 0.925314 0.866769 0.354327 0.045 Uiso calc 1
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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_site_symmetry_1
_geom_angle
P2 Ir1 C5 . 160.3(3)
P2 Ir1 P1 . 93.81(9)
C5 Ir1 P1 . 102.1(3)
P2 Ir1 C3 . 101.5(3)
C5 Ir1 C3 . 61.2(4)
P1 Ir1 C3 . 162.4(3)
P2 Ir1 C4 . 133.0(3)
C5 Ir1 C4 . 36.3(4)
P1 Ir1 C4 . 131.8(3)
C3 Ir1 C4 . 36.4(4)
P2 Ir1 C1 . 127.8(3)
C5 Ir1 C1 . 37.1(4)
P1 Ir1 C1 . 103.0(3)
C3 Ir1 C1 . 60.6(4)
C4 Ir1 C1 . 60.6(4)
P2 Ir1 C2 . 99.7(3)
C5 Ir1 C2 . 60.8(4)
P1 Ir1 C2 . 132.8(3)
C3 Ir1 C2 . 36.1(4)
C4 Ir1 C2 . 60.1(4)
C1 Ir1 C2 . 36.0(4)
P2 Ir1 Zn1 . 91.35(7)
C5 Ir1 Zn1 . 100.5(3)
P1 Ir1 Zn1 . 88.74(7)
C3 Ir1 Zn1 . 99.4(3)
C4 Ir1 Zn1 . 80.8(3)
C1 Ir1 Zn1 . 137.2(3)
C2 Ir1 Zn1 . 135.3(2)
Ir1 Zn1 I2 . 126.73(5)
Ir1 Zn1 I1 . 127.19(5)
I2 Zn1 I1 . 105.11(4)
C11 P1 C13 . 99.5(5)
C11 P1 C12 . 100.2(6)
C13 P1 C12 . 100.5(5)
C11 P1 Ir1 . 115.7(4)
C13 P1 Ir1 . 121.9(3)
C12 P1 Ir1 . 115.6(4)
C14 P2 C16 . 100.7(5)
C14 P2 C15 . 100.1(5)
C16 P2 C15 . 98.6(5)
C14 P2 Ir1 . 115.9(4)
C16 P2 Ir1 . 121.8(3)
C15 P2 Ir1 . 116.2(4)
C2 C1 C5 . 107.5(9)
C2 C1 C6 . 125.9(10)
C5 C1 C6 . 126.3(10)
C2 C1 Ir1 . 72.4(6)
C5 C1 Ir1 . 70.4(5)
C6 C1 Ir1 . 127.9(8)
C3 C2 C1 . 108.6(9)
C3 C2 C7 . 124.2(9)
C1 C2 C7 . 126.9(10)
C3 C2 Ir1 . 70.6(5)
C1 C2 Ir1 . 71.7(6)
C7 C2 Ir1 . 128.4(8)
C2 C3 C4 . 107.8(9)
C2 C3 C8 . 127.2(10)
C4 C3 C8 . 123.8(10)
C2 C3 Ir1 . 73.3(5)
C4 C3 Ir1 . 71.9(5)
C8 C3 Ir1 . 130.4(7)
C5 C4 C3 . 109.0(9)
C5 C4 C9 . 123.7(11)
C3 C4 C9 . 126.4(10)
C5 C4 Ir1 . 71.7(5)
C3 C4 Ir1 . 71.7(5)
C9 C4 Ir1 . 130.9(7)
C4 C5 C1 . 107.0(9)
C4 C5 C10 . 125.0(11)
C1 C5 C10 . 126.6(11)
C4 C5 Ir1 . 72.0(5)
C1 C5 Ir1 . 72.5(5)
C10 C5 Ir1 . 131.1(8)
C1 C6 H6A . 109.5
C1 C6 H6B . 109.5
H6A C6 H6B . 109.5
C1 C6 H6C . 109.5
H6A C6 H6C . 109.5
H6B C6 H6C . 109.5
C2 C7 H7A . 109.5
C2 C7 H7B . 109.5
H7A C7 H7B . 109.5
C2 C7 H7C . 109.5
H7A C7 H7C . 109.5
H7B C7 H7C . 109.5
C3 C8 H8A . 109.5
C3 C8 H8B . 109.5
H8A C8 H8B . 109.5
C3 C8 H8C . 109.5
H8A C8 H8C . 109.5
H8B C8 H8C . 109.5
C4 C9 H9A . 109.5
C4 C9 H9B . 109.5
H9A C9 H9B . 109.5
C4 C9 H9C . 109.5
H9A C9 H9C . 109.5
H9B C9 H9C . 109.5
C5 C10 H10A . 109.5
C5 C10 H10B . 109.5
H10A C10 H10B . 109.5
C5 C10 H10C . 109.5
H10A C10 H10C . 109.5
H10B C10 H10C . 109.5
P1 C11 H11A . 109.5
P1 C11 H11B . 109.5
H11A C11 H11B . 109.5
P1 C11 H11C . 109.5
H11A C11 H11C . 109.5
H11B C11 H11C . 109.5
P1 C12 H12A . 109.5
P1 C12 H12B . 109.5
H12A C12 H12B . 109.5
P1 C12 H12C . 109.5
H12A C12 H12C . 109.5
H12B C12 H12C . 109.5
P1 C13 H13A . 109.5
P1 C13 H13B . 109.5
H13A C13 H13B . 109.5
P1 C13 H13C . 109.5
H13A C13 H13C . 109.5
H13B C13 H13C . 109.5
P2 C14 H14A . 109.5
P2 C14 H14B . 109.5
H14A C14 H14B . 109.5
P2 C14 H14C . 109.5
H14A C14 H14C . 109.5
H14B C14 H14C . 109.5
P2 C15 H15A . 109.5
P2 C15 H15B . 109.5
H15A C15 H15B . 109.5
P2 C15 H15C . 109.5
H15A C15 H15C . 109.5
H15B C15 H15C . 109.5
P2 C16 H16A . 109.5
P2 C16 H16B . 109.5
H16A C16 H16B . 109.5
P2 C16 H16C . 109.5
H16A C16 H16C . 109.5
H16B C16 H16C . 109.5
C3S C1S C2S 2_776 119.9(11)
C3S C1S H1S 2_776 120.0
C2S C1S H1S . 120.0
C1S C2S C3S . 119.9(11)
C1S C2S H2S . 120.1
C3S C2S H2S . 120.1
C1S C3S C2S 2_776 120.2(11)
C1S C3S H3S 2_776 119.9
C2S C3S H3S . 119.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ir1 P2 . 2.251(2)
Ir1 C5 . 2.264(9)
Ir1 P1 . 2.265(2)
Ir1 C3 . 2.265(9)
Ir1 C4 . 2.267(9)
Ir1 C1 . 2.291(10)
Ir1 C2 . 2.301(9)
Ir1 Zn1 . 2.4516(11)
Zn1 I2 . 2.5819(13)
Zn1 I1 . 2.5880(13)
P1 C11 . 1.815(11)
P1 C13 . 1.825(11)
P1 C12 . 1.840(10)
P2 C14 . 1.822(10)
P2 C16 . 1.826(10)
P2 C15 . 1.840(10)
C1 C2 . 1.417(14)
C1 C5 . 1.449(15)
C1 C6 . 1.510(15)
C2 C3 . 1.414(14)
C2 C7 . 1.504(14)
C3 C4 . 1.417(15)
C3 C8 . 1.521(15)
C4 C5 . 1.412(15)
C4 C9 . 1.538(15)
C5 C10 . 1.509(15)
C6 H6A . 0.9800
C6 H6B . 0.9800
C6 H6C . 0.9800
C7 H7A . 0.9800
C7 H7B . 0.9800
C7 H7C . 0.9800
C8 H8A . 0.9800
C8 H8B . 0.9800
C8 H8C . 0.9800
C9 H9A . 0.9800
C9 H9B . 0.9800
C9 H9C . 0.9800
C10 H10A . 0.9800
C10 H10B . 0.9800
C10 H10C . 0.9800
C11 H11A . 0.9800
C11 H11B . 0.9800
C11 H11C . 0.9800
C12 H12A . 0.9800
C12 H12B . 0.9800
C12 H12C . 0.9800
C13 H13A . 0.9800
C13 H13B . 0.9800
C13 H13C . 0.9800
C14 H14A . 0.9800
C14 H14B . 0.9800
C14 H14C . 0.9800
C15 H15A . 0.9800
C15 H15B . 0.9800
C15 H15C . 0.9800
C16 H16A . 0.9800
C16 H16B . 0.9800
C16 H16C . 0.9800
C1S C3S 2_776 1.360(17)
C1S C2S . 1.381(17)
C1S H1S . 0.9500
C2S C3S . 1.393(18)
C2S H2S . 0.9500
C3S H3S . 0.9500
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C5 C1 C2 C3 . . 0.8(11)
C6 C1 C2 C3 . . 174.3(10)
Ir1 C1 C2 C3 . . -61.2(7)
C5 C1 C2 C7 . . -173.2(10)
C6 C1 C2 C7 . . 0.3(17)
Ir1 C1 C2 C7 . . 124.7(11)
C5 C1 C2 Ir1 . . 62.1(7)
C6 C1 C2 Ir1 . . -124.5(11)
C1 C2 C3 C4 . . -2.1(11)
C7 C2 C3 C4 . . 172.1(10)
Ir1 C2 C3 C4 . . -64.1(7)
C1 C2 C3 C8 . . -169.6(10)
C7 C2 C3 C8 . . 4.6(16)
Ir1 C2 C3 C8 . . 128.5(10)
C1 C2 C3 Ir1 . . 61.9(7)
C7 C2 C3 Ir1 . . -123.9(10)
C2 C3 C4 C5 . . 2.7(11)
C8 C3 C4 C5 . . 170.7(9)
Ir1 C3 C4 C5 . . -62.4(6)
C2 C3 C4 C9 . . -167.2(10)
C8 C3 C4 C9 . . 0.8(16)
Ir1 C3 C4 C9 . . 127.8(10)
C2 C3 C4 Ir1 . . 65.0(7)
C8 C3 C4 Ir1 . . -127.0(10)
C3 C4 C5 C1 . . -2.1(10)
C9 C4 C5 C1 . . 168.1(10)
Ir1 C4 C5 C1 . . -64.5(7)
C3 C4 C5 C10 . . -169.6(10)
C9 C4 C5 C10 . . 0.6(15)
Ir1 C4 C5 C10 . . 128.0(10)
C3 C4 C5 Ir1 . . 62.4(6)
C9 C4 C5 Ir1 . . -127.4(10)
C2 C1 C5 C4 . . 0.8(11)
C6 C1 C5 C4 . . -172.6(10)
Ir1 C1 C5 C4 . . 64.2(6)
C2 C1 C5 C10 . . 168.1(10)
C6 C1 C5 C10 . . -5.4(17)
Ir1 C1 C5 C10 . . -128.6(11)
C2 C1 C5 Ir1 . . -63.4(7)
C6 C1 C5 Ir1 . . 123.2(11)
C3S C1S C2S C3S 2_776 . 0(2)
C1S C2S C3S C1S . 2_776 0(2)

_cod_database_fobs_code 2243182
