# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_journal_coden_ASTM ?
_journal_coeditor_code ?
_journal_coeditor_name ?
_journal_coeditor_notes
;
?
;
_journal_date_accepted ?
_journal_date_from_coeditor ?
_journal_date_printers_final ?
_journal_date_printers_first ?
_journal_date_proofs_in ?
_journal_date_proofs_out ?
#=============================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
_journal_techeditor_code ?
_journal_techeditor_notes
;
?
;
_journal_volume ?
_journal_year ?
loop_
_publ_author_name
_publ_author_address
A.Hill
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
R.D.Dewhurst
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
A.C.Willis
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email willis@rsc.anu.edu.au
_publ_contact_author_fax ' 61 2 6125 0750 '
_publ_contact_author_phone ' 61 2 6125 4109 '
#_publ_requested_category 'FM '
_publ_contact_author_name 'Anthony C. Willis'
_publ_contact_letter
;
ENTER TEXT OF LETTER
;
_publ_requested_coeditor_name ?
#=============================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title
;
Crystal structure of
[{(C~9~H~10~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~].2CH~2~Cl~2~
#-- rian19
;
data_rian19
_database_code_depnum_ccdc_archive 'CCDC 689223'
_audit_creation_date 05-24-06
_audit_creation_method CRYSTALS_ver_12-03-99
# 5191230 rian19
_audit_update_record
;
2005-06-24 - Report on C67 H54 B2 Cl5 Hg Ir N12 O5 P2 W2
by Anthony C. Willis
for Anthony F. Hill and Rian Dewhurst
2005-06-24- passes checkcif tests with minor warnings
2009-01-29 - modify cif for referee
;
#==============================================================================
# 4. TEXT
_publ_section_abstract #Text of the abstract
;
The crystal structure of
[{(C~9~H~10~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~].2CH~2~Cl~2~
is reported.
;
_publ_section_comment #Text of the paper
;
The unit cell contains one
[{(C~9~H~10~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~] molecule
plus dichloromethane solvate molecules.
The organometallic species
is centred on a crystallographic inversion symmetry operation.
The HgCl and CO groups on the Ir each have only one-half occupancy
and are disordered with respect to each other.
The Ir atom was initially at 1/2,1/2,1/2, but its anisotropic displacement
ellipsoid was elongated in the direction of the Hg atom
and the Hg---Ir distance was shorter than would have been expected.
Ihe Ir atom was therefore displaced from the inversion centre in
the direction away from the Hg atom.
Initially a restraint was placed on the Ir---Hg distance,
but later it was removed.
Restraints were placed on the Ir---C and C---O distances
and on the displacement parameters of C4 and O4 as they are in close
proximity to the inversion image of the Hg atom.
The dichloromethane molecule is disordered over two orientations, with Cl2
common to both.
Restraints were placed on bonding distances and angles
and on displacement parameters in this molecule.
The biggest peaks in the final difference electron density map
have no chemical significance.
;
_publ_section_acknowledgements # Acknowledgments
;
?
;
_publ_section_figure_captions #Captions to figures
;
?
;
_publ_section_exptl_refinement
# see also _refine_ls_hydrogen for refinement keywords.
;
H atoms were included at idealized positions
and ride on the atom to which they are attached.
;
_publ_section_exptl_prep
;
The compound was prepared by RDD and
recrystallized from dichloromethane/ethanol
The sample ID was RD-4,58.
;
_refine_special_details #Text of the paper
;
The unit cell contains one
[{(C~9~H~10~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~] molecule
plus dichloromethane solvate molecules.
The organometallic species
is centred on a crystallographic inversion symmetry operation.
The HgCl and CO groups on the Ir each have only one-half occupancy
and are disordered with respect to each other.
The Ir atom was initially at 1/2,1/2,1/2, but its anisotropic displacement
ellipsoid was elongated in the direction of the Hg atom
and the Hg---Ir distance was shorter than would have been expected.
Ihe Ir atom was therefore displaced from the inversion centre in
the direction away from the Hg atom.
Initially a restraint was placed on the Ir---Hg distance,
but later it was removed.
Restraints were placed on the Ir---C and C---O distances
and on the displacement parameters of C4 and O4 as they are in close
proximity to the inversion image of the Hg atom.
The dichloromethane molecule is disordered over two orientations, with Cl2
common to both.
Restraints were placed on bonding distances and angles
and on displacement parameters in this molecule.
H atoms were included at idealized positions
and ride on the atom to which they are attached.
;
#==========================================================================
_chemical_name_systematic # IUPAC name, in full
;
?
;
_chemical_melting_point ?
# choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse'
_refine_ls_matrix_type full
# choose from 'heavy, direct, difmap, geom'
_atom_sites_solution_primary direct
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
# choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed'
_refine_ls_hydrogen_treatment noref
#****************************************************************************
# General computing
#=============================================================
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2003)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2003)
;
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
#=============================================================
_cell_length_a 12.0420(4)
_cell_angle_alpha 65.9070(17)
_cell_length_b 12.6900(4)
_cell_angle_beta 86.9260(19)
_cell_length_c 14.3350(3)
_cell_angle_gamma 66.3350(16)
_cell_volume 1815.59(10)
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
# choose from: rm (reference molecule of
# known chirality), ad (anomolous
# dispersion - ie. Flack param), rmad
# (both rm and ad), syn (known from
# synthetic pathway), unk (unknown)
# or . (not applicable).
_chemical_absolute_configuration .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 International_Tables_Vol_IV_Table_2.2B
'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'Hg ' -2.3894 9.2266 20.6809 0.5450 19.0417 8.4484 21.6575 1.5729 5.9676
38.3246 12.6089 International_Tables_Vol_IV_Table_2.2B
'Ir ' -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338
45.0011 11.4722 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 International_Tables_Vol_IV_Table_2.2B
'W ' -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 International_Tables_Vol_IV_Table_2.2B
_cell_formula_units_Z 1
_chemical_formula_sum ' C67 H54 B2 Cl5 Hg Ir N12 O5 P2 W2 '
_chemical_formula_moiety
' C65 H50 B2 Cl Hg Ir N12 O5 P2 W2 , 2(C H2 Cl2)'
_chemical_compound_source
;
?
;
_chemical_formula_weight 2128.59
_cell_measurement_reflns_used 25429
_cell_measurement_theta_min 3
_cell_measurement_theta_max 25
_cell_measurement_temperature 200
_exptl_crystal_description ' plate '
_exptl_crystal_colour ' orange '
_exptl_crystal_size_min 0.03
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_max 0.06
_exptl_crystal_density_diffrn 1.947
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1010
_exptl_absorpt_coefficient_mu 7.376
_diffrn_measurement_device_type
;
Nonius Kappa CCD
;
_diffrn_radiation_monochromator graphite
_computing_data_collection
;
COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_structure_solution
;
SIR92 (Altomare et al, 1994)
;
_diffrn_measurement_method ' \f and \w scans with CCD '
_diffrn_special_details
;
CCD data collecting conditions-
phi and omega scans of width 2.0 deg at rate 1160 sec/frame,
crystal-detector distance 28mm,
multiple scan sets so over 95 percent of data collected with 2-fold
redundancy or more.
;
# Absorption correction
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.005
-1 0 0 0.030
0 1 1 0.010
0 -1 -1 0.015
0 -1 1 0.030
0 1 -1 0.030
_exptl_absorpt_correction_type integration
_exptl_absorpt_correction_T_min 0.677
_exptl_absorpt_correction_T_max 0.855
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
# Sheldrick geometric definitions 0.74 0.80
_diffrn_standards_interval_time 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 0
_diffrn_standards_decay_% 0.00
_diffrn_ambient_temperature 200
_diffrn_reflns_number 31953
_reflns_number_total 6386
_diffrn_reflns_av_R_equivalents 0.05
# Number of reflections with Friedels Law is 6386
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 6442
_diffrn_reflns_theta_min 2.590
_diffrn_reflns_theta_max 25.0
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 25.
_diffrn_measured_fraction_theta_full 0.99
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_reflns_limit_h_min -14
_reflns_limit_h_max 14
_reflns_limit_k_min -13
_reflns_limit_k_max 15
_reflns_limit_l_min 0
_reflns_limit_l_max 17
_refine_diff_density_min -2.10
_refine_diff_density_max 1.97
_refine_ls_number_reflns 4285
_refine_ls_number_restraints 64
_refine_ls_number_parameters 478
#_refine_ls_R_factor_ref 0.0454
_refine_ls_wR_factor_ref 0.0377
_refine_ls_goodness_of_fit_ref 1.0179
#_reflns_number_all 6362
_refine_ls_R_factor_all 0.0738
_refine_ls_wR_factor_all 0.0410
# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression I>3.00u(I)
_reflns_number_gt 4285
_refine_ls_R_factor_gt 0.0454
_refine_ls_wR_factor_gt 0.0377
_refine_ls_shift/su_max 0.000980
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.18 -0.420 0.957 -0.0709
;
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
## -------------------REFERENCES ----------------------##
## Insert your own references - in alphabetic order
_publ_section_references
;
Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K.
(2000). maXus Computer Program for the Solution and Refinement of
Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The
University of Glasgow.
Coppens, P. (1970). The Evaluation of Absorption and Extinction in
Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed,
S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270.
Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C.,
Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution
of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Nonius BV, COLLECT Software, 1997-2001)
Otwinowski, Z. & Minor, W. (1996), Processing of X-ray
Diffraction Data Collected in Oscillation Mode. Methods Enzymol.
276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Watkin D.J. (1994),
Acta Cryst, A50, 411-437
Molecular Structure Corporation. (1992-1997). teXsan.
Single Crystal Structure Analysis Software. Version 1.8.
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.
Johnson, C.K. (1976)
ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138,
Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA.
;
# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3
# Replace trailing . with the number of unfound
# hydrogen atoms attaced to relavent atom
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Hg1 Hg 0.69223(12) 0.35546(16) 0.47776(10) 0.0374 0.5000 Uani . U . . . .
Ir1 Ir 0.4815(2) 0.5107(5) 0.5001(4) 0.0281 0.5000 Uani D . . . . .
W1 W 0.26830(3) 0.79760(3) 0.02036(3) 0.0295 1.0000 Uani . . . . . .
Cl1 Cl 0.8838(5) 0.2134(7) 0.4528(5) 0.0715 0.5000 Uani . . . . . .
Cl2 Cl 1.1151(5) 0.3375(6) 0.0869(5) 0.1500 1.0000 Uani D U . . . .
Cl31 Cl 0.9382(13) 0.2902(17) 0.2049(9) 0.0883 0.5000 Uani D U . S 1 .
Cl32 Cl 0.9425(18) 0.273(2) 0.2531(15) 0.1467 0.5000 Uani D U . S 2 .
P1 P 0.4269(2) 0.3381(2) 0.55298(16) 0.0351 1.0000 Uani . . . . . .
O4 O 0.2312(12) 0.7007(14) 0.5178(14) 0.0833 0.5000 Uani D U . . . .
O5 O 0.1835(6) 1.0287(7) 0.0792(6) 0.0522 1.0000 Uani . . . . . .
O6 O 0.0468(7) 0.7376(8) 0.1076(6) 0.0629 1.0000 Uani . . . . . .
N11 N 0.1702(7) 0.9236(7) -0.1450(5) 0.0342 1.0000 Uani . . . . . .
N12 N 0.2272(7) 0.9080(8) -0.2259(5) 0.0420 1.0000 Uani . . . . . .
N21 N 0.3269(6) 0.6560(7) -0.0436(6) 0.0368 1.0000 Uani . . . . . .
N22 N 0.3628(7) 0.6761(7) -0.1389(6) 0.0396 1.0000 Uani . . . . . .
N31 N 0.4193(6) 0.8376(7) -0.0576(5) 0.0337 1.0000 Uani . . . . . .
N32 N 0.4415(7) 0.8355(7) -0.1518(6) 0.0402 1.0000 Uani . . . . . .
C1 C 0.3425(8) 0.7007(8) 0.1527(7) 0.0328 1.0000 Uani . . . . . .
C2 C 0.3888(9) 0.6320(8) 0.2593(7) 0.0333 1.0000 Uani . . . . . .
C3 C 0.4303(8) 0.5763(8) 0.3491(6) 0.0343 1.0000 Uani . . . . . .
C4 C 0.319(2) 0.630(4) 0.504(3) 0.0387 0.5000 Uani D U . . . .
C5 C 0.2135(8) 0.9430(9) 0.0574(6) 0.0373 1.0000 Uani . . . . . .
C6 C 0.1286(9) 0.7605(9) 0.0745(7) 0.0427 1.0000 Uani . . . . . .
C13 C 0.1481(11) 0.9919(11) -0.3134(7) 0.0580 1.0000 Uani . . . . . .
C14 C 0.0425(10) 1.0595(10) -0.2879(8) 0.0582 1.0000 Uani . . . . . .
C15 C 0.0588(9) 1.0168(9) -0.1837(7) 0.0454 1.0000 Uani . . . . . .
C23 C 0.3953(9) 0.5723(10) -0.1560(8) 0.0505 1.0000 Uani . . . . . .
C24 C 0.3832(9) 0.4773(10) -0.0719(9) 0.0496 1.0000 Uani . . . . . .
C25 C 0.3405(11) 0.5386(11) -0.0073(9) 0.0651 1.0000 Uani . . . . . .
C33 C 0.5398(9) 0.8619(10) -0.1795(8) 0.0540 1.0000 Uani . . . . . .
C34 C 0.5840(9) 0.8786(10) -0.1035(9) 0.0536 1.0000 Uani . . . . . .
C35 C 0.5036(9) 0.8657(9) -0.0287(8) 0.0434 1.0000 Uani . . . . . .
C111 C 0.3076(9) 0.3692(8) 0.4593(7) 0.0435 1.0000 Uani . . . . . .
C112 C 0.3344(12) 0.3751(10) 0.3614(8) 0.0560 1.0000 Uani . . . . . .
C113 C 0.2430(12) 0.4020(11) 0.2884(8) 0.0584 1.0000 Uani . . . . . .
C114 C 0.1276(14) 0.4218(14) 0.3154(11) 0.0787 1.0000 Uani . . . . . .
C115 C 0.0977(13) 0.4148(19) 0.4123(14) 0.1046 1.0000 Uani . . . . . .
C116 C 0.1931(11) 0.3876(14) 0.4840(10) 0.0748 1.0000 Uani . . . . . .
C121 C 0.3580(8) 0.3037(9) 0.6726(7) 0.0372 1.0000 Uani . . . . . .
C122 C 0.3148(10) 0.3868(10) 0.7183(7) 0.0477 1.0000 Uani . . . . . .
C123 C 0.2483(9) 0.3639(10) 0.8014(7) 0.0485 1.0000 Uani . . . . . .
C124 C 0.2279(10) 0.2557(10) 0.8393(8) 0.0522 1.0000 Uani . . . . . .
C125 C 0.2738(11) 0.1692(10) 0.7974(9) 0.0599 1.0000 Uani . . . . . .
C126 C 0.3399(10) 0.1937(10) 0.7142(8) 0.0539 1.0000 Uani . . . . . .
C131 C 0.5473(9) 0.1812(9) 0.5762(7) 0.0393 1.0000 Uani . . . . . .
C132 C 0.6441(10) 0.1262(9) 0.6574(8) 0.0493 1.0000 Uani . . . . . .
C133 C 0.7395(11) 0.0110(9) 0.6767(8) 0.0508 1.0000 Uani . . . . . .
C134 C 0.7456(10) -0.0529(11) 0.6158(9) 0.0562 1.0000 Uani . . . . . .
C135 C 0.6543(10) -0.0001(10) 0.5383(9) 0.0556 1.0000 Uani . . . . . .
C136 C 0.5542(10) 0.1169(10) 0.5172(8) 0.0514 1.0000 Uani . . . . . .
C201 C 0.984(3) 0.313(6) 0.082(2) 0.1279 0.5000 Uani D U . S 1 .
C202 C 0.985(4) 0.298(6) 0.123(2) 0.1404 0.5000 Uani D U . S 2 .
B1 B 0.3594(10) 0.8085(10) -0.2096(7) 0.0365 1.0000 Uani . . . . . .
H1 H 0.3877 0.8113 -0.2772 0.0419 1.0000 Uiso R . . . . .
H131 H 0.1652 1.0020 -0.3849 0.0603 1.0000 Uiso R . . . . .
H141 H -0.0330 1.1276 -0.3361 0.0565 1.0000 Uiso R . . . . .
H151 H -0.0035 1.0503 -0.1422 0.0496 1.0000 Uiso R . . . . .
H231 H 0.4242 0.5653 -0.2208 0.0655 1.0000 Uiso R . . . . .
H241 H 0.4001 0.3886 -0.0600 0.0591 1.0000 Uiso R . . . . .
H251 H 0.3214 0.4948 0.0631 0.0743 1.0000 Uiso R . . . . .
H331 H 0.5746 0.8682 -0.2455 0.0609 1.0000 Uiso R . . . . .
H341 H 0.6574 0.8963 -0.1013 0.0679 1.0000 Uiso R . . . . .
H351 H 0.5089 0.8759 0.0363 0.0540 1.0000 Uiso R . . . . .
H1121 H 0.4193 0.3600 0.3437 0.0778 1.0000 Uiso R . . . . .
H1131 H 0.2612 0.4068 0.2182 0.0714 1.0000 Uiso R . . . . .
H1141 H 0.0619 0.4421 0.2629 0.0973 1.0000 Uiso R . . . . .
H1151 H 0.0132 0.4283 0.4304 0.1356 1.0000 Uiso R . . . . .
H1161 H 0.1754 0.3818 0.5544 0.0912 1.0000 Uiso R . . . . .
H1221 H 0.3312 0.4646 0.6916 0.0629 1.0000 Uiso R . . . . .
H1231 H 0.2157 0.4257 0.8331 0.0665 1.0000 Uiso R . . . . .
H1241 H 0.1791 0.2397 0.8981 0.0634 1.0000 Uiso R . . . . .
H1251 H 0.2601 0.0898 0.8262 0.0687 1.0000 Uiso R . . . . .
H1261 H 0.3748 0.1303 0.6841 0.0654 1.0000 Uiso R . . . . .
H1321 H 0.6425 0.1716 0.7007 0.0595 1.0000 Uiso R . . . . .
H1331 H 0.8056 -0.0276 0.7352 0.0573 1.0000 Uiso R . . . . .
H1341 H 0.8160 -0.1359 0.6292 0.0700 1.0000 Uiso R . . . . .
H1351 H 0.6578 -0.0456 0.4946 0.0724 1.0000 Uiso R . . . . .
H1361 H 0.4881 0.1531 0.4592 0.0638 1.0000 Uiso R . . . . .
H2011 H 0.919 0.390 0.027 0.1441 0.5000 Uiso R . . S 1 .
H2012 H 1.002 0.237 0.069 0.1441 0.5000 Uiso R . . S 1 .
H2021 H 0.912 0.368 0.072 0.1612 0.5000 Uiso R . . S 2 .
H2022 H 1.003 0.217 0.116 0.1612 0.5000 Uiso R . . S 2 .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Hg1 0.0427(5) 0.0401(6) 0.0278(6) -0.0099(4) 0.0039(4) -0.0203(4)
Ir1 0.0301(16) 0.0342(14) 0.0217(3) -0.0063(7) 0.0017(13) -0.0204(14)
W1 0.0329(2) 0.0321(2) 0.02497(18) -0.01136(15) 0.00502(13) -0.01575(16)
Cl1 0.049(3) 0.083(4) 0.061(3) -0.030(3) 0.018(3) -0.009(3)
Cl2 0.111(4) 0.155(5) 0.172(5) -0.100(4) -0.036(4) -0.005(3)
Cl31 0.056(4) 0.089(6) 0.111(8) -0.034(7) -0.023(6) -0.026(4)
Cl32 0.092(7) 0.105(8) 0.219(15) -0.059(12) -0.059(10) -0.018(6)
P1 0.0484(14) 0.0350(12) 0.0280(10) -0.0102(9) 0.0049(9) -0.0262(11)
O4 0.064(9) 0.062(9) 0.067(9) 0.007(8) 0.007(8) -0.008(8)
O5 0.055(4) 0.051(4) 0.063(5) -0.037(4) 0.010(3) -0.019(3)
O6 0.050(4) 0.081(6) 0.071(5) -0.033(4) 0.026(4) -0.041(4)
N11 0.035(4) 0.039(4) 0.031(4) -0.017(3) 0.007(3) -0.015(3)
N12 0.047(5) 0.049(5) 0.025(4) -0.008(3) -0.002(3) -0.022(4)
N21 0.035(4) 0.030(4) 0.039(4) -0.014(3) 0.000(3) -0.008(3)
N22 0.036(4) 0.044(4) 0.041(4) -0.026(4) 0.004(3) -0.011(4)
N31 0.033(4) 0.037(4) 0.031(4) -0.009(3) 0.004(3) -0.020(3)
N32 0.036(4) 0.049(5) 0.036(4) -0.013(3) 0.012(3) -0.024(4)
C1 0.038(5) 0.024(4) 0.036(5) -0.011(4) 0.002(4) -0.015(4)
C2 0.048(5) 0.032(5) 0.034(5) -0.017(4) 0.009(4) -0.026(4)
C3 0.044(5) 0.037(5) 0.027(5) -0.008(4) 0.006(4) -0.028(4)
C4 0.036(8) 0.040(8) 0.035(9) -0.017(7) 0.015(7) -0.012(7)
C5 0.036(5) 0.042(5) 0.030(4) -0.011(4) 0.010(4) -0.019(4)
C6 0.045(6) 0.038(5) 0.038(5) -0.014(4) 0.000(4) -0.011(4)
C13 0.067(8) 0.068(7) 0.016(4) -0.007(5) 0.004(4) -0.017(6)
C14 0.051(7) 0.050(6) 0.040(6) -0.002(5) -0.012(5) -0.005(5)
C15 0.036(5) 0.046(6) 0.042(5) -0.012(4) 0.008(4) -0.013(5)
C23 0.043(6) 0.060(6) 0.061(6) -0.041(6) 0.001(5) -0.017(5)
C24 0.037(5) 0.034(5) 0.077(7) -0.031(5) -0.004(5) -0.005(4)
C25 0.078(8) 0.061(7) 0.047(6) 0.006(5) -0.009(6) -0.048(7)
C33 0.047(6) 0.060(7) 0.045(6) -0.011(5) 0.015(5) -0.025(5)
C34 0.041(6) 0.062(7) 0.066(7) -0.025(6) 0.009(5) -0.033(5)
C35 0.045(5) 0.037(5) 0.053(6) -0.020(4) 0.011(4) -0.022(4)
C111 0.050(6) 0.030(5) 0.050(5) -0.012(4) -0.005(4) -0.020(4)
C112 0.088(8) 0.064(7) 0.043(5) -0.022(5) 0.018(5) -0.058(6)
C113 0.079(8) 0.063(7) 0.036(5) -0.015(5) -0.011(5) -0.037(6)
C114 0.079(10) 0.085(9) 0.079(9) -0.044(8) -0.007(7) -0.030(8)
C115 0.049(8) 0.175(18) 0.115(13) -0.096(13) 0.018(8) -0.036(9)
C116 0.044(7) 0.112(11) 0.072(8) -0.056(8) -0.002(6) -0.017(7)
C121 0.043(5) 0.040(5) 0.034(5) -0.012(4) 0.009(4) -0.027(4)
C122 0.065(6) 0.056(6) 0.037(5) -0.013(4) 0.012(4) -0.046(5)
C123 0.056(6) 0.069(7) 0.041(5) -0.026(5) 0.020(4) -0.045(6)
C124 0.050(6) 0.057(6) 0.052(6) -0.015(5) 0.014(5) -0.033(5)
C125 0.067(7) 0.043(6) 0.062(7) -0.009(5) 0.020(6) -0.030(6)
C126 0.065(7) 0.044(6) 0.055(6) -0.016(5) 0.033(5) -0.032(5)
C131 0.049(5) 0.046(5) 0.042(5) -0.023(4) 0.018(4) -0.035(5)
C132 0.059(6) 0.040(5) 0.050(6) -0.013(4) -0.002(5) -0.026(5)
C133 0.069(7) 0.032(5) 0.042(5) -0.006(4) 0.001(5) -0.022(5)
C134 0.056(7) 0.058(7) 0.061(7) -0.031(6) 0.019(5) -0.025(6)
C135 0.061(7) 0.054(6) 0.066(7) -0.037(6) 0.020(6) -0.027(6)
C136 0.052(6) 0.060(7) 0.048(6) -0.031(5) 0.009(5) -0.021(5)
C201 0.089(11) 0.130(11) 0.142(12) -0.071(11) -0.031(11) -0.004(10)
C202 0.103(11) 0.130(11) 0.170(14) -0.089(12) -0.046(12) 0.002(10)
B1 0.040(6) 0.040(6) 0.024(5) -0.012(4) 0.010(4) -0.015(5)
_refine_ls_extinction_method None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Hg1 . Ir1 . 2.615(3) yes
Hg1 . Cl1 . 2.408(6) yes
Hg1 . P1 . 3.380(3) yes
Ir1 . P1 2_666 2.428(6) yes
Ir1 . C3 2_666 2.092(10) yes
Ir1 . P1 . 2.356(6) yes
Ir1 . C3 . 2.004(10) yes
Ir1 . C4 . 1.952(9) yes
W1 . N11 . 2.294(7) yes
W1 . N21 . 2.197(7) yes
W1 . N31 . 2.207(7) yes
W1 . C1 . 1.818(9) yes
W1 . C5 . 1.976(10) yes
W1 . C6 . 1.962(10) yes
Cl1 . O4 2_666 1.544(10) yes
Cl2 . C201 . 1.735(18) yes
Cl2 . C202 . 1.820(18) yes
Cl31 . C201 . 1.758(18) yes
Cl32 . C202 . 1.845(18) yes
P1 . C111 . 1.828(9) yes
P1 . C121 . 1.829(9) yes
P1 . C131 . 1.836(10) yes
O4 . C4 . 1.149(9) yes
O5 . C5 . 1.167(11) yes
O6 . C6 . 1.161(11) yes
N11 . N12 . 1.359(10) yes
N11 . C15 . 1.332(12) yes
N12 . C13 . 1.356(12) yes
N12 . B1 . 1.539(13) yes
N21 . N22 . 1.363(10) yes
N21 . C25 . 1.303(13) yes
N22 . C23 . 1.337(12) yes
N22 . B1 . 1.553(13) yes
N31 . N32 . 1.371(10) yes
N31 . C35 . 1.336(11) yes
N32 . C33 . 1.353(12) yes
N32 . B1 . 1.542(13) yes
C1 . C2 . 1.421(13) yes
C2 . C3 . 1.205(12) yes
C13 . C14 . 1.348(16) yes
C13 . H131 . 1.000 no
C14 . C15 . 1.360(14) yes
C14 . H141 . 1.000 no
C15 . H151 . 1.000 no
C23 . C24 . 1.365(16) yes
C23 . H231 . 1.000 no
C24 . C25 . 1.394(17) yes
C24 . H241 . 1.000 no
C25 . H251 . 1.000 no
C33 . C34 . 1.362(15) yes
C33 . H331 . 1.000 no
C34 . C35 . 1.409(14) yes
C34 . H341 . 1.000 no
C35 . H351 . 1.000 no
C111 . C112 . 1.402(14) yes
C111 . C116 . 1.356(16) yes
C112 . C113 . 1.398(15) yes
C112 . H1121 . 1.000 no
C113 . C114 . 1.374(19) yes
C113 . H1131 . 1.000 no
C114 . C115 . 1.39(2) yes
C114 . H1141 . 1.000 no
C115 . C116 . 1.419(18) yes
C115 . H1151 . 1.000 no
C116 . H1161 . 1.000 no
C121 . C122 . 1.378(14) yes
C121 . C126 . 1.380(13) yes
C122 . C123 . 1.395(13) yes
C122 . H1221 . 1.000 no
C123 . C124 . 1.374(14) yes
C123 . H1231 . 1.000 no
C124 . C125 . 1.373(16) yes
C124 . H1241 . 1.000 no
C125 . C126 . 1.396(14) yes
C125 . H1251 . 1.000 no
C126 . H1261 . 1.000 no
C131 . C132 . 1.424(14) yes
C131 . C136 . 1.376(13) yes
C132 . C133 . 1.375(15) yes
C132 . H1321 . 1.000 no
C133 . C134 . 1.396(15) yes
C133 . H1331 . 1.000 no
C134 . C135 . 1.350(16) yes
C134 . H1341 . 1.000 no
C135 . C136 . 1.409(16) yes
C135 . H1351 . 1.000 no
C136 . H1361 . 1.000 no
C201 . H2011 . 1.000 no
C201 . H2012 . 1.000 no
C202 . H2021 . 1.000 no
C202 . H2022 . 1.000 no
B1 . H1 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ir1 . Hg1 . Cl1 . 178.4(2) yes
C3 2_666 Ir1 . P1 2_666 91.6(3) yes
C3 2_666 Ir1 . Hg1 . 80.6(3) yes
P1 2_666 Ir1 . Hg1 . 84.73(12) yes
C3 2_666 Ir1 . P1 . 85.2(3) yes
P1 2_666 Ir1 . P1 . 170.11(14) yes
Hg1 . Ir1 . P1 . 85.51(17) yes
C3 2_666 Ir1 . C3 . 168.53(17) yes
P1 2_666 Ir1 . C3 . 85.3(3) yes
Hg1 . Ir1 . C3 . 88.2(3) yes
C3 2_666 Ir1 . C4 . 104.7(13) yes
P1 2_666 Ir1 . C4 . 95.9(18) yes
Hg1 . Ir1 . C4 . 174.7(12) yes
P1 . Ir1 . C3 . 96.0(3) yes
P1 . Ir1 . C4 . 94.0(18) yes
C3 . Ir1 . C4 . 86.6(13) yes
N11 . W1 . N21 . 79.9(3) yes
N11 . W1 . N31 . 80.2(2) yes
N21 . W1 . N31 . 81.4(3) yes
N11 . W1 . C1 . 178.3(3) yes
N21 . W1 . C1 . 101.5(3) yes
N31 . W1 . C1 . 100.7(3) yes
N11 . W1 . C5 . 92.7(3) yes
N21 . W1 . C5 . 171.8(3) yes
N31 . W1 . C5 . 93.8(3) yes
C1 . W1 . C5 . 85.9(4) yes
N11 . W1 . C6 . 94.3(3) yes
N21 . W1 . C6 . 93.4(3) yes
N31 . W1 . C6 . 172.9(3) yes
C1 . W1 . C6 . 84.9(4) yes
C5 . W1 . C6 . 90.9(4) yes
Ir1 . P1 . C111 . 110.8(3) yes
Ir1 . P1 . C121 . 115.9(3) yes
C111 . P1 . C121 . 102.5(4) yes
Ir1 2_666 P1 . C111 . 115.8(3) yes
Ir1 2_666 P1 . C121 . 120.8(3) yes
Ir1 2_666 P1 . C131 . 108.3(3) yes
Ir1 . P1 . C131 . 118.2(3) yes
C111 . P1 . C131 . 106.0(4) yes
C121 . P1 . C131 . 101.8(4) yes
W1 . N11 . N12 . 120.4(5) yes
W1 . N11 . C15 . 132.6(6) yes
N12 . N11 . C15 . 107.1(7) yes
N11 . N12 . C13 . 108.0(8) yes
N11 . N12 . B1 . 121.3(7) yes
C13 . N12 . B1 . 130.7(8) yes
W1 . N21 . N22 . 124.5(6) yes
W1 . N21 . C25 . 133.3(8) yes
N22 . N21 . C25 . 102.3(8) yes
N21 . N22 . C23 . 111.1(8) yes
N21 . N22 . B1 . 118.8(7) yes
C23 . N22 . B1 . 130.1(8) yes
W1 . N31 . N32 . 122.0(5) yes
W1 . N31 . C35 . 131.0(6) yes
N32 . N31 . C35 . 107.0(7) yes
N31 . N32 . C33 . 108.8(8) yes
N31 . N32 . B1 . 121.2(7) yes
C33 . N32 . B1 . 130.0(8) yes
W1 . C1 . C2 . 173.9(7) yes
C1 . C2 . C3 . 177.6(9) yes
Ir1 2_666 C3 . C2 . 172.8(7) yes
Ir1 . C3 . C2 . 170.5(8) yes
Ir1 . C4 . O4 . 170(4) yes
W1 . C5 . O5 . 178.7(7) yes
W1 . C6 . O6 . 179.2(8) yes
N12 . C13 . C14 . 108.5(9) yes
N12 . C13 . H131 . 125.750 no
C14 . C13 . H131 . 125.728 no
C13 . C14 . C15 . 106.5(9) yes
C13 . C14 . H141 . 126.776 no
C15 . C14 . H141 . 126.765 no
C14 . C15 . N11 . 109.9(9) yes
C14 . C15 . H151 . 125.040 no
N11 . C15 . H151 . 125.033 no
N22 . C23 . C24 . 109.9(9) yes
N22 . C23 . H231 . 125.016 no
C24 . C23 . H231 . 125.038 no
C23 . C24 . C25 . 100.4(9) yes
C23 . C24 . H241 . 129.788 no
C25 . C24 . H241 . 129.810 no
C24 . C25 . N21 . 116.3(10) yes
C24 . C25 . H251 . 121.836 no
N21 . C25 . H251 . 121.830 no
N32 . C33 . C34 . 109.4(9) yes
N32 . C33 . H331 . 125.315 no
C34 . C33 . H331 . 125.308 no
C33 . C34 . C35 . 104.9(8) yes
C33 . C34 . H341 . 127.527 no
C35 . C34 . H341 . 127.539 no
C34 . C35 . N31 . 109.8(9) yes
C34 . C35 . H351 . 125.098 no
N31 . C35 . H351 . 125.090 no
P1 . C111 . C112 . 119.9(8) yes
P1 . C111 . C116 . 120.2(8) yes
C112 . C111 . C116 . 119.9(10) yes
C111 . C112 . C113 . 120.3(11) yes
C111 . C112 . H1121 . 119.864 no
C113 . C112 . H1121 . 119.854 no
C112 . C113 . C114 . 118.3(11) yes
C112 . C113 . H1131 . 120.827 no
C114 . C113 . H1131 . 120.827 no
C113 . C114 . C115 . 123.1(12) yes
C113 . C114 . H1141 . 118.428 no
C115 . C114 . H1141 . 118.430 no
C114 . C115 . C116 . 116.7(13) yes
C114 . C115 . H1151 . 121.663 no
C116 . C115 . H1151 . 121.678 no
C115 . C116 . C111 . 121.6(12) yes
C115 . C116 . H1161 . 119.178 no
C111 . C116 . H1161 . 119.180 no
P1 . C121 . C122 . 123.2(6) yes
P1 . C121 . C126 . 118.0(7) yes
C122 . C121 . C126 . 118.6(8) yes
C121 . C122 . C123 . 120.9(8) yes
C121 . C122 . H1221 . 119.572 no
C123 . C122 . H1221 . 119.560 no
C122 . C123 . C124 . 119.4(10) yes
C122 . C123 . H1231 . 120.297 no
C124 . C123 . H1231 . 120.290 no
C123 . C124 . C125 . 120.8(10) yes
C123 . C124 . H1241 . 119.597 no
C125 . C124 . H1241 . 119.596 no
C124 . C125 . C126 . 119.1(9) yes
C124 . C125 . H1251 . 120.456 no
C126 . C125 . H1251 . 120.453 no
C125 . C126 . C121 . 121.1(10) yes
C125 . C126 . H1261 . 119.436 no
C121 . C126 . H1261 . 119.433 no
P1 . C131 . C132 . 117.3(7) yes
P1 . C131 . C136 . 124.6(8) yes
C132 . C131 . C136 . 117.9(9) yes
C131 . C132 . C133 . 120.4(9) yes
C131 . C132 . H1321 . 119.802 no
C133 . C132 . H1321 . 119.796 no
C132 . C133 . C134 . 121.0(10) yes
C132 . C133 . H1331 . 119.484 no
C134 . C133 . H1331 . 119.497 no
C133 . C134 . C135 . 118.5(11) yes
C133 . C134 . H1341 . 120.753 no
C135 . C134 . H1341 . 120.766 no
C134 . C135 . C136 . 122.1(10) yes
C134 . C135 . H1351 . 118.947 no
C136 . C135 . H1351 . 118.936 no
C135 . C136 . C131 . 120.0(10) yes
C135 . C136 . H1361 . 119.986 no
C131 . C136 . H1361 . 119.991 no
Cl31 . C201 . Cl2 . 103.9(11) yes
Cl31 . C201 . H2011 . 110.679 no
Cl2 . C201 . H2011 . 110.673 no
Cl31 . C201 . H2012 . 111.015 no
Cl2 . C201 . H2012 . 111.022 no
H2011 . C201 . H2012 . 109.467 no
Cl32 . C202 . Cl2 . 118.4(14) yes
Cl32 . C202 . H2021 . 107.253 no
Cl2 . C202 . H2021 . 107.261 no
Cl32 . C202 . H2022 . 107.128 no
Cl2 . C202 . H2022 . 107.114 no
H2021 . C202 . H2022 . 109.467 no
N22 . B1 . N32 . 107.7(7) yes
N22 . B1 . N12 . 107.9(7) yes
N32 . B1 . N12 . 108.2(8) yes
N22 . B1 . H1 . 111.230 no
N32 . B1 . H1 . 110.967 no
N12 . B1 . H1 . 110.791 no
#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl1 Cl32 2.78(2) . . no
Cl1 Cl31 3.38(1) . . no
Cl2 C34 3.51(1) . 2_765 no
O5 C15 3.36(1) . 2_575 no
O5 O6 3.372(9) . 2_575 no
O5 C201 3.46(6) . 1_465 no
O5 C34 3.53(2) . 2_675 no
O5 C202 3.58(6) . 1_465 no
O6 C201 3.11(6) . 2_665 no
O6 C124 3.33(2) . 2_566 no
O6 C15 3.46(2) . 2_575 no
O6 C202 3.57(5) . 2_665 no
N11 C125 3.59(2) . 1_564 no
N21 C24 3.37(1) . 2_665 no
N22 C25 3.59(1) . 2_665 no
N31 C24 3.44(1) . 2_665 no
N31 C125 3.53(1) . 1_564 no
C6 C201 3.29(6) . 2_665 no
C23 C25 3.48(2) . 2_665 no
C24 C25 3.48(2) . 2_665 no
C24 C123 3.51(2) . 1_554 no
C25 C25 3.56(3) . 2_665 no
C25 C201 3.59(3) . 2_665 no
C33 C126 3.59(1) . 1_564 no
#------------------------------------------------------------------------------
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
HG1 Ir1 P1 C111 . . . . -112.7(4) no
HG1 Ir1 P1 C121 . . . . 131.1(3) no
HG1 Ir1 P1 C131 . . . . 9.9(4) no
Ir1 P1 C111 C112 . . . . 68.3(9) no
Ir1 P1 C111 C116 . . . . -111(1) no
Ir1 P1 C121 C122 . . . . 14.0(9) no
Ir1 P1 C121 C126 . . . . -171.3(7) no
Ir1 P1 C131 C132 . . . . 63.5(9) no
Ir1 P1 C131 C136 . . . . -113(1) no
W1 N11 N12 C13 . . . . 178.6(9) no
W1 N11 N12 B1 . . . . -2(2) no
W1 N11 C15 C14 . . . . -177.9(9) no
W1 N21 N22 C23 . . . . 178.9(7) no
W1 N21 N22 B1 . . . . -2(1) no
W1 N21 C25 C24 . . . . -178.5(7) no
W1 N31 N32 C33 . . . . -179.3(5) no
W1 N31 N32 B1 . . . . 1.7(9) no
W1 N31 C35 C34 . . . . 177.8(6) no
P1 C111 C112 C113 . . . . -178.4(9) no
P1 C111 C116 C115 . . . . 179(1) no
P1 C121 C122 C123 . . . . 171.2(7) no
P1 C121 C126 C125 . . . . -171.6(9) no
P1 C131 C132 C133 . . . . -177.7(9) no
P1 C131 C136 C135 . . . . 176.5(9) no
N11 W1 N21 N22 . . . . 42.4(7) no
N11 W1 N21 C25 . . . . -140(1) no
N11 W1 N31 N32 . . . . -42.5(6) no
N11 W1 N31 C35 . . . . 138.1(8) no
N11 N12 C13 C14 . . . . -0(2) no
N11 N12 B1 N22 . . . . 60(1) no
N11 N12 B1 N32 . . . . -57(1) no
N11 C15 C14 C13 . . . . -1(2) no
N12 N11 W1 N21 . . . . -40.3(9) no
N12 N11 W1 N31 . . . . 42.6(9) no
N12 N11 W1 C5 . . . . 136.0(9) no
N12 N11 W1 C6 . . . . -132.9(9) no
N12 N11 C15 C14 . . . . 1(2) no
N12 C13 C14 C15 . . . . 1(2) no
N12 B1 N22 N21 . . . . -58(1) no
N12 B1 N22 C23 . . . . 121(1) no
N12 B1 N32 N31 . . . . 57.7(9) no
N12 B1 N32 C33 . . . . -121.1(9) no
N21 W1 N11 C15 . . . . 139(1) no
N21 W1 N31 N32 . . . . 38.7(5) no
N21 W1 N31 C35 . . . . -140.7(7) no
N21 N22 C23 C24 . . . . -0(1) no
N21 N22 B1 N32 . . . . 58(1) no
N21 C25 C24 C23 . . . . -0(1) no
N22 N21 W1 N31 . . . . -39.2(7) no
N22 N21 W1 C1 . . . . -138.5(7) no
N22 N21 W1 C6 . . . . 136.1(7) no
N22 N21 C25 C24 . . . . -0(1) no
N22 C23 C24 C25 . . . . 0(1) no
N22 B1 N12 C13 . . . . -121(1) no
N22 B1 N32 N31 . . . . -59(1) no
N22 B1 N32 C33 . . . . 122.5(9) no
N31 W1 N11 C15 . . . . -138(1) no
N31 W1 N21 C25 . . . . 139(1) no
N31 N32 C33 C34 . . . . 1(1) no
N31 C35 C34 C33 . . . . 2(1) no
N32 N31 W1 C1 . . . . 138.9(6) no
N32 N31 W1 C5 . . . . -134.6(6) no
N32 N31 C35 C34 . . . . -1.7(9) no
N32 C33 C34 C35 . . . . -2(1) no
N32 B1 N12 C13 . . . . 123(1) no
N32 B1 N22 C23 . . . . -123(1) no
C1 W1 N21 C25 . . . . 40(1) no
C1 W1 N31 C35 . . . . -40.5(8) no
C3 Ir1 P1 C111 . . . . -25.1(5) no
C3 Ir1 P1 C121 . . . . -141.2(4) no
C3 Ir1 P1 C131 . . . . 97.5(5) no
C3 Ir1 P1 C111 . . 2_666 2_666 -159.6(4) no
C3 Ir1 P1 C121 . . 2_666 2_666 -35.0(4) no
C3 Ir1 P1 C131 . . 2_666 2_666 81.6(5) no
C4 Ir1 P1 C111 . . . . 62(1) no
C4 Ir1 P1 C121 . . . . -54(1) no
C4 Ir1 P1 C131 . . . . -175(1) no
C4 Ir1 P1 C111 . . 2_666 2_666 114(1) no
C4 Ir1 P1 C121 . . 2_666 2_666 -121(1) no
C4 Ir1 P1 C131 . . 2_666 2_666 -5(1) no
C5 W1 N11 C15 . . . . -45(1) no
C5 W1 N31 C35 . . . . 46.0(7) no
C6 W1 N11 C15 . . . . 46(1) no
C6 W1 N21 C25 . . . . -46(1) no
C13 N12 N11 C15 . . . . -1(1) no
C14 C13 N12 B1 . . . . -180(1) no
C15 N11 N12 B1 . . . . 179(1) no
C23 N22 N21 C25 . . . . 0(1) no
C24 C23 N22 B1 . . . . -180(1) no
C25 N21 N22 B1 . . . . 179.6(9) no
C33 N32 N31 C35 . . . . 0.3(9) no
C34 C33 N32 B1 . . . . -179.8(8) no
C35 N31 N32 B1 . . . . -178.8(7) no
C111 P1 C121 C122 . . . . -106.8(9) no
C111 P1 C121 C126 . . . . 67.9(8) no
C111 P1 C131 C132 . . . . -171.5(8) no
C111 P1 C131 C136 . . . . 12(1) no
C111 C112 C113 C114 . . . . -0(2) no
C111 C116 C115 C114 . . . . -0(3) no
C112 C111 P1 C121 . . . . -167.4(9) no
C112 C111 P1 C131 . . . . -61.1(9) no
C112 C111 C116 C115 . . . . -1(2) no
C112 C113 C114 C115 . . . . -1(2) no
C113 C112 C111 C116 . . . . 1(2) no
C113 C114 C115 C116 . . . . 1(3) no
C116 C111 P1 C121 . . . . 13(1) no
C116 C111 P1 C131 . . . . 119(1) no
C121 P1 C131 C132 . . . . -65(1) no
C121 P1 C131 C136 . . . . 119(1) no
C121 C122 C123 C124 . . . . 1(2) no
C121 C126 C125 C124 . . . . -1(2) no
C122 C121 P1 C131 . . . . 143.7(9) no
C122 C121 C126 C125 . . . . 3(2) no
C122 C123 C124 C125 . . . . 1(2) no
C123 C122 C121 C126 . . . . -3(1) no
C123 C124 C125 C126 . . . . -1(2) no
C126 C121 P1 C131 . . . . -41.6(9) no
C131 C132 C133 C134 . . . . 2(2) no
C131 C136 C135 C134 . . . . 0(2) no
C132 C131 C136 C135 . . . . 0(2) no
C132 C133 C134 C135 . . . . -1(2) no
C133 C132 C131 C136 . . . . -1(2) no
C133 C134 C135 C136 . . . . 0(2) no
#------------------------------------------------------------------------------
# start Validation Reply Form
_vrf_PLAT431_rian19
;
PROBLEM: Short Inter HL..A Contact Cl1 .. Cl32 .. 2.78 Ang.
RESPONSE: ...
This comes from the disorder - each of these sites has half-occupancy.
;
# end Validation Reply Form
#===END=
# Attachment 'New Compound 8b.cif'
data_rian20a
_database_code_depnum_ccdc_archive 'CCDC 689224'
_audit_creation_date 05-17-05
_audit_creation_method CRYSTALS_ver_12-03-99
# 7220937 rian20a
_audit_update_record
;
2005-05-17 - Report on C87 H98 B2 Cl Hg Ir N12 O5 P2 W2
by Anthony C. Willis
for Anthony F. Hill and Rian Dewhurst
2005-05-17- passes checkcif tests with minor warnings
2009-01-29 - modify cif for referee
;
#==============================================================================
# 4. TEXT
_publ_section_abstract #Text of the abstract
;
The crystal structure of
[{(C~15~H~22~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~].solvate
is reported.
;
_publ_section_comment #Text of the paper
;
The unit cell contains one
[{(C~15~H~22~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~] molecule
plus solvate molecules.
The organometallic species
is centred on a crystallographic inversion symmetry operation.
The HgCl and CO groups on the Ir each have only one-half occupancy
and are disordered with respect to each other.
The Ir atom was initially at 1/2,1/2,1/2, but its anisotropic displacement
ellipsoid was elongated in the direction of the Hg atom
and the Hg---Ir distance was shorter than would have been expected.
Ihe Ir atom was therefore displaced from the inversion centre in
the direction away from the Hg atom.
Initially a restraint was placed on the Ir---Hg distance,
but later it was removed.
Restraints were placed on the Ir---C and C---O distances
and on the displacement parameters of C4 and O4 as they are in close
proximity to the inversion image of the Hg atom.
A region of electron density was observed away from the principal species,
presumably indicating the presence of molecules of solvation.
It exhibited 5 adjacent peaks of almost equal intensity.
The crystals had been produced from CH~2~Cl~2~, with ethanol and hexane
having been used during synthesis.
Attempts to model the electron density as disordered dichloromethane molecules
was not successful. A fair fit can be obtained for a n-pentane molecule.
Possibly it represents disordered hexane
with multiple terminal sites of low occupancy not being observed.
Restraints were placed on distances, angles and displacement parameters in
this molecule.
The biggest peaks in the final difference electron density map are
near to W or Ir atoms and have no chemical significance.
;
_publ_section_acknowledgements # Acknowledgments
;
?
;
_publ_section_figure_captions #Captions to figures
;
?
;
_publ_section_exptl_refinement
# see also _refine_ls_hydrogen for refinement keywords.
;
H atoms were included at idealized positions
and ride on the atom to which they are attached.
The methyl hydrogens of the C~15~H~22~BN~6~ groups have been oriented to
match peaks in difference electron density maps.
;
_publ_section_exptl_prep
;
The compound was prepared by RDD and
recrystallized from dichloromethane,
tetrahydrofuran, ethanol and hexane being present in earlier synthetic steps.
The sample ID was RD-4,88.
;
_refine_special_details #Text of the paper
;
The unit cell contains one
[{(C~15~H~22~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~] molecule
plus solvate molecules.
The organometallic species
is centred on a crystallographic inversion symmetry operation.
The HgCl and CO groups on the Ir each have only one-half occupancy
and are disordered with respect to each other.
The Ir atom was initially at 1/2,1/2,1/2, but its anisotropic displacement
ellipsoid was elongated in the direction of the Hg atom
and the Hg---Ir distance was shorter than would have been expected.
Ihe Ir atom was therefore displaced from the inversion centre in
the direction away from the Hg atom.
Initially a restraint was placed on the Ir---Hg distance,
but later it was removed.
Restraints were placed on the Ir---C and C---O distances
and on the displacement parameters of C4 and O4 as they are in close
proximity to the inversion image of the Hg atom.
A region of electron density was observed away from the principal species,
presumably indicating the presence of molecules of solvation.
It exhibited 5 adjacent peaks of almost equal intensity.
The crystals had been produced from CH~2~Cl~2~, with ethanol and hexane
having been used during synthesis.
Attempts to model the electron density as disordered dichloromethane molecules
was not successful. A fair fit can be obtained for a n-pentane molecule.
Possibly it represents disordered hexane
with multiple terminal sites of low occupancy not being observed.
Restraints were placed on distances, angles and displacement parameters in
this molecule.
H atoms were included at idealized positions
and ride on the atom to which they are attached.
The methyl hydrogens of the C~15~H~22~BN~6~ groups have been oriented to
match peaks in difference electron density maps.
;
#==========================================================================
_chemical_name_systematic # IUPAC name, in full
;
?
;
_chemical_melting_point ?
# choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse'
_refine_ls_matrix_type full
# choose from 'heavy, direct, difmap, geom'
_atom_sites_solution_primary direct
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
# choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed'
_refine_ls_hydrogen_treatment noref
#****************************************************************************
# General computing
#=============================================================
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2003)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2003)
;
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
#=============================================================
_cell_length_a 11.4118(4)
_cell_angle_alpha 81.4328(17)
_cell_length_b 13.3666(4)
_cell_angle_beta 72.8924(16)
_cell_length_c 15.9096(3)
_cell_angle_gamma 69.1166(12)
_cell_volume 2164.41(11)
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
# choose from: rm (reference molecule of
# known chirality), ad (anomolous
# dispersion - ie. Flack param), rmad
# (both rm and ad), syn (known from
# synthetic pathway), unk (unknown)
# or . (not applicable).
_chemical_absolute_configuration .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 International_Tables_Vol_IV_Table_2.2B
'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'Hg ' -2.3894 9.2266 20.6809 0.5450 19.0417 8.4484 21.6575 1.5729 5.9676
38.3246 12.6089 International_Tables_Vol_IV_Table_2.2B
'Ir ' -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338
45.0011 11.4722 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 International_Tables_Vol_IV_Table_2.2B
'W ' -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 International_Tables_Vol_IV_Table_2.2B
_cell_formula_units_Z 1
_chemical_formula_sum ' C87 H98 B2 Cl Hg Ir N12 O5 P2 W2 '
_chemical_formula_moiety ' C77 H74 B2 Cl Hg Ir N12 O5 P2 W2 , 2(C5 H12)'
_chemical_compound_source
;
?
;
_chemical_formula_weight 2271.35
_cell_measurement_reflns_used 70955
_cell_measurement_theta_min 1
_cell_measurement_theta_max 27
_cell_measurement_temperature 200
_exptl_crystal_description ' plate '
_exptl_crystal_colour ' red '
_exptl_crystal_size_min 0.08
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_max 0.40
_exptl_crystal_density_diffrn 1.742
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1106
_exptl_absorpt_coefficient_mu 6.074
_diffrn_measurement_device_type
;
Nonius Kappa CCD
;
_diffrn_radiation_monochromator graphite
_computing_data_collection
;
COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_structure_solution
;
SIR92 (Altomare et al, 1994)
;
_diffrn_measurement_method ' \f and \w scans with CCD '
_diffrn_special_details
;
CCD data collecting conditions-
phi and omega scans of width 1.1 deg at rate 22 sec/frame,
crystal-detector distance 28mm,
multiple scan sets so over 95 percent of data collected with 2-fold
redundancy or more.
;
# Absorption correction
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.060
0 -1 0 0.030
6 3 -1 0.068
-6 -3 1 0.134
-1 -1 4 0.149
1 0 1 0.101
-1 1 -4 0.151
3 3 -12 0.127
3 -1 -1 0.038
-16 5 -4 0.147
_exptl_absorpt_correction_type integration
_exptl_absorpt_correction_T_min 0.230
_exptl_absorpt_correction_T_max 0.601
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents 0.054
# Sheldrick geometric definitions 0.30 0.62
_diffrn_standards_interval_time 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 0
_diffrn_standards_decay_% 0.00
_diffrn_ambient_temperature 200
_diffrn_reflns_number 45949
_reflns_number_total 9962
_diffrn_reflns_av_R_equivalents 0.07
# Number of reflections with Friedels Law is 9962
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 9992
_diffrn_reflns_theta_min 1.341
_diffrn_reflns_theta_max 27.5
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 27.547
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 20
_reflns_limit_h_min -13
_reflns_limit_h_max 14
_reflns_limit_k_min -17
_reflns_limit_k_max 17
_reflns_limit_l_min 0
_reflns_limit_l_max 20
_refine_diff_density_min -1.56
_refine_diff_density_max 1.57
_refine_ls_number_reflns 6453
_refine_ls_number_restraints 40
_refine_ls_number_parameters 526
#_refine_ls_R_factor_ref 0.0325
_refine_ls_wR_factor_ref 0.0369
_refine_ls_goodness_of_fit_ref 1.0852
#_reflns_number_all 9925
_refine_ls_R_factor_all 0.0568
_refine_ls_wR_factor_all 0.0444
# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression I>3.00u(I)
_reflns_number_gt 6453
_refine_ls_R_factor_gt 0.0325
_refine_ls_wR_factor_gt 0.0369
_refine_ls_shift/su_max 0.017
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.33 -0.0617 1.07
;
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
## -------------------REFERENCES ----------------------##
## Insert your own references - in alphabetic order
_publ_section_references
;
Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K.
(2000). maXus Computer Program for the Solution and Refinement of
Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The
University of Glasgow.
Coppens, P. (1970). The Evaluation of Absorption and Extinction in
Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed,
S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270.
Larson, A.C. (1970). The Inclusion of Secondary Extinction in Least-Squares
Refinement in Crystal Structures. Crystallographic Computing. F. R. Ahmed, S.
R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 291-294
Altomare, A., Cascarano, G., Giacovazzo C., Guagliardi A., Burla M.C.,
Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution
of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Nonius BV, COLLECT Software, 1997-2001)
Otwinowski, Z. & Minor, W. (1996), Processing of X-ray
Diffraction Data Collected in Oscillation Mode. Methods Enzymol.
276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Watkin D.J. (1994),
Acta Cryst, A50, 411-437
Molecular Structure Corporation. (1992-1997). teXsan.
Single Crystal Structure Analysis Software. Version 1.8.
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.
Johnson, C.K. (1976)
ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138,
Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA.
;
# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3
# Replace trailing . with the number of unfound
# hydrogen atoms attaced to relavent atom
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Hg1 Hg 0.29378(8) 0.63951(5) 0.51354(6) 0.0408 0.5000 Uani . U . . . .
Ir1 Ir 0.51740(18) 0.4902(2) 0.4994(2) 0.0293 0.5000 Uani D . . . . .
W1 W 0.63645(2) 0.655772(16) 0.090252(12) 0.0294 1.0000 Uani . . . . . .
Cl1 Cl 0.0908(5) 0.7783(4) 0.5291(4) 0.0935 0.5000 Uani . . . . . .
P1 P 0.57522(14) 0.62233(11) 0.54425(8) 0.0339 1.0000 Uani . . . . . .
O4 O 0.7937(11) 0.3232(9) 0.4778(9) 0.0745 0.5000 Uani D U . . . .
O5 O 0.3491(4) 0.6732(4) 0.1068(3) 0.0548 1.0000 Uani . . . . . .
O6 O 0.6998(5) 0.4123(3) 0.0612(3) 0.0527 1.0000 Uani . . . . . .
N11 N 0.6879(4) 0.7090(3) -0.0546(3) 0.0323 1.0000 Uani . . . . . .
N12 N 0.7667(4) 0.7715(3) -0.0820(3) 0.0331 1.0000 Uani . . . . . .
N21 N 0.8385(4) 0.6484(4) 0.0747(3) 0.0340 1.0000 Uani . . . . . .
N22 N 0.8791(4) 0.7343(4) 0.0387(3) 0.0340 1.0000 Uani . . . . . .
N31 N 0.5919(4) 0.8288(3) 0.1046(3) 0.0339 1.0000 Uani . . . . . .
N32 N 0.6675(4) 0.8847(3) 0.0496(3) 0.0331 1.0000 Uani . . . . . .
C1 C 0.5993(5) 0.6130(4) 0.2075(4) 0.0350 1.0000 Uani . . . . . .
C2 C 0.5687(5) 0.5807(5) 0.2951(4) 0.0379 1.0000 Uani . . . . . .
C3 C 0.5456(6) 0.5523(5) 0.3722(3) 0.0392 1.0000 Uani . . . . . .
C4 C 0.690(2) 0.3842(19) 0.488(2) 0.0408 0.5000 Uani D . . . . .
C5 C 0.4537(6) 0.6702(5) 0.0986(3) 0.0390 1.0000 Uani . . . . . .
C6 C 0.6803(5) 0.5011(5) 0.0684(4) 0.0409 1.0000 Uani . . . . . .
C13 C 0.8019(5) 0.7812(5) -0.1718(3) 0.0379 1.0000 Uani . . . . . .
C14 C 0.7445(6) 0.7238(5) -0.2023(3) 0.0409 1.0000 Uani . . . . . .
C15 C 0.6747(5) 0.6799(4) -0.1283(4) 0.0379 1.0000 Uani . . . . . .
C16 C 0.8889(7) 0.8427(6) -0.2225(5) 0.0570 1.0000 Uani . . . . . .
C17 C 0.5948(7) 0.6114(5) -0.1237(4) 0.0481 1.0000 Uani . . . . . .
C23 C 0.9965(5) 0.7199(5) 0.0517(4) 0.0406 1.0000 Uani . . . . . .
C24 C 1.0328(5) 0.6221(5) 0.0961(4) 0.0382 1.0000 Uani . . . . . .
C25 C 0.9342(5) 0.5794(4) 0.1092(3) 0.0362 1.0000 Uani . . . . . .
C26 C 1.0653(6) 0.8001(6) 0.0208(5) 0.0527 1.0000 Uani . . . . . .
C27 C 0.9281(6) 0.4731(5) 0.1519(4) 0.0484 1.0000 Uani . . . . . .
C33 C 0.6117(6) 0.9905(4) 0.0651(4) 0.0400 1.0000 Uani . . . . . .
C34 C 0.4997(6) 1.0033(5) 0.1304(4) 0.0451 1.0000 Uani . . . . . .
C35 C 0.4897(5) 0.9007(5) 0.1554(4) 0.0396 1.0000 Uani . . . . . .
C36 C 0.6693(8) 1.0716(5) 0.0160(5) 0.0534 1.0000 Uani . . . . . .
C37 C 0.3858(7) 0.8702(6) 0.2240(5) 0.0532 1.0000 Uani . . . . . .
C111 C 0.6128(6) 0.7166(5) 0.4543(4) 0.0394 1.0000 Uani . . . . . .
C112 C 0.7217(6) 0.6788(5) 0.3839(4) 0.0459 1.0000 Uani . . . . . .
C113 C 0.7505(7) 0.7446(6) 0.3109(4) 0.0544 1.0000 Uani . . . . . .
C114 C 0.6670(8) 0.8491(6) 0.3072(5) 0.0634 1.0000 Uani . . . . . .
C115 C 0.5577(8) 0.8859(6) 0.3753(6) 0.0687 1.0000 Uani . . . . . .
C116 C 0.5306(7) 0.8198(6) 0.4487(5) 0.0529 1.0000 Uani . . . . . .
C121 C 0.7208(6) 0.5629(5) 0.5855(4) 0.0410 1.0000 Uani . . . . . .
C122 C 0.7270(6) 0.4772(6) 0.6472(4) 0.0501 1.0000 Uani . . . . . .
C123 C 0.8299(7) 0.4378(7) 0.6850(5) 0.0616 1.0000 Uani . . . . . .
C124 C 0.9263(7) 0.4813(7) 0.6629(5) 0.0642 1.0000 Uani . . . . . .
C125 C 0.9228(7) 0.5675(7) 0.6012(5) 0.0602 1.0000 Uani . . . . . .
C126 C 0.8196(6) 0.6080(6) 0.5628(5) 0.0508 1.0000 Uani . . . . . .
C131 C 0.4654(5) 0.7061(4) 0.6353(4) 0.0375 1.0000 Uani . . . . . .
C132 C 0.3506(6) 0.6919(5) 0.6871(4) 0.0440 1.0000 Uani . . . . . .
C133 C 0.2753(7) 0.7547(6) 0.7576(4) 0.0574 1.0000 Uani . . . . . .
C134 C 0.3120(8) 0.8348(6) 0.7761(4) 0.0599 1.0000 Uani . . . . . .
C135 C 0.4267(8) 0.8494(6) 0.7269(5) 0.0590 1.0000 Uani . . . . . .
C136 C 0.5058(7) 0.7845(5) 0.6573(4) 0.0492 1.0000 Uani . . . . . .
C501 C 0.7873(17) 0.9236(13) 0.5445(13) 0.1505 1.0000 Uani D U . . . .
C502 C 0.789(2) 0.9422(17) 0.4560(15) 0.1935 1.0000 Uani D U . . . .
C503 C 0.870(2) 1.0085(16) 0.3985(14) 0.1885 1.0000 Uani D U . . . .
C504 C 0.983(2) 0.9074(18) 0.3548(15) 0.2123 1.0000 Uani D U . . . .
C505 C 0.9868(15) 0.9083(13) 0.2622(13) 0.1556 1.0000 Uani D U . . . .
B1 B 0.7962(6) 0.8240(5) -0.0138(4) 0.0341 1.0000 Uani . . . . . .
H1 H 0.8439 0.8748 -0.0441 0.0430 1.0000 Uiso R . . . . .
H141 H 0.7517 0.7154 -0.2652 0.0466 1.0000 Uiso R . . . . .
H161 H 0.9013 0.8389 -0.2870 0.0651 1.0000 Uiso R . . . . .
H162 H 0.8487 0.9193 -0.2061 0.0651 1.0000 Uiso R . . . . .
H163 H 0.9750 0.8112 -0.2084 0.0651 1.0000 Uiso R . . . . .
H171 H 0.5972 0.5989 -0.1847 0.0613 1.0000 Uiso R . . . . .
H172 H 0.5031 0.6482 -0.0908 0.0613 1.0000 Uiso R . . . . .
H173 H 0.6305 0.5411 -0.0927 0.0613 1.0000 Uiso R . . . . .
H241 H 1.1150 0.5882 0.1152 0.0454 1.0000 Uiso R . . . . .
H261 H 1.1497 0.7731 0.0374 0.0674 1.0000 Uiso R . . . . .
H262 H 1.0101 0.8696 0.0489 0.0674 1.0000 Uiso R . . . . .
H263 H 1.0824 0.8113 -0.0446 0.0674 1.0000 Uiso R . . . . .
H271 H 1.0079 0.4346 0.1730 0.0580 1.0000 Uiso R . . . . .
H272 H 0.8495 0.4843 0.2031 0.0580 1.0000 Uiso R . . . . .
H273 H 0.9228 0.4293 0.1082 0.0580 1.0000 Uiso R . . . . .
H341 H 0.4368 1.0725 0.1557 0.0544 1.0000 Uiso R . . . . .
H361 H 0.6126 1.1442 0.0379 0.0688 1.0000 Uiso R . . . . .
H362 H 0.7575 1.0549 0.0250 0.0688 1.0000 Uiso R . . . . .
H363 H 0.6767 1.0708 -0.0481 0.0688 1.0000 Uiso R . . . . .
H371 H 0.3198 0.9357 0.2536 0.0614 1.0000 Uiso R . . . . .
H372 H 0.4248 0.8185 0.2686 0.0614 1.0000 Uiso R . . . . .
H373 H 0.3429 0.8358 0.1959 0.0614 1.0000 Uiso R . . . . .
H1121 H 0.7799 0.6027 0.3865 0.0553 1.0000 Uiso R . . . . .
H1131 H 0.8300 0.7174 0.2617 0.0689 1.0000 Uiso R . . . . .
H1141 H 0.6862 0.8979 0.2549 0.0762 1.0000 Uiso R . . . . .
H1151 H 0.4975 0.9612 0.3717 0.0783 1.0000 Uiso R . . . . .
H1161 H 0.4509 0.8473 0.4977 0.0614 1.0000 Uiso R . . . . .
H1221 H 0.6568 0.4441 0.6641 0.0620 1.0000 Uiso R . . . . .
H1231 H 0.8336 0.3762 0.7294 0.0726 1.0000 Uiso R . . . . .
H1241 H 1.0003 0.4515 0.6910 0.0751 1.0000 Uiso R . . . . .
H1251 H 0.9938 0.5996 0.5848 0.0747 1.0000 Uiso R . . . . .
H1261 H 0.8160 0.6699 0.5186 0.0634 1.0000 Uiso R . . . . .
H1321 H 0.3221 0.6351 0.6731 0.0546 1.0000 Uiso R . . . . .
H1331 H 0.1941 0.7421 0.7952 0.0664 1.0000 Uiso R . . . . .
H1341 H 0.2552 0.8825 0.8256 0.0686 1.0000 Uiso R . . . . .
H1351 H 0.4533 0.9072 0.7413 0.0725 1.0000 Uiso R . . . . .
H1361 H 0.5907 0.7933 0.6232 0.0597 1.0000 Uiso R . . . . .
H5011 H 0.7306 0.8793 0.5736 0.1941 1.0000 Uiso R . . . . .
H5012 H 0.7525 0.9936 0.5734 0.1941 1.0000 Uiso R . . . . .
H5013 H 0.8776 0.8845 0.5503 0.1941 1.0000 Uiso R . . . . .
H5021 H 0.697 0.9798 0.4529 0.2351 1.0000 Uiso R . . . . .
H5022 H 0.823 0.8707 0.4298 0.2351 1.0000 Uiso R . . . . .
H5031 H 0.898 1.0483 0.4330 0.2245 1.0000 Uiso R . . . . .
H5032 H 0.827 1.0595 0.3555 0.2245 1.0000 Uiso R . . . . .
H5041 H 1.067 0.9087 0.3596 0.2501 1.0000 Uiso R . . . . .
H5042 H 0.967 0.8409 0.3860 0.2501 1.0000 Uiso R . . . . .
H5051 H 1.0584 0.8438 0.2349 0.2018 1.0000 Uiso R . . . . .
H5052 H 1.0028 0.9747 0.2309 0.2018 1.0000 Uiso R . . . . .
H5053 H 0.9020 0.9069 0.2573 0.2018 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Hg1 0.0418(4) 0.0405(4) 0.0407(2) -0.0034(3) -0.0116(2) -0.0132(3)
Ir1 0.0372(9) 0.0319(8) 0.02217(16) 0.0006(5) -0.0073(7) -0.0165(7)
W1 0.03302(11) 0.03191(11) 0.02435(10) 0.00144(7) -0.00799(7) -0.01267(8)
Cl1 0.064(2) 0.077(3) 0.120(4) -0.017(3) -0.031(3) 0.011(2)
P1 0.0420(7) 0.0376(7) 0.0267(6) -0.0025(5) -0.0064(5) -0.0203(6)
O4 0.041(6) 0.068(7) 0.105(8) -0.021(6) -0.027(5) 0.006(5)
O5 0.042(2) 0.056(3) 0.071(3) 0.006(2) -0.022(2) -0.020(2)
O6 0.063(3) 0.031(2) 0.065(3) -0.0059(19) -0.009(2) -0.021(2)
N11 0.040(2) 0.036(2) 0.024(2) 0.0023(16) -0.0088(17) -0.0174(18)
N12 0.038(2) 0.035(2) 0.026(2) 0.0025(16) -0.0082(17) -0.0138(18)
N21 0.032(2) 0.038(2) 0.031(2) 0.0031(17) -0.0082(17) -0.0113(18)
N22 0.034(2) 0.036(2) 0.035(2) 0.0021(17) -0.0099(17) -0.0150(18)
N31 0.036(2) 0.031(2) 0.037(2) -0.0014(17) -0.0134(18) -0.0115(18)
N32 0.039(2) 0.031(2) 0.032(2) 0.0060(17) -0.0164(18) -0.0108(18)
C1 0.035(3) 0.034(3) 0.039(3) 0.002(2) -0.011(2) -0.014(2)
C2 0.046(3) 0.040(3) 0.032(3) -0.001(2) -0.008(2) -0.023(2)
C3 0.048(3) 0.049(3) 0.023(2) -0.001(2) -0.002(2) -0.025(3)
C4 0.0418(4) 0.0405(4) 0.0407(2) -0.0034(3) -0.0116(2) -0.0132(3)
C5 0.045(3) 0.044(3) 0.029(3) 0.001(2) -0.013(2) -0.014(2)
C6 0.035(3) 0.051(4) 0.035(3) 0.000(2) -0.003(2) -0.017(2)
C13 0.035(3) 0.046(3) 0.025(2) 0.005(2) -0.009(2) -0.006(2)
C14 0.044(3) 0.050(3) 0.023(2) -0.001(2) -0.008(2) -0.009(2)
C15 0.036(3) 0.038(3) 0.038(3) -0.006(2) -0.011(2) -0.006(2)
C16 0.050(4) 0.065(4) 0.047(4) 0.010(3) -0.003(3) -0.022(3)
C17 0.061(4) 0.051(3) 0.042(3) -0.010(3) -0.019(3) -0.021(3)
C23 0.037(3) 0.049(3) 0.043(3) 0.000(2) -0.013(2) -0.021(2)
C24 0.031(3) 0.042(3) 0.040(3) 0.000(2) -0.013(2) -0.008(2)
C25 0.034(3) 0.040(3) 0.031(2) -0.004(2) -0.010(2) -0.006(2)
C26 0.046(3) 0.053(4) 0.069(4) 0.005(3) -0.021(3) -0.027(3)
C27 0.049(3) 0.042(3) 0.053(4) 0.011(3) -0.023(3) -0.012(3)
C33 0.050(3) 0.028(3) 0.049(3) 0.001(2) -0.030(3) -0.009(2)
C34 0.053(3) 0.033(3) 0.049(3) -0.011(2) -0.023(3) -0.003(2)
C35 0.040(3) 0.039(3) 0.037(3) -0.012(2) -0.014(2) -0.001(2)
C36 0.079(5) 0.034(3) 0.059(4) 0.004(3) -0.036(3) -0.021(3)
C37 0.052(4) 0.052(4) 0.049(4) -0.016(3) -0.006(3) -0.011(3)
C111 0.046(3) 0.043(3) 0.036(3) 0.000(2) -0.009(2) -0.024(3)
C112 0.056(3) 0.043(3) 0.039(3) -0.001(2) -0.002(3) -0.026(3)
C113 0.065(4) 0.070(4) 0.038(3) 0.000(3) -0.006(3) -0.041(4)
C114 0.071(5) 0.069(5) 0.051(4) 0.022(3) -0.017(3) -0.032(4)
C115 0.068(5) 0.053(4) 0.075(5) 0.019(4) -0.022(4) -0.014(4)
C116 0.051(4) 0.052(4) 0.050(4) 0.012(3) -0.016(3) -0.015(3)
C121 0.045(3) 0.044(3) 0.034(3) -0.009(2) -0.008(2) -0.015(2)
C122 0.053(4) 0.061(4) 0.040(3) 0.003(3) -0.017(3) -0.023(3)
C123 0.060(4) 0.078(5) 0.043(4) 0.003(3) -0.024(3) -0.013(4)
C124 0.046(4) 0.094(6) 0.047(4) -0.015(4) -0.018(3) -0.008(4)
C125 0.044(3) 0.091(5) 0.052(4) -0.015(4) -0.009(3) -0.027(4)
C126 0.045(3) 0.061(4) 0.052(4) -0.011(3) -0.011(3) -0.022(3)
C131 0.045(3) 0.037(3) 0.036(3) -0.004(2) -0.012(2) -0.017(2)
C132 0.050(3) 0.047(3) 0.039(3) -0.006(2) -0.010(2) -0.021(3)
C133 0.062(4) 0.059(4) 0.045(4) -0.012(3) -0.002(3) -0.019(3)
C134 0.080(5) 0.053(4) 0.039(3) -0.015(3) -0.009(3) -0.013(3)
C135 0.077(5) 0.046(4) 0.059(4) -0.020(3) -0.023(4) -0.014(3)
C136 0.062(4) 0.041(3) 0.046(3) -0.008(3) -0.012(3) -0.018(3)
C501 0.154(11) 0.120(10) 0.211(17) 0.009(11) -0.086(12) -0.061(9)
C502 0.185(13) 0.159(12) 0.244(17) -0.017(13) -0.078(14) -0.045(10)
C503 0.176(13) 0.180(14) 0.205(16) 0.021(12) -0.061(12) -0.058(11)
C504 0.178(13) 0.197(14) 0.250(17) 0.006(14) -0.048(14) -0.062(11)
C505 0.120(9) 0.145(11) 0.240(18) 0.030(12) -0.079(12) -0.078(9)
B1 0.037(3) 0.038(3) 0.033(3) 0.007(2) -0.015(2) -0.017(2)
_refine_ls_extinction_coef 90(10)
_refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22'
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Hg1 . Ir1 . 2.5905(16) yes
Hg1 . Cl1 . 2.367(4) yes
Ir1 . P1 2_666 2.395(3) yes
Ir1 . C3 2_666 2.024(6) yes
Ir1 . P1 . 2.356(3) yes
Ir1 . C3 . 2.047(6) yes
Ir1 . C4 . 1.945(19) yes
W1 . N11 . 2.275(4) yes
W1 . N21 . 2.213(4) yes
W1 . N31 . 2.216(4) yes
W1 . C1 . 1.838(5) yes
W1 . C5 . 1.990(6) yes
W1 . C6 . 2.005(6) yes
P1 . C111 . 1.819(6) yes
P1 . C121 . 1.834(6) yes
P1 . C131 . 1.827(6) yes
O4 . C4 . 1.156(18) yes
O5 . C5 . 1.148(7) yes
O6 . C6 . 1.144(7) yes
N11 . N12 . 1.376(6) yes
N11 . C15 . 1.353(7) yes
N12 . C13 . 1.365(6) yes
N12 . B1 . 1.546(7) yes
N21 . N22 . 1.374(6) yes
N21 . C25 . 1.352(7) yes
N22 . C23 . 1.357(7) yes
N22 . B1 . 1.546(7) yes
N31 . N32 . 1.375(6) yes
N31 . C35 . 1.347(7) yes
N32 . C33 . 1.355(7) yes
N32 . B1 . 1.535(8) yes
C1 . C2 . 1.375(8) yes
C2 . C3 . 1.209(7) yes
C13 . C14 . 1.382(8) yes
C13 . C16 . 1.492(8) yes
C14 . C15 . 1.393(8) yes
C14 . H141 . 1.000 no
C15 . C17 . 1.487(8) yes
C16 . H161 . 1.000 no
C16 . H162 . 1.000 no
C16 . H163 . 1.000 no
C17 . H171 . 1.000 no
C17 . H172 . 1.000 no
C17 . H173 . 1.000 no
C23 . C24 . 1.374(8) yes
C23 . C26 . 1.492(8) yes
C24 . C25 . 1.386(8) yes
C24 . H241 . 1.000 no
C25 . C27 . 1.497(8) yes
C26 . H261 . 1.000 no
C26 . H262 . 1.000 no
C26 . H263 . 1.000 no
C27 . H271 . 1.000 no
C27 . H272 . 1.000 no
C27 . H273 . 1.000 no
C33 . C34 . 1.362(9) yes
C33 . C36 . 1.473(9) yes
C34 . C35 . 1.405(9) yes
C34 . H341 . 1.000 no
C35 . C37 . 1.488(9) yes
C36 . H361 . 1.000 no
C36 . H362 . 1.000 no
C36 . H363 . 1.000 no
C37 . H371 . 1.000 no
C37 . H372 . 1.000 no
C37 . H373 . 1.000 no
C111 . C112 . 1.398(8) yes
C111 . C116 . 1.372(9) yes
C112 . C113 . 1.381(9) yes
C112 . H1121 . 1.000 no
C113 . C114 . 1.386(11) yes
C113 . H1131 . 1.000 no
C114 . C115 . 1.378(11) yes
C114 . H1141 . 1.000 no
C115 . C116 . 1.383(10) yes
C115 . H1151 . 1.000 no
C116 . H1161 . 1.000 no
C121 . C122 . 1.389(9) yes
C121 . C126 . 1.395(8) yes
C122 . C123 . 1.378(9) yes
C122 . H1221 . 1.000 no
C123 . C124 . 1.357(11) yes
C123 . H1231 . 1.000 no
C124 . C125 . 1.395(12) yes
C124 . H1241 . 1.000 no
C125 . C126 . 1.387(10) yes
C125 . H1251 . 1.000 no
C126 . H1261 . 1.000 no
C131 . C132 . 1.388(8) yes
C131 . C136 . 1.407(8) yes
C132 . C133 . 1.378(9) yes
C132 . H1321 . 1.000 no
C133 . C134 . 1.376(10) yes
C133 . H1331 . 1.000 no
C134 . C135 . 1.378(11) yes
C134 . H1341 . 1.000 no
C135 . C136 . 1.391(9) yes
C135 . H1351 . 1.000 no
C136 . H1361 . 1.000 no
C501 . C502 . 1.388(19) yes
C501 . H5011 . 1.000 no
C501 . H5012 . 1.000 no
C501 . H5013 . 1.000 no
C502 . C503 . 1.52(2) yes
C502 . H5021 . 1.000 no
C502 . H5022 . 1.000 no
C503 . C504 . 1.57(2) yes
C503 . H5031 . 1.000 no
C503 . H5032 . 1.000 no
C504 . C505 . 1.46(2) yes
C504 . H5041 . 1.000 no
C504 . H5042 . 1.000 no
C505 . H5051 . 1.000 no
C505 . H5052 . 1.000 no
C505 . H5053 . 1.000 no
B1 . H1 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ir1 . Hg1 . Cl1 . 178.46(16) yes
P1 2_666 Ir1 . C3 2_666 91.0(2) yes
P1 2_666 Ir1 . Hg1 . 86.78(8) yes
C3 2_666 Ir1 . Hg1 . 88.09(19) yes
P1 2_666 Ir1 . P1 . 170.71(7) yes
C3 2_666 Ir1 . P1 . 88.6(2) yes
Hg1 . Ir1 . P1 . 83.94(9) yes
P1 2_666 Ir1 . C3 . 86.99(19) yes
C3 2_666 Ir1 . C3 . 169.12(9) yes
Hg1 . Ir1 . C3 . 81.12(18) yes
P1 2_666 Ir1 . C4 . 96.1(9) yes
C3 2_666 Ir1 . C4 . 93.2(9) yes
Hg1 . Ir1 . C4 . 176.8(9) yes
P1 . Ir1 . C3 . 91.6(2) yes
P1 . Ir1 . C4 . 93.2(9) yes
C3 . Ir1 . C4 . 97.6(9) yes
N11 . W1 . N21 . 80.63(15) yes
N11 . W1 . N31 . 80.96(16) yes
N21 . W1 . N31 . 83.40(16) yes
N11 . W1 . C1 . 178.33(19) yes
N21 . W1 . C1 . 97.72(19) yes
N31 . W1 . C1 . 98.6(2) yes
N11 . W1 . C5 . 96.31(18) yes
N21 . W1 . C5 . 176.36(19) yes
N31 . W1 . C5 . 94.2(2) yes
C1 . W1 . C5 . 85.3(2) yes
N11 . W1 . C6 . 95.12(19) yes
N21 . W1 . C6 . 96.0(2) yes
N31 . W1 . C6 . 176.08(19) yes
C1 . W1 . C6 . 85.3(2) yes
C5 . W1 . C6 . 86.2(2) yes
Ir1 . P1 . C111 . 112.2(2) yes
Ir1 . P1 . C121 . 111.5(2) yes
C111 . P1 . C121 . 106.1(3) yes
Ir1 . P1 . C131 . 120.42(19) yes
C111 . P1 . C131 . 104.8(3) yes
C121 . P1 . C131 . 100.3(3) yes
W1 . N11 . N12 . 118.9(3) yes
W1 . N11 . C15 . 133.7(4) yes
N12 . N11 . C15 . 106.6(4) yes
N11 . N12 . C13 . 109.9(4) yes
N11 . N12 . B1 . 120.3(4) yes
C13 . N12 . B1 . 129.7(5) yes
W1 . N21 . N22 . 121.0(3) yes
W1 . N21 . C25 . 131.8(4) yes
N22 . N21 . C25 . 106.0(4) yes
N21 . N22 . C23 . 110.4(4) yes
N21 . N22 . B1 . 119.0(4) yes
C23 . N22 . B1 . 130.4(4) yes
W1 . N31 . N32 . 121.2(3) yes
W1 . N31 . C35 . 131.5(4) yes
N32 . N31 . C35 . 107.0(4) yes
N31 . N32 . C33 . 109.6(5) yes
N31 . N32 . B1 . 119.7(4) yes
C33 . N32 . B1 . 130.7(5) yes
W1 . C1 . C2 . 178.5(4) yes
C1 . C2 . C3 . 177.8(6) yes
Ir1 . C3 . C2 . 174.6(5) yes
Ir1 . C4 . O4 . 178(2) yes
W1 . C5 . O5 . 175.9(5) yes
W1 . C6 . O6 . 175.4(5) yes
N12 . C13 . C14 . 107.4(5) yes
N12 . C13 . C16 . 123.3(6) yes
C14 . C13 . C16 . 129.3(5) yes
C13 . C14 . C15 . 106.6(5) yes
C13 . C14 . H141 . 126.708 no
C15 . C14 . H141 . 126.707 no
C14 . C15 . N11 . 109.7(5) yes
C14 . C15 . C17 . 128.8(5) yes
N11 . C15 . C17 . 121.5(5) yes
C13 . C16 . H161 . 109.466 no
C13 . C16 . H162 . 109.467 no
H161 . C16 . H162 . 109.476 no
C13 . C16 . H163 . 109.467 no
H161 . C16 . H163 . 109.476 no
H162 . C16 . H163 . 109.476 no
C15 . C17 . H171 . 109.467 no
C15 . C17 . H172 . 109.466 no
H171 . C17 . H172 . 109.476 no
C15 . C17 . H173 . 109.467 no
H171 . C17 . H173 . 109.476 no
H172 . C17 . H173 . 109.476 no
N22 . C23 . C24 . 107.0(5) yes
N22 . C23 . C26 . 123.0(5) yes
C24 . C23 . C26 . 130.0(5) yes
C23 . C24 . C25 . 107.0(5) yes
C23 . C24 . H241 . 126.487 no
C25 . C24 . H241 . 126.487 no
C24 . C25 . N21 . 109.6(5) yes
C24 . C25 . C27 . 128.2(5) yes
N21 . C25 . C27 . 122.1(5) yes
C23 . C26 . H261 . 109.467 no
C23 . C26 . H262 . 109.467 no
H261 . C26 . H262 . 109.475 no
C23 . C26 . H263 . 109.466 no
H261 . C26 . H263 . 109.476 no
H262 . C26 . H263 . 109.476 no
C25 . C27 . H271 . 109.467 no
C25 . C27 . H272 . 109.466 no
H271 . C27 . H272 . 109.476 no
C25 . C27 . H273 . 109.467 no
H271 . C27 . H273 . 109.475 no
H272 . C27 . H273 . 109.476 no
N32 . C33 . C34 . 107.9(5) yes
N32 . C33 . C36 . 122.6(6) yes
C34 . C33 . C36 . 129.5(6) yes
C33 . C34 . C35 . 106.9(5) yes
C33 . C34 . H341 . 126.561 no
C35 . C34 . H341 . 126.562 no
C34 . C35 . N31 . 108.6(5) yes
C34 . C35 . C37 . 128.6(5) yes
N31 . C35 . C37 . 122.8(5) yes
C33 . C36 . H361 . 109.467 no
C33 . C36 . H362 . 109.466 no
H361 . C36 . H362 . 109.476 no
C33 . C36 . H363 . 109.466 no
H361 . C36 . H363 . 109.476 no
H362 . C36 . H363 . 109.476 no
C35 . C37 . H371 . 109.467 no
C35 . C37 . H372 . 109.467 no
H371 . C37 . H372 . 109.476 no
C35 . C37 . H373 . 109.467 no
H371 . C37 . H373 . 109.476 no
H372 . C37 . H373 . 109.476 no
P1 . C111 . C112 . 118.5(5) yes
P1 . C111 . C116 . 122.1(5) yes
C112 . C111 . C116 . 119.0(6) yes
C111 . C112 . C113 . 121.3(6) yes
C111 . C112 . H1121 . 119.354 no
C113 . C112 . H1121 . 119.354 no
C112 . C113 . C114 . 118.7(7) yes
C112 . C113 . H1131 . 120.659 no
C114 . C113 . H1131 . 120.658 no
C113 . C114 . C115 . 120.3(6) yes
C113 . C114 . H1141 . 119.853 no
C115 . C114 . H1141 . 119.852 no
C114 . C115 . C116 . 120.6(7) yes
C114 . C115 . H1151 . 119.713 no
C116 . C115 . H1151 . 119.712 no
C115 . C116 . C111 . 120.1(7) yes
C115 . C116 . H1161 . 119.945 no
C111 . C116 . H1161 . 119.944 no
P1 . C121 . C122 . 119.0(5) yes
P1 . C121 . C126 . 121.6(5) yes
C122 . C121 . C126 . 119.1(6) yes
C121 . C122 . C123 . 119.9(7) yes
C121 . C122 . H1221 . 120.026 no
C123 . C122 . H1221 . 120.025 no
C122 . C123 . C124 . 121.1(7) yes
C122 . C123 . H1231 . 119.461 no
C124 . C123 . H1231 . 119.459 no
C123 . C124 . C125 . 120.3(6) yes
C123 . C124 . H1241 . 119.862 no
C125 . C124 . H1241 . 119.862 no
C124 . C125 . C126 . 119.2(7) yes
C124 . C125 . H1251 . 120.397 no
C126 . C125 . H1251 . 120.397 no
C121 . C126 . C125 . 120.4(7) yes
C121 . C126 . H1261 . 119.814 no
C125 . C126 . H1261 . 119.813 no
P1 . C131 . C132 . 124.0(4) yes
P1 . C131 . C136 . 117.1(4) yes
C132 . C131 . C136 . 118.7(5) yes
C131 . C132 . C133 . 121.1(6) yes
C131 . C132 . H1321 . 119.463 no
C133 . C132 . H1321 . 119.463 no
C132 . C133 . C134 . 119.9(7) yes
C132 . C133 . H1331 . 120.034 no
C134 . C133 . H1331 . 120.034 no
C133 . C134 . C135 . 120.3(6) yes
C133 . C134 . H1341 . 119.859 no
C135 . C134 . H1341 . 119.861 no
C134 . C135 . C136 . 120.4(6) yes
C134 . C135 . H1351 . 119.792 no
C136 . C135 . H1351 . 119.792 no
C131 . C136 . C135 . 119.4(6) yes
C131 . C136 . H1361 . 120.278 no
C135 . C136 . H1361 . 120.279 no
C502 . C501 . H5011 . 109.468 no
C502 . C501 . H5012 . 109.450 no
H5011 . C501 . H5012 . 109.477 no
C502 . C501 . H5013 . 109.482 no
H5011 . C501 . H5013 . 109.475 no
H5012 . C501 . H5013 . 109.476 no
C501 . C502 . C503 . 118.5(15) yes
C501 . C502 . H5021 . 107.176 no
C503 . C502 . H5021 . 107.169 no
C501 . C502 . H5022 . 107.144 no
C503 . C502 . H5022 . 107.159 no
H5021 . C502 . H5022 . 109.467 no
C502 . C503 . C504 . 93.4(13) yes
C502 . C503 . H5031 . 113.333 no
C504 . C503 . H5031 . 113.325 no
C502 . C503 . H5032 . 113.321 no
C504 . C503 . H5032 . 113.329 no
H5031 . C503 . H5032 . 109.467 no
C503 . C504 . C505 . 109.9(15) yes
C503 . C504 . H5041 . 109.378 no
C505 . C504 . H5041 . 109.380 no
C503 . C504 . H5042 . 109.362 no
C505 . C504 . H5042 . 109.362 no
H5041 . C504 . H5042 . 109.466 no
C504 . C505 . H5051 . 109.467 no
C504 . C505 . H5052 . 109.457 no
H5051 . C505 . H5052 . 109.476 no
C504 . C505 . H5053 . 109.476 no
H5051 . C505 . H5053 . 109.476 no
H5052 . C505 . H5053 . 109.476 no
N12 . B1 . N22 . 108.3(4) yes
N12 . B1 . N32 . 108.9(4) yes
N22 . B1 . N32 . 109.1(4) yes
N12 . B1 . H1 . 110.505 no
N22 . B1 . H1 . 110.231 no
N32 . B1 . H1 . 109.734 no
#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl1 C501 3.27(2) . 1_455 no
Cl1 C504 3.35(2) . 1_455 no
Cl1 C503 3.44(3) . 2_676 no
O5 O6 3.317(8) . 2_665 no
O6 C26 3.251(7) . 2_765 no
O6 C24 3.261(7) . 2_765 no
O6 C17 3.33(1) . 2_665 no
O6 C23 3.358(6) . 2_765 no
C6 C24 3.561(7) . 2_765 no
C13 C34 3.569(7) . 2_675 no
C115 C502 3.59(3) . . no
C125 C125 3.59(2) . 2_766 no
#------------------------------------------------------------------------------
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Hg1 Ir1 P1 C111 . . . . -79.5(2) no
Hg1 Ir1 P1 C121 . . . . 161.5(2) no
Hg1 Ir1 P1 C131 . . . . 44.5(2) no
Ir1 P1 C111 C112 . . . . -65.6(7) no
Ir1 P1 C111 C116 . . . . 107.1(7) no
Ir1 P1 C121 C122 . . . . -49.1(6) no
Ir1 P1 C121 C126 . . . . 137.1(5) no
Ir1 P1 C131 C132 . . . . 5.7(6) no
Ir1 P1 C131 C136 . . . . -179.0(4) no
W1 N11 N12 C13 . . . . 170.9(3) no
W1 N11 N12 B1 . . . . -12.6(5) no
W1 N11 C15 C14 . . . . -168.9(3) no
W1 N11 C15 C17 . . . . 11.3(7) no
W1 N21 N22 C23 . . . . 167.9(4) no
W1 N21 N22 B1 . . . . -16.6(6) no
W1 N21 C25 C24 . . . . -166.3(4) no
W1 N21 C25 C27 . . . . 15.2(8) no
W1 N31 N32 C33 . . . . 172.9(4) no
W1 N31 N32 B1 . . . . -9.2(7) no
W1 N31 C35 C34 . . . . -171.5(5) no
W1 N31 C35 C37 . . . . 7(1) no
P1 C111 C112 C113 . . . . 175.6(7) no
P1 C111 C116 C115 . . . . -174.4(8) no
P1 C121 C122 C123 . . . . -174.0(5) no
P1 C121 C126 C125 . . . . 174.0(6) no
P1 C131 C132 C133 . . . . 176.8(5) no
P1 C131 C136 C135 . . . . -179.1(5) no
N11 W1 N21 N22 . . . . 51.7(4) no
N11 W1 N21 C25 . . . . -142.8(5) no
N11 W1 N31 N32 . . . . -37.7(4) no
N11 W1 N31 C35 . . . . 134.5(6) no
N11 N12 C13 C14 . . . . -0.0(5) no
N11 N12 C13 C16 . . . . -179.1(5) no
N11 N12 B1 N22 . . . . 67.2(5) no
N11 N12 B1 N32 . . . . -51.4(5) no
N11 C15 C14 C13 . . . . 0.1(6) no
N12 N11 W1 N21 . . . . -36.0(3) no
N12 N11 W1 N31 . . . . 48.8(3) no
N12 N11 W1 C5 . . . . 142.1(3) no
N12 N11 W1 C6 . . . . -131.2(3) no
N12 N11 C15 C14 . . . . -0.1(5) no
N12 N11 C15 C17 . . . . -179.9(4) no
N12 C13 C14 C15 . . . . -0.1(6) no
N12 B1 N22 N21 . . . . -50.0(6) no
N12 B1 N22 C23 . . . . 124.6(6) no
N12 B1 N32 N31 . . . . 65.4(6) no
N12 B1 N32 C33 . . . . -117.3(7) no
N21 W1 N11 C15 . . . . 131.8(4) no
N21 W1 N31 N32 . . . . 43.9(4) no
N21 W1 N31 C35 . . . . -144.0(6) no
N21 N22 C23 C24 . . . . 0.7(6) no
N21 N22 C23 C26 . . . . -179.4(6) no
N21 N22 B1 N32 . . . . 68.5(7) no
N21 C25 C24 C23 . . . . -0.4(6) no
N22 N21 W1 N31 . . . . -30.2(4) no
N22 N21 W1 C1 . . . . -128.0(4) no
N22 N21 W1 C6 . . . . 146.0(4) no
N22 N21 C25 C24 . . . . 0.8(6) no
N22 N21 C25 C27 . . . . -177.7(5) no
N22 C23 C24 C25 . . . . -0.2(7) no
N22 B1 N12 C13 . . . . -117.0(5) no
N22 B1 N32 N31 . . . . -52.8(8) no
N22 B1 N32 C33 . . . . 124.6(7) no
N31 W1 N11 C15 . . . . -143.5(4) no
N31 W1 N21 C25 . . . . 135.3(5) no
N31 N32 C33 C34 . . . . 0.1(8) no
N31 N32 C33 C36 . . . . -179.6(7) no
N31 C35 C34 C33 . . . . -1.4(8) no
N32 N31 W1 C1 . . . . 140.7(4) no
N32 N31 W1 C5 . . . . -133.4(4) no
N32 N31 C35 C34 . . . . 1.5(7) no
N32 N31 C35 C37 . . . . -179.7(7) no
N32 C33 C34 C35 . . . . 0.8(8) no
N32 B1 N12 C13 . . . . 124.4(5) no
N32 B1 N22 C23 . . . . -117.0(6) no
C1 W1 N21 C25 . . . . 37.5(5) no
C1 W1 N31 C35 . . . . -47.1(6) no
C3 Ir1 P1 C111 . . . . 1.4(3) no
C3 Ir1 P1 C121 . . . . -117.6(3) no
C3 Ir1 P1 C131 . . . . 125.4(3) no
C3 Ir1 P1 C111 . . 2_666 2_666 174.7(2) no
C3 Ir1 P1 C121 . . 2_666 2_666 -61.3(3) no
C3 Ir1 P1 C131 . . 2_666 2_666 57.4(3) no
C5 W1 N11 C15 . . . . -50.2(4) no
C5 W1 N31 C35 . . . . 38.8(6) no
C6 W1 N11 C15 . . . . 36.5(4) no
C6 W1 N21 C25 . . . . -48.5(5) no
C13 N12 N11 C15 . . . . 0.1(5) no
C13 C14 C15 C17 . . . . 179.8(5) no
C14 C13 N12 B1 . . . . -176.2(4) no
C15 N11 N12 B1 . . . . 176.6(4) no
C15 C14 C13 C16 . . . . 178.9(5) no
C16 C13 N12 B1 . . . . 4.8(8) no
C23 N22 N21 C25 . . . . -0.9(6) no
C23 C24 C25 C27 . . . . 178.0(5) no
C24 C23 N22 B1 . . . . -174.2(5) no
C25 N21 N22 B1 . . . . 174.6(4) no
C25 C24 C23 C26 . . . . 179.9(6) no
C26 C23 N22 B1 . . . . 6(1) no
C33 N32 N31 C35 . . . . -1.0(7) no
C33 C34 C35 C37 . . . . 179.9(8) no
C34 C33 N32 B1 . . . . -177.5(6) no
C35 N31 N32 B1 . . . . 176.9(6) no
C35 C34 C33 C36 . . . . -179.5(8) no
C36 C33 N32 B1 . . . . 3(1) no
C111 P1 C121 C122 . . . . -171.6(5) no
C111 P1 C121 C126 . . . . 14.5(6) no
C111 P1 C131 C132 . . . . 133.3(5) no
C111 P1 C131 C136 . . . . -51.4(6) no
C111 C112 C113 C114 . . . . -2(1) no
C111 C116 C115 C114 . . . . 0(2) no
C112 C111 P1 C121 . . . . 56.5(7) no
C112 C111 P1 C131 . . . . 162.1(6) no
C112 C111 C116 C115 . . . . -2(1) no
C112 C113 C114 C115 . . . . 0(2) no
C113 C112 C111 C116 . . . . 3(1) no
C113 C114 C115 C116 . . . . 1(2) no
C116 C111 P1 C121 . . . . -130.8(7) no
C116 C111 P1 C131 . . . . -25.2(8) no
C121 P1 C131 C132 . . . . -116.8(6) no
C121 P1 C131 C136 . . . . 58.4(5) no
C121 C122 C123 C124 . . . . -0(1) no
C121 C126 C125 C124 . . . . -0(1) no
C122 C121 P1 C131 . . . . 79.6(6) no
C122 C121 C126 C125 . . . . 0(1) no
C122 C123 C124 C125 . . . . 0(1) no
C123 C122 C121 C126 . . . . -0(1) no
C123 C124 C125 C126 . . . . -0(1) no
C126 C121 P1 C131 . . . . -94.3(6) no
C131 C132 C133 C134 . . . . 2(1) no
C131 C136 C135 C134 . . . . 2(1) no
C132 C131 C136 C135 . . . . -3.5(9) no
C132 C133 C134 C135 . . . . -3(1) no
C133 C132 C131 C136 . . . . 1.5(9) no
C133 C134 C135 C136 . . . . 1(1) no
C501 C502 C503 C504 . . . . 103(2) no
C502 C503 C504 C505 . . . . 111(2) no
#------------------------------------------------------------------------------
# start Validation Reply Form
_vrf_PLAT410_rian20a
;
PROBLEM: Short Intra H...H Contact H5022 .. H5042 .. 1.51 Ang.
RESPONSE: ... The solvate is ill-defined so these calculated H positions
are not well defined either.
;
# end Validation Reply Form
#===END