# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_biqbH
_audit_creation_date 2013-04-22
_audit_creation_method
;
Olex2 1.2-alpha
(compiled Apr 9 2013 14:06:00, GUI svn.r4458)
;
_chemical_name_common ?
_chemical_name_systematic
;
1,3-Bis(1-isoquinolyl)benzene
;
_chemical_formula_moiety 'C24 H16 N2'
_chemical_formula_sum 'C24 H16 N2'
_chemical_formula_weight 332.39
_chemical_absolute_configuration ?
_chemical_melting_point 406(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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 8
_space_group_name_H-M_alt 'C 1 m 1'
_space_group_name_Hall 'C -2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
_cell_length_a 8.6722(15)
_cell_length_b 24.417(4)
_cell_length_c 3.9321(6)
_cell_angle_alpha 90
_cell_angle_beta 103.73(4)
_cell_angle_gamma 90
_cell_volume 808.8(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 825
_cell_measurement_temperature 120(2)
_cell_measurement_theta_max 24.88
_cell_measurement_theta_min 2.56
_exptl_absorpt_coefficient_mu 0.080
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.365
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 348
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.015
_exptl_crystal_size_min 0.015
_exptl_special_details
; The data collection nominally covered full sphere of reciprocal
space, by a combination of 3 runs of narrow-frame \w-scans (scan
width 0.3\% \w, 20s exposure), every run at a different \f angle.
Crystal to detector distance 4.84 cm.
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0602
_diffrn_reflns_av_unetI/netI 0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 4
_diffrn_reflns_limit_l_min -4
_diffrn_reflns_number 3258
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.01
_diffrn_reflns_theta_max 25.01
_diffrn_reflns_theta_min 1.668
_diffrn_ambient_temperature 120(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker SMART 6000 CCD area detector'
_diffrn_measurement_method 'narrow frame \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_reflns_Friedel_coverage 0.976
_reflns_Friedel_fraction_full 0.996
_reflns_Friedel_fraction_max 0.996
_reflns_number_gt 1178
_reflns_number_total 1464
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_data_collection 'SMART version 5.625 (Bruker, 2001)'
_computing_cell_refinement 'SAINT version 7.46A (Bruker, 2007)'
_computing_data_reduction 'SAINT version 7.46A (Bruker, 2007)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement 'SHELXL-2013/2 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_refine_diff_density_max 0.162
_refine_diff_density_min -0.305
_refine_diff_density_rms 0.047
_refine_ls_abs_structure_details
; Absolute polarity undeterminable
;
_refine_ls_abs_structure_Flack ?
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 121
_refine_ls_number_reflns 1464
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0618
_refine_ls_R_factor_gt 0.0442
_refine_ls_restrained_S_all 1.039
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.1084P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1014
_refine_ls_wR_factor_ref 0.1120
_refine_special_details
;
?
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Riding coordinates:
C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
C15(H15)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.8529(4) 0.36101(14) 0.4914(9) 0.0218(9) Uani 1 1 d . . . . .
C1 C 0.8268(5) 0.45010(17) 0.2399(9) 0.0193(10) Uani 1 1 d . . . . .
C2 C 0.7558(7) 0.5000 0.2860(14) 0.0192(13) Uani 1 2 d S T P . .
H2 H 0.6572 0.5000 0.3519 0.023 Uiso 1 2 d R U P . .
C3 C 1.0437(7) 0.5000 0.1004(15) 0.0212(14) Uani 1 2 d S T P . .
H3 H 1.1428 0.5000 0.0372 0.025 Uiso 1 2 d R U P . .
C4 C 0.9726(5) 0.45072(18) 0.1457(10) 0.0192(9) Uani 1 1 d . . . . .
H4 H 1.0224 0.4172 0.1112 0.023 Uiso 1 1 d R U . . .
C7 C 0.7548(5) 0.39666(17) 0.2961(9) 0.0183(10) Uani 1 1 d . . . . .
C8 C 0.5911(5) 0.38426(18) 0.1489(10) 0.0188(9) Uani 1 1 d . . . . .
C9 C 0.4870(5) 0.41959(18) -0.0837(10) 0.0214(10) Uani 1 1 d . . . . .
H9 H 0.5255 0.4533 -0.1512 0.026 Uiso 1 1 d R U . . .
C10 C 0.3314(5) 0.40589(19) -0.2159(11) 0.0252(10) Uani 1 1 d . . . . .
H10 H 0.2632 0.4305 -0.3683 0.030 Uiso 1 1 d R U . . .
C11 C 0.2707(5) 0.35592(19) -0.1256(11) 0.0260(11) Uani 1 1 d . . . . .
H11 H 0.1621 0.3469 -0.2153 0.031 Uiso 1 1 d R U . . .
C12 C 0.3700(5) 0.31987(19) 0.0919(10) 0.0250(11) Uani 1 1 d . . . . .
H12 H 0.3298 0.2858 0.1503 0.030 Uiso 1 1 d R U . . .
C13 C 0.5315(5) 0.33303(18) 0.2303(10) 0.0213(10) Uani 1 1 d . . . . .
C14 C 0.6388(5) 0.29691(18) 0.4465(11) 0.0239(11) Uani 1 1 d . . . . .
H14 H 0.6036 0.2625 0.5125 0.029 Uiso 1 1 d R U . . .
C15 C 0.7935(5) 0.31190(17) 0.5616(11) 0.0232(10) Uani 1 1 d . . . . .
H15 H 0.8647 0.2864 0.6985 0.028 Uiso 1 1 d R U . . .
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
N1 0.021(2) 0.021(2) 0.026(2) -0.0010(16) 0.0093(16) 0.0016(16)
C1 0.018(2) 0.022(2) 0.018(2) -0.0002(17) 0.0045(17) 0.0009(19)
C2 0.018(3) 0.020(3) 0.021(3) 0.000 0.008(2) 0.000
C3 0.016(3) 0.025(4) 0.025(3) 0.000 0.011(3) 0.000
C4 0.014(2) 0.024(2) 0.020(2) -0.0036(18) 0.0046(17) 0.003(2)
C7 0.018(3) 0.019(2) 0.019(2) -0.0031(18) 0.0080(18) 0.0012(19)
C8 0.022(3) 0.017(2) 0.022(2) -0.0033(18) 0.0125(18) 0.000(2)
C9 0.026(3) 0.018(2) 0.022(2) -0.0055(18) 0.0106(19) -0.0026(19)
C10 0.024(3) 0.022(3) 0.030(2) -0.005(2) 0.007(2) 0.003(2)
C11 0.018(2) 0.033(3) 0.029(3) -0.0079(19) 0.009(2) -0.001(2)
C12 0.026(3) 0.023(3) 0.031(3) -0.008(2) 0.016(2) -0.003(2)
C13 0.026(3) 0.019(2) 0.023(2) -0.004(2) 0.0128(18) 0.000(2)
C14 0.032(3) 0.016(2) 0.028(2) 0.0002(18) 0.015(2) 0.000(2)
C15 0.028(3) 0.018(2) 0.026(2) 0.002(2) 0.010(2) 0.005(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C7 1.327(5) . ?
N1 C15 1.359(5) . ?
C2 H2 0.9501 . ?
C2 C1 1.397(5) . ?
C2 C1 1.396(5) 2_565 ?
C1 C4 1.399(5) . ?
C1 C7 1.485(6) . ?
C4 H4 0.9499 . ?
C4 C3 1.383(5) . ?
C3 C4 1.383(5) 2_565 ?
C3 H3 0.9500 . ?
C7 C8 1.433(6) . ?
C8 C9 1.415(6) . ?
C8 C13 1.419(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.368(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.407(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.378(6) . ?
C12 H12 0.9502 . ?
C12 C13 1.414(6) . ?
C13 C14 1.411(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.360(6) . ?
C15 H15 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N1 C15 118.3(4) . . ?
C1 C2 H2 119.2 . . ?
C1 C2 H2 119.2 2_565 . ?
C1 C2 C1 121.5(5) 2_565 . ?
C2 C1 C4 118.6(4) . . ?
C2 C1 C7 122.2(4) . . ?
C4 C1 C7 119.1(4) . . ?
C1 C4 H4 119.9 . . ?
C3 C4 C1 120.1(4) . . ?
C3 C4 H4 119.9 . . ?
C4 C3 C4 121.0(5) 2_565 . ?
C4 C3 H3 119.5 . . ?
C4 C3 H3 119.5 2_565 . ?
N1 C7 C1 115.3(3) . . ?
N1 C7 C8 122.2(4) . . ?
C8 C7 C1 122.5(4) . . ?
C9 C8 C7 123.4(4) . . ?
C9 C8 C13 118.2(4) . . ?
C13 C8 C7 118.3(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 121.1(4) . . ?
C10 C9 H9 119.1 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.7(4) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.6(4) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.6(4) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C8 119.6(4) . . ?
C14 C13 C8 117.6(4) . . ?
C14 C13 C12 122.8(4) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 C13 119.3(4) . . ?
C15 C14 H14 120.1 . . ?
N1 C15 C14 124.1(4) . . ?
N1 C15 H15 117.9 . . ?
C14 C15 H15 118.0 . . ?
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_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.
;
_shelxl_version_number 2013-2
_iucr_refine_instructions_details
;
TITL 08srv303 in Cm
CELL 0.71073 8.6722 24.4169 3.9321 90 103.73 90
ZERR 2 0.0015 0.0038 0.0006 0 0.04 0
LATT -7
SYMM +X,-Y,+Z
SFAC C H N
UNIT 48 32 4
L.S. 8
PLAN 5
TEMP -153
BOND $H
fmap 2
acta 50
REM I:/andrei/papers/Williams/08srv303/08srv303.hkl
WGHT 0.0293 0.1084
FVAR 0.85767
N1 3 0.85285 0.36101 0.49141 11.00000 0.02054 0.02073 0.02594 =
-0.00098 0.00927 0.00159
C1 1 0.75577 0.50000 0.28605 10.50000 0.01790 0.02027 0.02124 =
-0.00000 0.00804 0.00000
AFIX 3
H1 2 0.65721 0.50000 0.35189 10.50000 -1.20000
AFIX 0
C2 1 0.82681 0.45010 0.23990 11.00000 0.01791 0.02219 0.01789 =
-0.00021 0.00450 0.00093
C3 1 0.97257 0.45072 0.14566 11.00000 0.01426 0.02365 0.01988 =
-0.00363 0.00463 0.00320
AFIX 3
H3 2 1.02243 0.41722 0.11116 11.00000 -1.20000
AFIX 0
C4 1 1.04365 0.50000 0.10036 10.50000 0.01620 0.02541 0.02501 =
0.00000 0.01107 0.00000
AFIX 3
H4 2 1.14280 0.50000 0.03718 10.50000 -1.20000
AFIX 0
C7 1 0.75479 0.39666 0.29610 11.00000 0.01846 0.01867 0.01943 =
-0.00305 0.00799 0.00124
C8 1 0.59106 0.38426 0.14891 11.00000 0.02155 0.01698 0.02164 =
-0.00325 0.01253 -0.00002
C9 1 0.48704 0.41959 -0.08370 11.00000 0.02639 0.01806 0.02229 =
-0.00547 0.01063 -0.00258
AFIX 3
H9 2 0.52551 0.45333 -0.15124 11.00000 -1.20000
AFIX 0
C10 1 0.33140 0.40589 -0.21588 11.00000 0.02362 0.02197 0.03013 =
-0.00481 0.00663 0.00298
AFIX 3
H10 2 0.26322 0.43053 -0.36827 11.00000 -1.20000
AFIX 0
C11 1 0.27068 0.35592 -0.12565 11.00000 0.01847 0.03255 0.02858 =
-0.00795 0.00891 -0.00146
AFIX 3
H11 2 0.16209 0.34686 -0.21533 11.00000 -1.20000
AFIX 0
C12 1 0.37001 0.31987 0.09192 11.00000 0.02571 0.02344 0.03052 =
-0.00783 0.01584 -0.00334
AFIX 3
H12 2 0.32979 0.28584 0.15033 11.00000 -1.20000
AFIX 0
C13 1 0.53149 0.33303 0.23033 11.00000 0.02612 0.01865 0.02259 =
-0.00427 0.01277 0.00006
C14 1 0.63875 0.29691 0.44646 11.00000 0.03232 0.01600 0.02754 =
0.00020 0.01520 0.00017
AFIX 3
H14 2 0.60355 0.26254 0.51250 11.00000 -1.20000
AFIX 0
C15 1 0.79345 0.31190 0.56160 11.00000 0.02751 0.01830 0.02583 =
0.00182 0.01018 0.00500
AFIX 3
H15 2 0.86466 0.28635 0.69851 11.00000 -1.20000
AFIX 0
HKLF 4
END
;
_database_code_depnum_ccdc_archive 'CCDC 937441'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_2a
_audit_creation_date 2011-12-05
_audit_creation_method
;
Olex2 1.1-beta (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C35 H23 Cl N3 Rh,3(C Cl3 D)'
_chemical_formula_sum 'C38 H23 Cl10 D3 N3 Rh'
_chemical_formula_weight 985.05
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system Monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.7369(5)
_cell_length_b 20.9651(9)
_cell_length_c 15.5635(9)
_cell_angle_alpha 90.00
_cell_angle_beta 110.547(14)
_cell_angle_gamma 90.00
_cell_volume 3891.5(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9814
_cell_measurement_temperature 120
_cell_measurement_theta_max 29.93
_cell_measurement_theta_min 2.39
_exptl_absorpt_coefficient_mu 1.160
_exptl_absorpt_correction_T_max 0.9689
_exptl_absorpt_correction_T_min 0.7285
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0897 before and 0.0377 after correction.
The \l/2 correction factor is 0.0015.
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 1.00 -1.00 0.0200
-1.00 -1.00 1.00 0.0200
-1.00 1.00 1.00 0.0200
1.00 -1.00 -1.00 0.0200
-3.00 2.00 -3.00 0.1700
3.00 -2.00 3.00 0.1700
1.00 0.00 -1.00 0.0150
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.681
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description blade
_exptl_crystal_F_000 1960
_exptl_crystal_size_max 0.37
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.04
_exptl_special_details
;
The data collection nominally covered a full sphere of reciprocal space by
a combination of 3 sets of \w scans each set at different \f angles and
each scan (30 s exposure) covering -0.3\% in \w. The crystal to detector
distance was 4.85 cm. The crystal comprised a non-merohedral twin with
partially overlapping reflections, for which no satisfactory model was
found.
;
_diffrn_reflns_av_R_equivalents 0.0377
_diffrn_reflns_av_unetI/netI 0.0312
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 52935
_diffrn_reflns_theta_full 29.99
_diffrn_reflns_theta_max 29.99
_diffrn_reflns_theta_min 1.70
_diffrn_ambient_temperature 120
_diffrn_detector 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type 'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_xray_symbol K-L~3~
_diffrn_source 'sealed X-ray tube'
_diffrn_source_current 35.0
_diffrn_source_power 1.75
_diffrn_source_target Mo
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_reflns_number_gt 9377
_reflns_number_total 11310
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v7.46A (Bruker, 2008)'
_computing_data_collection 'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction 'SAINT v7.46A (Bruker, 2008)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'SHELXL-2013/2, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122'
_computing_structure_solution
'XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122'
_refine_diff_density_max 3.115
_refine_diff_density_min -1.103
_refine_diff_density_rms 0.148
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 2.047
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 504
_refine_ls_number_reflns 11310
_refine_ls_number_restraints 25
_refine_ls_R_factor_all 0.0682
_refine_ls_R_factor_gt 0.0571
_refine_ls_restrained_S_all 1.090
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+31.4764P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1498
_refine_ls_wR_factor_ref 0.1559
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.
In d-chloroform molecule DC(37)Cl~3~ atoms Cl(5), Cl(6), Cl(7) are
disordered between positions A and B with occupancies 0.88 and 0.12,
respectively. Components A were refined in anisotropic and B in isotropic
approximation. In d-chloroform molecule DC(38)Cl~3~ atoms Cl(8), C(38) and
D(38) are disordered equally between positions A and B.
All H and D atoms were treated as riding (constr), except those involved
in short intramolecular contacts, viz. H(4), H(6), H(9) and H(18) which
were refined with C---H distances restrained to 0.95 \%A and
U(iso) = 1.2\\times U(eq) of the bearing C atom.
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2. Restrained distances
C9-H9 = C6-H6 = C4-H4 = C18-H18
0.95 with sigma of 0.02
Cl5A-C37 \\sim Cl7B-C37 \\sim Cl7A-C37 \\sim Cl6B-C37 \\sim Cl6A-C37
\\sim Cl5B-C37 with sigma of 0.02
Cl10-C38B \\sim Cl10-C38A \\sim Cl9-C38A \\sim Cl9-C38B
with sigma of 0.02
3. Others
Fixed Sof: Cl5A(0.88) Cl5B(0.12) Cl6A(0.88) Cl6B(0.12) Cl7A(0.88) Cl7B(0.12)
Cl8A(0.5) Cl8B(0.5) C38A(0.5) D38A(0.5) C38B(0.5) D38B(0.5)
4.a Riding coordinates:
C5(H5), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C19(H19), C20(H20),
C21(H21), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33),
C34(H34), C35(H35), C36(D36), C37(D37), C38A(D38A), C38B(D38B)
;
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh Rh 0.88186(2) 0.32848(2) 1.59237(2) 0.01318(8) Uani 1 1 d . . . . .
Cl1 Cl 1.07255(8) 0.33320(5) 1.58403(7) 0.02072(19) Uani 1 1 d . . . . .
N1 N 0.9450(3) 0.37454(16) 1.7162(2) 0.0153(6) Uani 1 1 d . . . . .
N2 N 0.8346(3) 0.25631(16) 1.4978(2) 0.0158(6) Uani 1 1 d . . . . .
N3 N 0.8220(3) 0.40957(16) 1.5006(2) 0.0173(6) Uani 1 1 d . . . . .
C2 C 0.9195(3) 0.25696(19) 1.6732(3) 0.0160(7) Uani 1 1 d . . . . .
C1 C 0.9633(3) 0.26818(19) 1.7684(3) 0.0166(7) Uani 1 1 d . . . . .
C6 C 0.9901(4) 0.2146(2) 1.8261(3) 0.0253(9) Uani 1 1 d D . . . .
H6 H 1.021(5) 0.217(3) 1.8908(14) 0.030 Uiso 1 1 d D U . . .
C5 C 0.9626(5) 0.1543(2) 1.7880(3) 0.0316(11) Uani 1 1 d . . . . .
H5 H 0.9764 0.1186 1.8281 0.038 Uiso 1 1 d R U . . .
C4 C 0.9173(4) 0.1436(2) 1.6937(3) 0.0253(9) Uani 1 1 d D . . . .
H4 H 0.891(5) 0.1032(15) 1.669(4) 0.030 Uiso 1 1 d D U . . .
C3 C 0.9002(4) 0.1952(2) 1.6344(3) 0.0185(7) Uani 1 1 d . . . . .
C7 C 0.9777(3) 0.33705(19) 1.7910(3) 0.0153(7) Uani 1 1 d . . . . .
C8 C 1.0235(3) 0.3655(2) 1.8807(3) 0.0168(7) Uani 1 1 d . . . . .
C9 C 1.0465(4) 0.3321(2) 1.9646(3) 0.0232(8) Uani 1 1 d D . . . .
H9 H 1.021(5) 0.2894(13) 1.965(4) 0.028 Uiso 1 1 d D U . . .
C10 C 1.0939(4) 0.3627(2) 2.0473(3) 0.0271(9) Uani 1 1 d . . . . .
H10 H 1.1073 0.3392 2.1024 0.033 Uiso 1 1 d R U . . .
C11 C 1.1214(4) 0.4275(2) 2.0521(3) 0.0263(9) Uani 1 1 d . . . . .
H11 H 1.1567 0.4473 2.1101 0.032 Uiso 1 1 d R U . . .
C12 C 1.0977(4) 0.4620(2) 1.9729(3) 0.0223(8) Uani 1 1 d . . . . .
H12 H 1.1156 0.5061 1.9763 0.027 Uiso 1 1 d R U . . .
C13 C 1.0461(3) 0.4327(2) 1.8858(3) 0.0189(8) Uani 1 1 d . . . . .
C14 C 1.0125(4) 0.4689(2) 1.8042(3) 0.0203(8) Uani 1 1 d . . . . .
H14 H 1.0257 0.5135 1.8059 0.024 Uiso 1 1 d R U . . .
C15 C 0.9606(3) 0.43892(19) 1.7229(3) 0.0171(7) Uani 1 1 d . . . . .
H15 H 0.9342 0.4639 1.6685 0.021 Uiso 1 1 d R U . . .
C16 C 0.8570(3) 0.19633(19) 1.5328(3) 0.0158(7) Uani 1 1 d . . . . .
C17 C 0.8400(3) 0.14299(19) 1.4717(3) 0.0161(7) Uani 1 1 d . . . . .
C18 C 0.8772(4) 0.0802(2) 1.5003(3) 0.0211(8) Uani 1 1 d D . . . .
H18 H 0.919(4) 0.071(3) 1.5629(17) 0.025 Uiso 1 1 d D U . . .
C19 C 0.8573(4) 0.0310(2) 1.4388(3) 0.0236(8) Uani 1 1 d . . . . .
H19 H 0.8818 -0.0109 1.4600 0.028 Uiso 1 1 d R U . . .
C20 C 0.7995(4) 0.0419(2) 1.3445(3) 0.0227(8) Uani 1 1 d . . . . .
H20 H 0.7839 0.0073 1.3023 0.027 Uiso 1 1 d R U . . .
C21 C 0.7670(4) 0.1024(2) 1.3132(3) 0.0205(8) Uani 1 1 d . . . . .
H21 H 0.7294 0.1098 1.2495 0.025 Uiso 1 1 d R U . . .
C22 C 0.7879(3) 0.1542(2) 1.3754(3) 0.0172(7) Uani 1 1 d . . . . .
C23 C 0.7593(3) 0.2172(2) 1.3439(3) 0.0191(8) Uani 1 1 d . . . . .
H23 H 0.7212 0.2254 1.2805 0.023 Uiso 1 1 d R U . . .
C24 C 0.7864(4) 0.2662(2) 1.4054(3) 0.0193(8) Uani 1 1 d . . . . .
H24 H 0.7716 0.3087 1.3832 0.023 Uiso 1 1 d R U . . .
C25 C 0.7248(3) 0.33451(18) 1.5903(2) 0.0135(6) Uani 1 1 d . . . . .
C26 C 0.6728(4) 0.2944(2) 1.6355(3) 0.0197(8) Uani 1 1 d . . . . .
H26 H 0.711(5) 0.262(3) 1.675(4) 0.024 Uiso 1 1 d . U . . .
C27 C 0.5600(4) 0.3011(2) 1.6246(3) 0.0226(8) Uani 1 1 d . . . . .
H27 H 0.5266 0.2730 1.6555 0.027 Uiso 1 1 d R U . . .
C28 C 0.4950(4) 0.3492(2) 1.5675(3) 0.0239(9) Uani 1 1 d . . . . .
H28 H 0.4179 0.3537 1.5595 0.029 Uiso 1 1 d R U . . .
C29 C 0.5452(4) 0.3902(2) 1.5234(3) 0.0215(8) Uani 1 1 d . . . . .
H29 H 0.5018 0.4230 1.4851 0.026 Uiso 1 1 d R U . . .
C30 C 0.6583(3) 0.3836(2) 1.5343(3) 0.0180(7) Uani 1 1 d . . . . .
C31 C 0.7137(4) 0.4256(2) 1.4871(3) 0.0186(7) Uani 1 1 d . . . . .
C32 C 0.6637(4) 0.4775(2) 1.4322(3) 0.0240(9) Uani 1 1 d . . . . .
H32 H 0.5879 0.4883 1.4225 0.029 Uiso 1 1 d R U . . .
C33 C 0.7250(4) 0.5132(2) 1.3916(3) 0.0291(10) Uani 1 1 d . . . . .
H33 H 0.6926 0.5495 1.3553 0.035 Uiso 1 1 d R U . . .
C34 C 0.8338(4) 0.4957(2) 1.4045(3) 0.0276(9) Uani 1 1 d . . . . .
H34 H 0.8768 0.5190 1.3762 0.033 Uiso 1 1 d R U . . .
C35 C 0.8804(4) 0.4437(2) 1.4594(3) 0.0224(8) Uani 1 1 d . . . . .
H35 H 0.9554 0.4317 1.4685 0.027 Uiso 1 1 d R U . . .
Cl2 Cl 0.53458(11) 0.44923(8) 1.79415(11) 0.0438(3) Uani 1 1 d . . . . .
Cl3 Cl 0.76699(10) 0.41079(6) 1.85311(9) 0.0315(2) Uani 1 1 d . . . . .
Cl4 Cl 0.68218(11) 0.50570(6) 1.70997(8) 0.0329(3) Uani 1 1 d . . . . .
C36 C 0.6506(4) 0.4360(2) 1.7595(3) 0.0255(9) Uani 1 1 d . . . . .
D36 D 0.6306 0.4015 1.7122 0.031 Uiso 1 1 d R U . . .
Cl5A Cl 1.0007(2) 0.33299(19) 1.29890(19) 0.0879(10) Uani 0.88 1 d D . P A 1
Cl5B Cl 1.0068(10) 0.2877(7) 1.3281(9) 0.046(3) Uiso 0.12 1 d D . P A 2
Cl6A Cl 1.2254(2) 0.28009(13) 1.35893(17) 0.0596(6) Uani 0.88 1 d D . P A 1
Cl6B Cl 1.2420(11) 0.3044(7) 1.3532(11) 0.039(3) Uiso 0.12 1 d D . P A 2
Cl7A Cl 1.1875(2) 0.40910(10) 1.40536(18) 0.0626(6) Uani 0.88 1 d D . P A 1
Cl7B Cl 1.1208(17) 0.4095(6) 1.3594(13) 0.064(4) Uiso 0.12 1 d D . P A 2
C37 C 1.1318(4) 0.3306(3) 1.3860(3) 0.0346(11) Uani 1 1 d D . . . .
D37 D 1.1242 0.3148 1.4442 0.041 Uiso 1 1 d R U . A .
Cl8A Cl 1.3080(2) 0.22548(18) 1.6027(3) 0.0531(9) Uani 0.5 1 d . . P B 1
Cl8B Cl 1.3390(3) 0.1752(3) 1.5745(3) 0.0735(13) Uani 0.5 1 d . . P C 2
Cl9 Cl 1.20156(17) 0.13616(8) 1.68260(13) 0.0551(4) Uani 1 1 d D . . . .
Cl10 Cl 1.10967(14) 0.15730(9) 1.48654(13) 0.0556(4) Uani 1 1 d D . . . .
C38A C 1.1806(12) 0.1901(5) 1.5945(6) 0.034(3) Uiso 0.5 1 d D . P B 1
D38A D 1.1317 0.2247 1.6040 0.041 Uiso 0.5 1 d R U P B 1
C38B C 1.2063(13) 0.1841(7) 1.5892(7) 0.047(4) Uiso 0.5 1 d D . P C 2
D38B D 1.1921 0.2299 1.5995 0.057 Uiso 0.5 1 d R U P C 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
Rh 0.01465(13) 0.01235(13) 0.01174(13) 0.00106(10) 0.00365(10) -0.00075(10)
Cl1 0.0197(4) 0.0231(5) 0.0201(4) -0.0005(4) 0.0081(3) -0.0023(4)
N1 0.0146(14) 0.0176(15) 0.0136(14) -0.0002(12) 0.0046(12) -0.0008(12)
N2 0.0175(15) 0.0164(15) 0.0126(14) 0.0012(12) 0.0039(12) -0.0007(12)
N3 0.0214(16) 0.0150(15) 0.0129(14) 0.0011(12) 0.0029(12) -0.0014(13)
C2 0.0168(17) 0.0167(17) 0.0146(16) 0.0026(13) 0.0057(14) -0.0003(14)
C1 0.0185(18) 0.0160(17) 0.0150(17) 0.0010(13) 0.0057(14) -0.0012(14)
C6 0.036(2) 0.022(2) 0.0145(18) 0.0021(15) 0.0045(17) -0.0012(18)
C5 0.055(3) 0.018(2) 0.0146(19) 0.0057(15) 0.0027(19) -0.007(2)
C4 0.042(3) 0.0148(19) 0.0188(19) -0.0003(15) 0.0099(18) -0.0064(18)
C3 0.0207(18) 0.0191(18) 0.0138(17) 0.0010(14) 0.0036(14) -0.0020(15)
C7 0.0144(16) 0.0169(18) 0.0150(16) -0.0004(13) 0.0057(13) -0.0011(13)
C8 0.0157(17) 0.0196(18) 0.0138(16) -0.0035(14) 0.0036(14) -0.0003(14)
C9 0.029(2) 0.023(2) 0.0138(17) -0.0026(15) 0.0024(15) 0.0012(17)
C10 0.034(2) 0.029(2) 0.0152(19) -0.0011(16) 0.0038(17) 0.0032(19)
C11 0.026(2) 0.030(2) 0.0184(19) -0.0071(17) 0.0017(16) 0.0016(18)
C12 0.0219(19) 0.022(2) 0.0212(19) -0.0062(16) 0.0048(16) -0.0017(16)
C13 0.0162(17) 0.0195(19) 0.0209(19) -0.0027(15) 0.0065(15) 0.0005(14)
C14 0.0228(19) 0.0164(18) 0.0218(19) -0.0025(15) 0.0078(16) -0.0004(15)
C15 0.0173(17) 0.0165(18) 0.0171(17) -0.0002(14) 0.0056(14) -0.0005(14)
C16 0.0152(16) 0.0159(17) 0.0157(17) -0.0010(14) 0.0047(13) -0.0007(13)
C17 0.0145(17) 0.0151(17) 0.0183(17) -0.0021(14) 0.0052(14) -0.0006(13)
C18 0.024(2) 0.0173(19) 0.0203(19) -0.0001(15) 0.0058(16) 0.0028(15)
C19 0.029(2) 0.0183(19) 0.023(2) -0.0014(16) 0.0087(17) 0.0028(16)
C20 0.022(2) 0.023(2) 0.023(2) -0.0065(16) 0.0072(16) -0.0022(16)
C21 0.0211(19) 0.023(2) 0.0173(18) -0.0047(15) 0.0062(15) -0.0018(15)
C22 0.0157(17) 0.0189(18) 0.0169(17) -0.0021(14) 0.0056(14) -0.0023(14)
C23 0.0198(18) 0.0214(19) 0.0141(17) 0.0011(14) 0.0032(14) 0.0018(15)
C24 0.0214(19) 0.0192(19) 0.0147(17) 0.0029(14) 0.0031(14) 0.0007(15)
C25 0.0119(15) 0.0162(17) 0.0120(15) -0.0027(13) 0.0037(12) -0.0011(13)
C26 0.0228(19) 0.0162(18) 0.0203(19) -0.0019(15) 0.0076(16) -0.0017(15)
C27 0.0204(19) 0.022(2) 0.025(2) -0.0010(16) 0.0074(16) -0.0039(16)
C28 0.0162(18) 0.029(2) 0.025(2) -0.0069(17) 0.0051(16) -0.0030(16)
C29 0.0216(19) 0.022(2) 0.0190(18) -0.0031(15) 0.0050(15) 0.0011(16)
C30 0.0208(19) 0.0189(18) 0.0122(16) -0.0022(14) 0.0032(14) -0.0009(15)
C31 0.0224(19) 0.0164(18) 0.0160(17) 0.0004(14) 0.0054(15) 0.0017(15)
C32 0.022(2) 0.023(2) 0.024(2) 0.0065(16) 0.0051(16) 0.0043(16)
C33 0.033(2) 0.026(2) 0.025(2) 0.0129(18) 0.0058(18) 0.0027(19)
C34 0.032(2) 0.025(2) 0.025(2) 0.0095(17) 0.0087(18) -0.0033(18)
C35 0.025(2) 0.022(2) 0.0196(19) 0.0034(15) 0.0074(16) -0.0017(16)
Cl2 0.0237(6) 0.0643(10) 0.0445(7) 0.0057(7) 0.0131(5) 0.0106(6)
Cl3 0.0216(5) 0.0348(6) 0.0351(6) 0.0036(5) 0.0063(4) 0.0032(4)
Cl4 0.0391(6) 0.0271(6) 0.0294(6) -0.0017(4) 0.0081(5) 0.0014(5)
C36 0.021(2) 0.028(2) 0.025(2) -0.0074(17) 0.0044(17) 0.0023(17)
Cl5A 0.0436(11) 0.143(3) 0.0629(15) -0.0282(17) 0.0014(10) -0.0122(15)
Cl6A 0.0762(16) 0.0565(14) 0.0558(12) -0.0111(11) 0.0352(11) 0.0105(12)
Cl7A 0.0789(16) 0.0394(10) 0.0738(14) -0.0028(9) 0.0321(13) -0.0152(10)
C37 0.037(3) 0.044(3) 0.026(2) -0.005(2) 0.016(2) -0.006(2)
Cl8A 0.0250(12) 0.0546(19) 0.068(2) 0.0216(16) 0.0012(13) -0.0153(12)
Cl8B 0.0305(15) 0.126(4) 0.063(2) -0.011(2) 0.0152(15) -0.022(2)
Cl9 0.0672(11) 0.0403(8) 0.0657(11) -0.0056(7) 0.0332(9) -0.0092(8)
Cl10 0.0432(8) 0.0665(11) 0.0625(10) -0.0242(9) 0.0251(8) -0.0218(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh Cl1 2.4793(11) . ?
Rh N1 2.050(3) . ?
Rh N2 2.049(3) . ?
Rh N3 2.178(3) . ?
Rh C2 1.907(4) . ?
Rh C25 1.993(4) . ?
N1 C7 1.345(5) . ?
N1 C15 1.363(5) . ?
N2 C16 1.360(5) . ?
N2 C24 1.367(5) . ?
N3 C31 1.362(5) . ?
N3 C35 1.346(5) . ?
C2 C1 1.408(5) . ?
C2 C3 1.413(6) . ?
C1 C6 1.402(6) . ?
C1 C7 1.482(5) . ?
C6 C5 1.389(6) . ?
C5 C4 1.395(6) . ?
C4 C3 1.389(6) . ?
C3 C16 1.481(5) . ?
C7 C8 1.439(5) . ?
C8 C9 1.418(6) . ?
C8 C13 1.434(6) . ?
C9 C10 1.374(6) . ?
C10 C11 1.399(7) . ?
C11 C12 1.368(7) . ?
C12 C13 1.422(6) . ?
C13 C14 1.411(6) . ?
C14 C15 1.359(6) . ?
C16 C17 1.434(5) . ?
C17 C18 1.418(6) . ?
C17 C22 1.429(5) . ?
C18 C19 1.369(6) . ?
C19 C20 1.411(6) . ?
C20 C21 1.370(6) . ?
C21 C22 1.416(6) . ?
C22 C23 1.412(6) . ?
C23 C24 1.362(6) . ?
C25 C26 1.403(6) . ?
C25 C30 1.421(5) . ?
C26 C27 1.394(6) . ?
C27 C28 1.405(7) . ?
C28 C29 1.388(6) . ?
C29 C30 1.397(6) . ?
C30 C31 1.476(6) . ?
C31 C32 1.393(6) . ?
C32 C33 1.383(7) . ?
C33 C34 1.379(7) . ?
C34 C35 1.384(6) . ?
Cl2 C36 1.764(5) . ?
Cl3 C36 1.756(5) . ?
Cl4 C36 1.763(5) . ?
Cl5A C37 1.744(5) . ?
Cl5B C37 1.775(11) . ?
Cl6A C37 1.753(5) . ?
Cl6B C37 1.742(12) . ?
Cl7A C37 1.775(5) . ?
Cl7B C37 1.699(13) . ?
Cl8A C38A 1.747(14) . ?
Cl8B C38B 1.793(17) . ?
Cl9 C38A 1.724(10) . ?
Cl9 C38B 1.785(11) . ?
Cl10 C38A 1.746(10) . ?
Cl10 C38B 1.733(11) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Rh Cl1 87.83(10) . . ?
N1 Rh N3 100.37(13) . . ?
N2 Rh Cl1 92.19(10) . . ?
N2 Rh N1 160.48(13) . . ?
N2 Rh N3 99.12(13) . . ?
N3 Rh Cl1 93.36(10) . . ?
C2 Rh Cl1 92.39(12) . . ?
C2 Rh N1 79.96(15) . . ?
C2 Rh N2 80.54(15) . . ?
C2 Rh N3 174.25(16) . . ?
C2 Rh C25 94.54(16) . . ?
C25 Rh Cl1 173.03(11) . . ?
C25 Rh N1 92.61(14) . . ?
C25 Rh N2 89.71(14) . . ?
C25 Rh N3 79.71(15) . . ?
C7 N1 Rh 116.1(3) . . ?
C7 N1 C15 121.3(3) . . ?
C15 N1 Rh 122.5(3) . . ?
C16 N2 Rh 115.3(3) . . ?
C16 N2 C24 121.0(3) . . ?
C24 N2 Rh 123.7(3) . . ?
C31 N3 Rh 113.4(3) . . ?
C35 N3 Rh 127.0(3) . . ?
C35 N3 C31 119.6(4) . . ?
C1 C2 Rh 118.5(3) . . ?
C1 C2 C3 123.2(4) . . ?
C3 C2 Rh 118.2(3) . . ?
C2 C1 C7 112.5(3) . . ?
C6 C1 C2 117.2(4) . . ?
C6 C1 C7 130.2(4) . . ?
C5 C6 C1 119.2(4) . . ?
C6 C5 C4 122.9(4) . . ?
C3 C4 C5 119.0(4) . . ?
C2 C3 C16 112.7(4) . . ?
C4 C3 C2 117.8(4) . . ?
C4 C3 C16 129.4(4) . . ?
N1 C7 C1 112.9(3) . . ?
N1 C7 C8 119.7(4) . . ?
C8 C7 C1 127.4(4) . . ?
C9 C8 C7 124.8(4) . . ?
C9 C8 C13 117.4(4) . . ?
C13 C8 C7 117.8(4) . . ?
C10 C9 C8 120.9(4) . . ?
C9 C10 C11 121.5(4) . . ?
C12 C11 C10 119.5(4) . . ?
C11 C12 C13 120.9(4) . . ?
C12 C13 C8 119.6(4) . . ?
C14 C13 C8 119.1(4) . . ?
C14 C13 C12 121.3(4) . . ?
C15 C14 C13 119.0(4) . . ?
C14 C15 N1 122.6(4) . . ?
N2 C16 C3 112.9(3) . . ?
N2 C16 C17 119.6(4) . . ?
C17 C16 C3 127.5(4) . . ?
C18 C17 C16 124.1(4) . . ?
C18 C17 C22 117.6(4) . . ?
C22 C17 C16 118.3(4) . . ?
C19 C18 C17 121.4(4) . . ?
C18 C19 C20 120.4(4) . . ?
C21 C20 C19 120.1(4) . . ?
C20 C21 C22 120.4(4) . . ?
C21 C22 C17 119.9(4) . . ?
C23 C22 C17 119.1(4) . . ?
C23 C22 C21 121.1(4) . . ?
C24 C23 C22 119.4(4) . . ?
C23 C24 N2 122.3(4) . . ?
C26 C25 Rh 127.0(3) . . ?
C26 C25 C30 117.2(4) . . ?
C30 C25 Rh 115.8(3) . . ?
C27 C26 C25 121.8(4) . . ?
C26 C27 C28 120.1(4) . . ?
C29 C28 C27 119.1(4) . . ?
C28 C29 C30 120.8(4) . . ?
C25 C30 C31 116.8(4) . . ?
C29 C30 C25 121.0(4) . . ?
C29 C30 C31 122.2(4) . . ?
N3 C31 C30 114.3(4) . . ?
N3 C31 C32 120.6(4) . . ?
C32 C31 C30 125.2(4) . . ?
C33 C32 C31 119.5(4) . . ?
C34 C33 C32 119.3(4) . . ?
C33 C34 C35 119.4(4) . . ?
N3 C35 C34 121.6(4) . . ?
Cl3 C36 Cl2 110.3(3) . . ?
Cl3 C36 Cl4 110.9(3) . . ?
Cl4 C36 Cl2 110.3(3) . . ?
Cl5A C37 Cl6A 112.2(3) . . ?
Cl5A C37 Cl7A 108.8(3) . . ?
Cl6A C37 Cl7A 109.6(3) . . ?
Cl6B C37 Cl5B 111.3(7) . . ?
Cl7B C37 Cl5B 112.8(9) . . ?
Cl7B C37 Cl6B 104.0(9) . . ?
Cl9 C38A Cl8A 109.9(7) . . ?
Cl9 C38A Cl10 113.0(6) . . ?
Cl10 C38A Cl8A 113.0(7) . . ?
Cl9 C38B Cl8B 110.4(8) . . ?
Cl10 C38B Cl8B 104.1(8) . . ?
Cl10 C38B Cl9 110.6(7) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C37 D37 Cl1 1.00 2.52 3.421(5) 150.5 .
C38A D38A Cl1 1.00 2.38 3.280(13) 149.1 .
C38B D38B Cl1 1.00 2.61 3.547(17) 156.1 .
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_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.
;
_shelxl_version_number 2013-2
_iucr_refine_instructions_details
;
TITL 08srv302 in P2(1)/n
CELL 0.71073 12.7369 20.9651 15.5635 90 110.547 90
ZERR 4 0.0006 0.0009 0.0009 0 0.014 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N Cl Rh D
UNIT 152 92 12 40 4 12
DFIX 0.95 C9 H9 C6 H6 C4 H4 C18 H18
SADI Cl5A C37 Cl7B C37 Cl7A C37 Cl6B C37 Cl6A C37 Cl5B C37
SADI Cl10 C38B Cl10 C38A Cl9 C38A Cl9 C38B
L.S. 7
PLAN 7
TEMP -153.15
HTAB C37 Cl1
HTAB C38A Cl1
HTAB C38B Cl1
BOND
fmap 2
acta 60
OMIT 7 1 3
OMIT 2 6 8
OMIT 4 7 6
OMIT -2 2 12
OMIT 8 12 2
OMIT 2 5 8
OMIT 7 11 3
OMIT -7 5 4
OMIT 4 5 6
OMIT -4 6 14
OMIT -3 13 13
OMIT -8 2 11
OMIT 4 4 6
OMIT 7 7 3
OMIT 0 8 10
OMIT -9 3 12
OMIT 5 0 5
OMIT -2 18 12
OMIT -11 4 8
OMIT -3 6 13
OMIT -11 2 4
OMIT 13 1 0
OMIT -5 3 2
OMIT -9 2 2
OMIT -8 12 1
OMIT 0 15 3
REM I:/andrei/papers/Williams/08srv302/08srv302.hkl
WGHT 0.0393 31.4764
FVAR 0.06361
Rh 5 0.88186 0.32848 1.59237 11.00000 0.01465 0.01235 0.01174 =
0.00106 0.00365 -0.00075
Cl1 4 1.07255 0.33320 1.58403 11.00000 0.01974 0.02314 0.02014 =
-0.00050 0.00806 -0.00230
N1 3 0.94497 0.37454 1.71616 11.00000 0.01459 0.01760 0.01359 =
-0.00019 0.00462 -0.00084
N2 3 0.83457 0.25631 1.49779 11.00000 0.01747 0.01636 0.01257 =
0.00115 0.00394 -0.00070
N3 3 0.82198 0.40957 1.50065 11.00000 0.02141 0.01503 0.01289 =
0.00106 0.00288 -0.00145
C2 1 0.91952 0.25696 1.67318 11.00000 0.01678 0.01674 0.01460 =
0.00257 0.00574 -0.00025
C1 1 0.96329 0.26818 1.76840 11.00000 0.01850 0.01602 0.01502 =
0.00105 0.00569 -0.00125
C6 1 0.99006 0.21464 1.82607 11.00000 0.03640 0.02154 0.01451 =
0.00211 0.00447 -0.00118
H6 2 1.02079 0.21744 1.89082 11.00000 -1.20000
C5 1 0.96258 0.15426 1.78803 11.00000 0.05476 0.01774 0.01457 =
0.00568 0.00268 -0.00673
AFIX 3
H5 2 0.97643 0.11861 1.82814 11.00000 -1.20000
AFIX 0
C4 1 0.91728 0.14362 1.69366 11.00000 0.04176 0.01479 0.01882 =
-0.00034 0.00994 -0.00639
H4 2 0.89058 0.10320 1.66925 11.00000 -1.20000
C3 1 0.90017 0.19524 1.63438 11.00000 0.02070 0.01913 0.01382 =
0.00097 0.00363 -0.00201
C7 1 0.97766 0.33705 1.79103 11.00000 0.01440 0.01688 0.01504 =
-0.00042 0.00566 -0.00106
C8 1 1.02354 0.36547 1.88069 11.00000 0.01573 0.01957 0.01381 =
-0.00347 0.00359 -0.00032
C9 1 1.04652 0.33209 1.96456 11.00000 0.02854 0.02318 0.01376 =
-0.00258 0.00235 0.00119
H9 2 1.02140 0.28944 1.96533 11.00000 -1.20000
C10 1 1.09390 0.36268 2.04733 11.00000 0.03354 0.02884 0.01518 =
-0.00114 0.00382 0.00322
AFIX 3
H10 2 1.10726 0.33925 2.10243 11.00000 -1.20000
AFIX 0
C11 1 1.12135 0.42753 2.05213 11.00000 0.02551 0.03017 0.01840 =
-0.00706 0.00171 0.00157
AFIX 3
H11 2 1.15667 0.44730 2.11008 11.00000 -1.20000
AFIX 0
C12 1 1.09774 0.46197 1.97294 11.00000 0.02191 0.02165 0.02124 =
-0.00624 0.00476 -0.00169
AFIX 3
H12 2 1.11561 0.50610 1.97626 11.00000 -1.20000
AFIX 0
C13 1 1.04608 0.43268 1.88583 11.00000 0.01624 0.01951 0.02092 =
-0.00270 0.00649 0.00055
C14 1 1.01254 0.46886 1.80422 11.00000 0.02275 0.01639 0.02182 =
-0.00253 0.00782 -0.00038
AFIX 3
H14 2 1.02567 0.51355 1.80593 11.00000 -1.20000
AFIX 0
C15 1 0.96057 0.43892 1.72287 11.00000 0.01732 0.01649 0.01709 =
-0.00019 0.00556 -0.00048
AFIX 3
H15 2 0.93419 0.46387 1.66853 11.00000 -1.20000
AFIX 0
C16 1 0.85701 0.19633 1.53279 11.00000 0.01515 0.01587 0.01567 =
-0.00098 0.00467 -0.00073
C17 1 0.84002 0.14299 1.47170 11.00000 0.01453 0.01508 0.01826 =
-0.00210 0.00522 -0.00059
C18 1 0.87724 0.08015 1.50032 11.00000 0.02404 0.01730 0.02034 =
-0.00005 0.00582 0.00282
H18 2 0.91943 0.07139 1.56287 11.00000 -1.20000
C19 1 0.85732 0.03097 1.43880 11.00000 0.02884 0.01833 0.02318 =
-0.00143 0.00872 0.00280
AFIX 3
H19 2 0.88178 -0.01087 1.45997 11.00000 -1.20000
AFIX 0
C20 1 0.79949 0.04189 1.34446 11.00000 0.02203 0.02261 0.02281 =
-0.00648 0.00723 -0.00225
AFIX 3
H20 2 0.78394 0.00733 1.30235 11.00000 -1.20000
AFIX 0
C21 1 0.76701 0.10244 1.31319 11.00000 0.02112 0.02282 0.01730 =
-0.00473 0.00624 -0.00184
AFIX 3
H21 2 0.72936 0.10978 1.24954 11.00000 -1.20000
AFIX 0
C22 1 0.78789 0.15419 1.37542 11.00000 0.01574 0.01895 0.01689 =
-0.00209 0.00563 -0.00230
C23 1 0.75926 0.21721 1.34394 11.00000 0.01981 0.02137 0.01408 =
0.00110 0.00321 0.00182
AFIX 3
H23 2 0.72115 0.22537 1.28054 11.00000 -1.20000
AFIX 0
C24 1 0.78636 0.26619 1.40537 11.00000 0.02144 0.01915 0.01473 =
0.00287 0.00315 0.00070
AFIX 3
H24 2 0.77163 0.30870 1.38324 11.00000 -1.20000
AFIX 0
C25 1 0.72482 0.33451 1.59032 11.00000 0.01190 0.01620 0.01203 =
-0.00267 0.00373 -0.00108
C26 1 0.67280 0.29440 1.63552 11.00000 0.02279 0.01618 0.02025 =
-0.00187 0.00763 -0.00171
H26 2 0.71145 0.26244 1.67513 11.00000 -1.20000
C27 1 0.55997 0.30111 1.62463 11.00000 0.02035 0.02187 0.02514 =
-0.00098 0.00743 -0.00388
AFIX 3
H27 2 0.52658 0.27303 1.65554 11.00000 -1.20000
AFIX 0
C28 1 0.49503 0.34918 1.56747 11.00000 0.01619 0.02921 0.02472 =
-0.00692 0.00509 -0.00301
AFIX 3
H28 2 0.41795 0.35369 1.55947 11.00000 -1.20000
AFIX 0
C29 1 0.54522 0.39024 1.52340 11.00000 0.02165 0.02220 0.01900 =
-0.00305 0.00501 0.00106
AFIX 3
H29 2 0.50177 0.42301 1.48513 11.00000 -1.20000
AFIX 0
C30 1 0.65828 0.38360 1.53431 11.00000 0.02084 0.01891 0.01216 =
-0.00217 0.00324 -0.00088
C31 1 0.71373 0.42559 1.48708 11.00000 0.02245 0.01638 0.01597 =
0.00041 0.00542 0.00172
C32 1 0.66365 0.47754 1.43217 11.00000 0.02227 0.02287 0.02431 =
0.00650 0.00514 0.00432
AFIX 3
H32 2 0.58790 0.48828 1.42251 11.00000 -1.20000
AFIX 0
C33 1 0.72498 0.51321 1.39162 11.00000 0.03337 0.02572 0.02457 =
0.01294 0.00579 0.00267
AFIX 3
H33 2 0.69265 0.54948 1.35535 11.00000 -1.20000
AFIX 0
C34 1 0.83378 0.49567 1.40450 11.00000 0.03164 0.02503 0.02525 =
0.00953 0.00874 -0.00326
AFIX 3
H34 2 0.87681 0.51904 1.37622 11.00000 -1.20000
AFIX 0
C35 1 0.88036 0.44368 1.45942 11.00000 0.02517 0.02203 0.01956 =
0.00343 0.00735 -0.00168
AFIX 3
H35 2 0.95542 0.43170 1.46850 11.00000 -1.20000
AFIX 0
Cl2 4 0.53458 0.44923 1.79415 11.00000 0.02366 0.06429 0.04450 =
0.00570 0.01309 0.01061
Cl3 4 0.76699 0.41079 1.85311 11.00000 0.02160 0.03484 0.03509 =
0.00359 0.00627 0.00321
Cl4 4 0.68218 0.50570 1.70997 11.00000 0.03907 0.02714 0.02936 =
-0.00169 0.00812 0.00140
C36 1 0.65065 0.43602 1.75950 11.00000 0.02078 0.02813 0.02477 =
-0.00742 0.00436 0.00233
AFIX 3
D36 6 0.63061 0.40149 1.71218 11.00000 -1.20000
AFIX 0
PART 1
Cl5A 4 1.00066 0.33299 1.29890 10.88000 0.04361 0.14343 0.06289 =
-0.02815 0.00140 -0.01224
PART 0
PART 2
Cl5B 4 1.00679 0.28766 1.32812 10.12000 0.04602
PART 0
PART 1
Cl6A 4 1.22544 0.28009 1.35893 10.88000 0.07619 0.05653 0.05583 =
-0.01107 0.03524 0.01054
PART 0
PART 2
Cl6B 4 1.24205 0.30441 1.35321 10.12000 0.03899
PART 0
PART 1
Cl7A 4 1.18747 0.40910 1.40536 10.88000 0.07887 0.03944 0.07375 =
-0.00284 0.03211 -0.01516
PART 0
PART 2
Cl7B 4 1.12084 0.40949 1.35944 10.12000 0.06449
PART 0
C37 1 1.13184 0.33059 1.38601 11.00000 0.03749 0.04410 0.02599 =
-0.00539 0.01599 -0.00610
AFIX 3
D37 6 1.12423 0.31481 1.44418 11.00000 -1.20000
AFIX 0
PART 1
Cl8A 4 1.30800 0.22548 1.60272 10.50000 0.02499 0.05459 0.06775 =
0.02157 0.00121 -0.01529
PART 0
PART 2
Cl8B 4 1.33898 0.17523 1.57447 10.50000 0.03054 0.12601 0.06310 =
-0.01132 0.01522 -0.02185
PART 0
Cl9 4 1.20156 0.13616 1.68260 11.00000 0.06723 0.04028 0.06571 =
-0.00562 0.03319 -0.00920
Cl10 4 1.10967 0.15730 1.48654 11.00000 0.04320 0.06649 0.06246 =
-0.02415 0.02511 -0.02179
PART 1
C38A 1 1.18060 0.19013 1.59452 10.50000 0.03407
AFIX 3
D38A 6 1.13175 0.22474 1.60401 10.50000 -1.20000
AFIX 0
PART 0
PART 2
C38B 1 1.20630 0.18410 1.58923 10.50000 0.04716
AFIX 3
D38B 6 1.19206 0.22988 1.59954 10.50000 -1.20000
AFIX 0
HKLF 4
END
;
_database_code_depnum_ccdc_archive 'CCDC 937442'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_2b
_audit_creation_date 2013-05-04
_audit_creation_method
;
Olex2 1.2-alpha
(compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C35 H23 Cl Ir N3, 1.67(C H4 O), 0.67(H2 O)'
_chemical_formula_sum 'C36.67 H31 Cl Ir N3 O2.33'
_chemical_formula_weight 778.63
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
_space_group_crystal_system monoclinic
_space_group_IT_number 8
_space_group_name_H-M_alt Im
_space_group_name_Hall 'I -2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
_cell_length_a 10.6873(11)
_cell_length_b 32.019(4)
_cell_length_c 14.1789(19)
_cell_angle_alpha 90
_cell_angle_beta 104.476(13)
_cell_angle_gamma 90
_cell_volume 4697.9(10)
_cell_formula_units_Z 6
_cell_measurement_reflns_used 5305
_cell_measurement_temperature 120
_cell_measurement_theta_max 24.948
_cell_measurement_theta_min 2.497
_exptl_absorpt_coefficient_mu 4.388
_exptl_absorpt_correction_T_max 0.4285
_exptl_absorpt_correction_T_min 0.2916
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1031 before and 0.0732 after correction.
The Ratio of minimum to maximum transmission is 0.6805.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.651
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 2308
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.01
_exptl_special_details
;
The data collection nominally covered a full sphere of reciprocal space by
a combination of 4 sets of \w scans each set at different \f and/or
2\q angles and each scan (35 s exposure) covering -0.3\% in \w.
The crystal to detector distance was 4.424 cm.
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0561
_diffrn_reflns_av_unetI/netI 0.1076
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -38
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 13063
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full 24.988
_diffrn_reflns_theta_max 24.988
_diffrn_reflns_theta_min 1.614
_diffrn_ambient_temperature 120
_diffrn_detector 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'Bruker SMART CCD 1000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker SMART CCD 1000 area detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_xray_symbol K-L~3~
_diffrn_source 'sealed X-ray tube'
_diffrn_source_current 35.0
_diffrn_source_power 1.75
_diffrn_source_target Mo
_diffrn_source_voltage 50.0
_reflns_Friedel_coverage 0.839
_reflns_Friedel_fraction_full 0.842
_reflns_Friedel_fraction_max 0.842
_reflns_number_gt 6214
_reflns_number_total 7756
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v7.46A (Bruker, 2008)'
_computing_data_collection 'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction 'SAINT v7.46A (Bruker, 2008)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL-2013/2, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
;
_computing_structure_solution ?
_refine_diff_density_max 1.268
_refine_diff_density_min -1.245
_refine_diff_density_rms 0.168
_refine_ls_abs_structure_details
;
Flack x determined using 2363 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61), Hooft y=0.022(13).
;
_refine_ls_abs_structure_Flack 0.032(12)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 635
_refine_ls_number_reflns 7756
_refine_ls_number_restraints 381
_refine_ls_R_factor_all 0.0754
_refine_ls_R_factor_gt 0.0504
_refine_ls_restrained_S_all 1.004
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0326P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0972
_refine_ls_wR_factor_ref 0.1080
_refine_special_details
;
Cyclometallated ligands show strong librational motion around Ir
atoms and were refined using rigid-bond restraints (RIGU).
Methanol molecule H~3~C(62)O(3)H is disordered between two positions
related by a crystallographic mirror plane. The hydrogen atoms at O(1)
and O(3) (methanol hydroxyls) and O(4) (water molecule) were not
located and are probably disordered.
All H atoms were treated as riding, except those involved in short
intramolecular contacts, viz. H(4), H(6), H(9) and H(18), which were
refined with C---H distances restrained to 0.96 \%A and
U(iso) = 1.2\\times U(eq) of the bearing C atom.
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2. Restrained distances
C4-H4 = C6-H6 = C9-H9 = C18-H18
0.96 with sigma of 0.02
3. Others
Fixed Sof: O3(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5)
4.a Riding coordinates:
C5(H5), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C19(H19), C20(H20),
C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32),
C33(H33), C34(H34), C35(H35), C38(H38), C42(H42), C43(H43), C44(H44),
C45(H45), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C56(H56),
C57(H57), C58(H58), C59(H59), C60(H60A,H60B,H60C), O2(H2), C61(H61A,H61B,
H61C), C62(H62A,H62B,H62C)
4.b Aromatic/amide H refined with riding coordinates:
C39(H39)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.40808(6) 0.80159(2) 0.13800(5) 0.02662(19) Uani 1 1 d . . . . .
Cl1 Cl 0.1857(7) 0.80618(16) 0.1569(5) 0.0393(17) Uani 1 1 d . . . . .
N1 N 0.3511(13) 0.8326(4) 0.0085(10) 0.026(3) Uani 1 1 d . U . . .
N2 N 0.4467(16) 0.7527(5) 0.2358(13) 0.035(4) Uani 1 1 d . . . . .
N3 N 0.4700(16) 0.8547(5) 0.2350(11) 0.037(4) Uani 1 1 d . U . . .
C1 C 0.344(2) 0.7626(6) -0.0521(13) 0.030(5) Uani 1 1 d . . . . .
C2 C 0.3736(19) 0.7548(6) 0.0478(14) 0.028(4) Uani 1 1 d . U . . .
C3 C 0.389(2) 0.7146(6) 0.0904(16) 0.036(5) Uani 1 1 d . U . . .
C4 C 0.388(2) 0.6808(6) 0.0250(15) 0.040(5) Uani 1 1 d D U . . .
H4 H 0.399(19) 0.6520(19) 0.044(12) 0.048 Uiso 1 1 d D U . . .
C5 C 0.366(3) 0.6887(7) -0.0718(16) 0.057(7) Uani 1 1 d . U . . .
H5 H 0.3640 0.6657 -0.1156 0.068 Uiso 1 1 d R U . . .
C6 C 0.345(3) 0.7288(6) -0.1107(16) 0.051(6) Uani 1 1 d D U . . .
H6 H 0.36(2) 0.738(6) -0.171(8) 0.061 Uiso 1 1 d D U . . .
C7 C 0.3278(17) 0.8085(5) -0.0726(13) 0.026(4) Uani 1 1 d . U . . .
C8 C 0.2860(19) 0.8281(6) -0.1672(13) 0.029(4) Uani 1 1 d . U . . .
C9 C 0.255(2) 0.8059(7) -0.2561(15) 0.044(5) Uani 1 1 d D U . . .
H9 H 0.228(18) 0.778(2) -0.249(13) 0.053 Uiso 1 1 d D U . . .
C10 C 0.214(2) 0.8261(7) -0.3450(15) 0.048(6) Uani 1 1 d . U . . .
H10 H 0.1947 0.8101 -0.4042 0.058 Uiso 1 1 d R U . . .
C11 C 0.205(2) 0.8707(7) -0.3485(15) 0.048(6) Uani 1 1 d . U . . .
H11 H 0.1791 0.8853 -0.4094 0.057 Uiso 1 1 d R U . . .
C12 C 0.2334(19) 0.8922(6) -0.2622(13) 0.036(4) Uani 1 1 d . U . . .
H12 H 0.2249 0.9221 -0.2623 0.043 Uiso 1 1 d R U . . .
C13 C 0.2727(17) 0.8716(5) -0.1724(13) 0.026(4) Uani 1 1 d . U . . .
C14 C 0.3009(18) 0.8946(5) -0.0863(13) 0.030(4) Uani 1 1 d . U . . .
H14 H 0.2872 0.9243 -0.0888 0.035 Uiso 1 1 d R U . . .
C15 C 0.3394(18) 0.8753(5) 0.0011(13) 0.032(4) Uani 1 1 d . U . . .
H15 H 0.3620 0.8920 0.0590 0.038 Uiso 1 1 d R U . . .
C16 C 0.421(2) 0.7143(6) 0.1955(14) 0.029(5) Uani 1 1 d . . . . .
C17 C 0.426(2) 0.6793(6) 0.2597(14) 0.029(5) Uani 1 1 d . . . . .
C18 C 0.379(2) 0.6391(6) 0.2245(15) 0.039(5) Uani 1 1 d D . . . .
H18 H 0.336(16) 0.632(6) 0.159(5) 0.047 Uiso 1 1 d D U . . .
C19 C 0.394(2) 0.6049(7) 0.2871(17) 0.044(6) Uani 1 1 d . . . . .
H19 H 0.3649 0.5779 0.2608 0.053 Uiso 1 1 d R U . . .
C20 C 0.450(2) 0.6088(7) 0.3838(17) 0.042(6) Uani 1 1 d . . . . .
H20 H 0.4656 0.5846 0.4251 0.051 Uiso 1 1 d R U . . .
C21 C 0.494(2) 0.6485(6) 0.4212(16) 0.045(5) Uani 1 1 d . . . . .
H21 H 0.5247 0.6512 0.4905 0.053 Uiso 1 1 d R U . . .
C22 C 0.4782(19) 0.6840(7) 0.3620(14) 0.033(5) Uani 1 1 d . . . . .
C23 C 0.514(2) 0.7248(6) 0.3976(14) 0.037(5) Uani 1 1 d . . . . .
H23 H 0.5581 0.7285 0.4650 0.045 Uiso 1 1 d R U . . .
C24 C 0.489(2) 0.7580(7) 0.3337(16) 0.038(6) Uani 1 1 d . . . . .
H24 H 0.5000 0.7856 0.3609 0.046 Uiso 1 1 d R U . . .
C25 C 0.596(2) 0.8054(6) 0.1301(15) 0.026(4) Uani 1 1 d . U . . .
C26 C 0.657(2) 0.7816(6) 0.0777(14) 0.037(4) Uani 1 1 d . U . . .
H26 H 0.6097 0.7593 0.0395 0.045 Uiso 1 1 d R U . . .
C27 C 0.785(2) 0.7889(7) 0.0788(16) 0.047(5) Uani 1 1 d . U . . .
H27 H 0.8282 0.7712 0.0423 0.056 Uiso 1 1 d R U . . .
C28 C 0.848(2) 0.8240(7) 0.1303(15) 0.051(5) Uani 1 1 d . U . . .
H28 H 0.9370 0.8292 0.1306 0.061 Uiso 1 1 d R U . . .
C29 C 0.791(2) 0.8491(7) 0.1818(15) 0.049(5) Uani 1 1 d . U . . .
H29 H 0.8352 0.8727 0.2167 0.059 Uiso 1 1 d R U . . .
C30 C 0.6616(18) 0.8409(6) 0.1845(12) 0.034(4) Uani 1 1 d . U . . .
C31 C 0.5931(19) 0.8659(5) 0.2409(12) 0.034(4) Uani 1 1 d . U . . .
C32 C 0.645(3) 0.8985(7) 0.3045(15) 0.058(6) Uani 1 1 d . U . . .
H32 H 0.7351 0.9055 0.3163 0.070 Uiso 1 1 d R U . . .
C33 C 0.568(3) 0.9205(7) 0.3522(18) 0.065(6) Uani 1 1 d . U . . .
H33 H 0.6032 0.9432 0.3949 0.078 Uiso 1 1 d R U . . .
C34 C 0.444(3) 0.9097(7) 0.3427(16) 0.055(5) Uani 1 1 d . U . . .
H34 H 0.3881 0.9257 0.3725 0.066 Uiso 1 1 d R U . . .
C35 C 0.401(2) 0.8753(6) 0.2829(14) 0.043(5) Uani 1 1 d . U . . .
H35 H 0.3136 0.8666 0.2787 0.052 Uiso 1 1 d R U . . .
Ir2 Ir 0.09205(9) 0.5000 0.36159(7) 0.0240(3) Uani 1 2 d S T P . .
Cl2 Cl 0.3199(8) 0.5000 0.3548(6) 0.0308(19) Uani 1 2 d S T P . .
N4 N 0.0817(14) 0.5628(4) 0.3365(10) 0.027(3) Uani 1 1 d . U . . .
N5 N 0.142(2) 0.5000 0.5171(14) 0.029(4) Uani 1 2 d S TU P . .
C36 C 0.030(3) 0.5000 0.2202(18) 0.033(6) Uani 1 2 d S TU P . .
C37 C -0.0089(18) 0.5394(5) 0.1745(13) 0.024(4) Uani 1 1 d . U . . .
C38 C -0.088(2) 0.5374(6) 0.0787(13) 0.038(5) Uani 1 1 d . U . . .
H38 H -0.1149 0.5627 0.0431 0.045 Uiso 1 1 d R U . . .
C39 C -0.129(3) 0.5000 0.034(2) 0.055(9) Uani 1 2 d S TU P . .
H39 H -0.1876 0.5000 -0.0290 0.066 Uiso 1 2 calc R U P . .
C40 C 0.040(2) 0.5750(6) 0.2415(14) 0.035(4) Uani 1 1 d . U . . .
C41 C 0.049(2) 0.6164(6) 0.2128(16) 0.039(5) Uani 1 1 d . U . . .
C42 C 0.035(2) 0.6296(7) 0.1151(18) 0.053(6) Uani 1 1 d . U . . .
H42 H 0.0178 0.6086 0.0650 0.063 Uiso 1 1 d R U . . .
C43 C 0.047(2) 0.6708(7) 0.0905(19) 0.056(6) Uani 1 1 d . U . . .
H43 H 0.0299 0.6798 0.0238 0.068 Uiso 1 1 d R U . . .
C44 C 0.073(3) 0.6990(9) 0.163(2) 0.068(6) Uani 1 1 d . U . . .
H44 H 0.0858 0.7276 0.1467 0.082 Uiso 1 1 d R U . . .
C45 C 0.093(2) 0.6903(6) 0.2585(19) 0.056(6) Uani 1 1 d . U . . .
H45 H 0.1131 0.7118 0.3070 0.068 Uiso 1 1 d R U . . .
C46 C 0.087(2) 0.6471(6) 0.2856(16) 0.041(4) Uani 1 1 d . U . . .
C47 C 0.1206(18) 0.6346(5) 0.3843(14) 0.039(4) Uani 1 1 d . U . . .
H47 H 0.1405 0.6549 0.4358 0.047 Uiso 1 1 d R U . . .
C48 C 0.121(2) 0.5933(6) 0.4059(14) 0.039(5) Uani 1 1 d . U . . .
H48 H 0.1549 0.5845 0.4721 0.047 Uiso 1 1 d R U . . .
C49 C -0.078(3) 0.5000 0.391(2) 0.035(6) Uani 1 2 d S TU P . .
C50 C -0.205(3) 0.5000 0.3213(19) 0.035(5) Uani 1 2 d S TU P . .
H50 H -0.2072 0.5000 0.2532 0.042 Uiso 1 2 d R U P . .
C51 C -0.321(3) 0.5000 0.3492(19) 0.034(5) Uani 1 2 d S TU P . .
H51 H -0.4020 0.5000 0.3005 0.040 Uiso 1 2 d R U P . .
C52 C -0.321(3) 0.5000 0.4449(19) 0.036(5) Uani 1 2 d S TU P . .
H52 H -0.3987 0.5000 0.4667 0.043 Uiso 1 2 d R U P . .
C53 C -0.201(3) 0.5000 0.516(2) 0.038(5) Uani 1 2 d S TU P . .
H53 H -0.1949 0.5000 0.5848 0.045 Uiso 1 2 d R U P . .
C54 C -0.082(3) 0.5000 0.4880(17) 0.026(4) Uani 1 2 d S TU P . .
C55 C 0.042(2) 0.5000 0.5600(16) 0.025(4) Uani 1 2 d S TU P . .
C56 C 0.058(3) 0.5000 0.6591(17) 0.037(6) Uani 1 2 d S TU P . .
H56 H -0.0151 0.5000 0.6865 0.044 Uiso 1 2 d R U P . .
C57 C 0.180(3) 0.5000 0.719(2) 0.043(6) Uani 1 2 d S TU P . .
H57 H 0.1927 0.5000 0.7881 0.052 Uiso 1 2 d R U P . .
C58 C 0.286(3) 0.5000 0.6765(18) 0.044(7) Uani 1 2 d S TU P . .
H58 H 0.3724 0.5000 0.7168 0.053 Uiso 1 2 d R U P . .
C59 C 0.263(3) 0.5000 0.5760(17) 0.033(6) Uani 1 2 d S TU P . .
H59 H 0.3367 0.5000 0.5492 0.040 Uiso 1 2 d R U P . .
O1 O 0.134(3) 0.9587(7) 0.2292(17) 0.125(9) Uani 1 1 d . . . . .
C60 C 0.085(3) 0.9331(8) 0.1438(19) 0.085(10) Uani 1 1 d . . . . .
H60A H 0.0536 0.9510 0.0867 0.128 Uiso 1 1 d R U . . .
H60B H 0.0131 0.9159 0.1539 0.128 Uiso 1 1 d R U . . .
H60C H 0.1537 0.9149 0.1334 0.128 Uiso 1 1 d R U . . .
O2 O 0.123(2) 0.8393(7) 0.3412(18) 0.114(7) Uani 1 1 d . . . . .
H2 H 0.1141 0.8332 0.2824 0.170 Uiso 1 1 d R U . . .
C61 C 0.205(5) 0.8067(12) 0.404(2) 0.150(18) Uani 1 1 d . . . . .
H61A H 0.2786 0.7997 0.3777 0.225 Uiso 1 1 d R U . . .
H61B H 0.1533 0.7815 0.4060 0.225 Uiso 1 1 d R U . . .
H61C H 0.2365 0.8177 0.4705 0.225 Uiso 1 1 d R U . . .
O3 O -0.092(5) 0.9571(10) 0.456(3) 0.099(14) Uani 0.5 1 d . . P . .
C62 C -0.124(7) 0.950(2) 0.543(4) 0.10(2) Uiso 0.5 1 d . . P . .
H62A H -0.1922 0.9696 0.5465 0.147 Uiso 0.5 1 d R U P . .
H62B H -0.0491 0.9541 0.5981 0.147 Uiso 0.5 1 d R U P . .
H62C H -0.1563 0.9211 0.5450 0.147 Uiso 0.5 1 d R U P . .
O4 O 0.108(4) 0.9225(8) 0.3923(17) 0.212(19) Uani 1 1 d . . . . .
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
Ir1 0.0246(4) 0.0193(4) 0.0330(4) 0.0001(4) 0.0016(3) 0.0007(4)
Cl1 0.032(4) 0.034(3) 0.050(4) 0.001(2) 0.008(3) 0.004(2)
N1 0.021(8) 0.020(6) 0.035(7) 0.005(5) 0.004(6) 0.006(5)
N2 0.018(10) 0.036(10) 0.047(11) 0.004(8) 0.000(8) 0.008(7)
N3 0.038(7) 0.026(8) 0.044(9) 0.003(6) 0.004(6) -0.004(6)
C1 0.041(13) 0.020(10) 0.029(10) -0.003(8) 0.006(9) -0.001(8)
C2 0.024(12) 0.019(8) 0.036(10) -0.011(7) 0.000(9) 0.001(7)
C3 0.032(14) 0.023(8) 0.045(9) -0.004(7) -0.004(8) 0.003(7)
C4 0.043(14) 0.024(8) 0.045(8) -0.003(6) -0.003(8) 0.003(8)
C5 0.10(2) 0.021(9) 0.040(9) -0.008(7) 0.002(9) 0.004(9)
C6 0.08(2) 0.019(9) 0.053(12) -0.002(8) 0.023(12) 0.016(9)
C7 0.018(9) 0.027(7) 0.033(6) 0.001(5) 0.005(6) 0.004(6)
C8 0.023(11) 0.026(7) 0.036(6) 0.003(5) 0.002(6) -0.001(6)
C9 0.058(15) 0.031(9) 0.038(7) -0.002(6) 0.001(7) -0.007(8)
C10 0.062(17) 0.040(9) 0.033(8) 0.001(6) -0.007(8) -0.014(8)
C11 0.059(17) 0.037(9) 0.039(8) 0.002(6) -0.002(8) -0.011(8)
C12 0.035(12) 0.025(8) 0.042(7) 0.004(5) -0.002(6) -0.014(7)
C13 0.010(9) 0.024(6) 0.042(6) 0.001(5) 0.002(6) -0.002(5)
C14 0.025(10) 0.018(7) 0.042(7) 0.001(5) 0.001(6) 0.000(6)
C15 0.031(11) 0.020(7) 0.042(8) -0.001(5) 0.005(7) 0.009(6)
C16 0.032(13) 0.027(11) 0.028(11) -0.001(9) 0.008(9) 0.007(9)
C17 0.031(13) 0.025(11) 0.039(12) -0.002(9) 0.021(10) -0.004(9)
C18 0.036(14) 0.030(12) 0.044(12) 0.016(10) -0.005(10) 0.004(9)
C19 0.034(14) 0.037(13) 0.065(15) -0.009(11) 0.020(11) -0.007(10)
C20 0.033(13) 0.028(12) 0.065(16) 0.011(11) 0.009(11) -0.003(10)
C21 0.035(13) 0.039(13) 0.056(13) 0.015(10) 0.006(10) 0.001(10)
C22 0.020(11) 0.034(12) 0.041(12) 0.001(9) 0.002(9) 0.000(8)
C23 0.039(14) 0.034(12) 0.031(11) -0.004(9) -0.005(9) -0.005(9)
C24 0.046(16) 0.030(13) 0.045(13) -0.012(10) 0.025(11) -0.012(10)
C25 0.029(9) 0.028(8) 0.020(8) 0.019(6) 0.004(7) 0.001(6)
C26 0.037(9) 0.036(9) 0.042(9) 0.014(7) 0.017(7) 0.008(7)
C27 0.035(9) 0.048(10) 0.060(11) 0.027(8) 0.017(8) 0.010(7)
C28 0.033(9) 0.060(11) 0.059(11) 0.023(8) 0.010(8) 0.005(7)
C29 0.035(8) 0.055(10) 0.056(11) 0.016(8) 0.007(7) -0.004(7)
C30 0.033(8) 0.034(8) 0.033(8) 0.015(6) 0.002(6) -0.005(6)
C31 0.035(8) 0.028(8) 0.035(8) 0.014(6) 0.000(6) -0.003(6)
C32 0.063(11) 0.050(10) 0.056(11) -0.007(9) 0.004(8) -0.018(8)
C33 0.079(12) 0.050(11) 0.062(12) -0.012(10) 0.012(10) -0.019(9)
C34 0.078(12) 0.037(10) 0.049(11) -0.008(9) 0.013(9) -0.009(8)
C35 0.048(10) 0.033(9) 0.045(10) -0.001(7) 0.007(8) 0.002(7)
Ir2 0.0268(7) 0.0157(5) 0.0272(6) 0.000 0.0027(5) 0.000
Cl2 0.027(5) 0.021(4) 0.045(5) 0.000 0.008(4) 0.000
N4 0.022(8) 0.019(6) 0.037(6) -0.001(5) 0.001(5) -0.002(5)
N5 0.034(8) 0.027(12) 0.021(8) 0.000 -0.003(6) 0.000
C36 0.038(15) 0.028(9) 0.034(11) 0.000 0.009(10) 0.000
C37 0.023(9) 0.024(7) 0.028(7) 0.005(5) 0.009(6) -0.001(5)
C38 0.044(11) 0.033(9) 0.033(7) 0.004(6) 0.003(7) -0.003(7)
C39 0.08(2) 0.029(11) 0.041(13) 0.000 -0.015(13) 0.000
C40 0.040(12) 0.020(6) 0.040(7) 0.004(5) 0.001(6) 0.003(6)
C41 0.030(12) 0.021(7) 0.065(8) 0.011(5) 0.010(7) 0.005(6)
C42 0.052(16) 0.036(9) 0.065(9) 0.021(7) 0.006(8) 0.001(8)
C43 0.041(15) 0.042(9) 0.080(11) 0.028(7) 0.003(10) 0.001(9)
C44 0.062(17) 0.044(10) 0.092(11) 0.025(8) 0.008(10) -0.004(10)
C45 0.049(15) 0.026(8) 0.089(11) 0.013(7) 0.009(9) -0.003(7)
C46 0.025(11) 0.028(7) 0.071(8) 0.003(6) 0.013(7) -0.005(6)
C47 0.031(12) 0.018(7) 0.065(9) -0.008(6) 0.006(7) -0.007(6)
C48 0.044(13) 0.022(7) 0.044(8) -0.008(6) -0.001(8) -0.008(7)
C49 0.053(12) 0.016(14) 0.031(9) 0.000 0.004(7) 0.000
C50 0.048(11) 0.023(13) 0.031(10) 0.000 0.003(8) 0.000
C51 0.049(12) 0.007(12) 0.042(10) 0.000 0.007(8) 0.000
C52 0.046(11) 0.018(13) 0.043(10) 0.000 0.009(8) 0.000
C53 0.043(9) 0.029(14) 0.039(10) 0.000 0.008(7) 0.000
C54 0.038(8) 0.005(11) 0.031(8) 0.000 0.001(6) 0.000
C55 0.038(8) 0.006(10) 0.027(7) 0.000 0.002(6) 0.000
C56 0.041(11) 0.041(16) 0.024(8) 0.000 -0.001(6) 0.000
C57 0.047(11) 0.047(18) 0.030(9) 0.000 -0.002(7) 0.000
C58 0.043(12) 0.057(19) 0.023(9) 0.000 -0.007(7) 0.000
C59 0.033(10) 0.036(15) 0.025(9) 0.000 -0.005(7) 0.000
O1 0.15(3) 0.084(17) 0.117(19) -0.044(14) 0.001(16) 0.026(15)
C60 0.13(3) 0.060(19) 0.07(2) 0.024(15) 0.048(19) 0.028(18)
O2 0.092(19) 0.116(19) 0.14(2) -0.031(15) 0.038(14) -0.013(14)
C61 0.25(6) 0.15(4) 0.06(2) 0.03(2) 0.05(3) -0.02(4)
O3 0.15(4) 0.05(2) 0.09(3) -0.020(18) 0.02(3) -0.04(2)
O4 0.41(6) 0.09(2) 0.10(2) 0.006(15) 0.00(3) -0.03(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 Cl1 2.462(7) . ?
Ir1 N1 2.043(13) . ?
Ir1 N2 2.064(17) . ?
Ir1 N3 2.183(16) . ?
Ir1 C2 1.945(17) . ?
Ir1 C25 2.04(2) . ?
N1 C7 1.36(2) . ?
N1 C15 1.37(2) . ?
N2 C16 1.36(2) . ?
N2 C24 1.36(3) . ?
N3 C31 1.35(2) . ?
N3 C35 1.30(3) . ?
C1 C2 1.40(2) . ?
C1 C6 1.36(3) . ?
C1 C7 1.50(2) . ?
C2 C3 1.41(3) . ?
C3 C4 1.42(3) . ?
C3 C16 1.44(2) . ?
C4 C5 1.36(3) . ?
C5 C6 1.39(3) . ?
C7 C8 1.45(2) . ?
C8 C9 1.41(3) . ?
C8 C13 1.40(2) . ?
C9 C10 1.39(3) . ?
C10 C11 1.43(3) . ?
C11 C12 1.37(3) . ?
C12 C13 1.40(2) . ?
C13 C14 1.39(2) . ?
C14 C15 1.35(2) . ?
C16 C17 1.44(3) . ?
C17 C18 1.43(3) . ?
C17 C22 1.43(3) . ?
C18 C19 1.39(3) . ?
C19 C20 1.36(3) . ?
C20 C21 1.41(3) . ?
C21 C22 1.40(3) . ?
C22 C23 1.42(3) . ?
C23 C24 1.38(3) . ?
C25 C26 1.34(3) . ?
C25 C30 1.45(3) . ?
C26 C27 1.39(3) . ?
C27 C28 1.41(3) . ?
C28 C29 1.33(3) . ?
C29 C30 1.42(3) . ?
C30 C31 1.45(3) . ?
C31 C32 1.40(3) . ?
C32 C33 1.38(3) . ?
C33 C34 1.35(3) . ?
C34 C35 1.40(3) . ?
Ir2 Cl2 2.461(9) . ?
Ir2 N4 2.041(13) 2_565 ?
Ir2 N4 2.040(13) . ?
Ir2 N5 2.13(2) . ?
Ir2 C36 1.95(3) . ?
Ir2 C49 1.96(4) . ?
N4 C40 1.37(2) . ?
N4 C48 1.38(2) . ?
N5 C55 1.36(3) . ?
N5 C59 1.35(3) . ?
C36 C37 1.43(2) . ?
C36 C37 1.43(2) 2_565 ?
C37 C38 1.41(2) . ?
C37 C40 1.49(3) . ?
C38 C39 1.38(2) . ?
C39 C38 1.38(2) 2_565 ?
C40 C41 1.40(3) . ?
C41 C42 1.42(3) . ?
C41 C46 1.41(3) . ?
C42 C43 1.38(3) . ?
C43 C44 1.34(3) . ?
C44 C45 1.35(3) . ?
C45 C46 1.44(3) . ?
C46 C47 1.41(3) . ?
C47 C48 1.36(2) . ?
C49 C50 1.46(4) . ?
C49 C54 1.39(4) . ?
C50 C51 1.40(4) . ?
C51 C52 1.35(3) . ?
C52 C53 1.42(4) . ?
C53 C54 1.42(4) . ?
C54 C55 1.46(3) . ?
C55 C56 1.37(3) . ?
C56 C57 1.36(4) . ?
C57 C58 1.40(4) . ?
C58 C59 1.38(3) . ?
O1 C60 1.45(3) . ?
O2 C61 1.51(4) . ?
O3 C62 1.39(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ir1 Cl1 89.4(4) . . ?
N1 Ir1 N2 159.7(6) . . ?
N1 Ir1 N3 99.4(6) . . ?
N2 Ir1 Cl1 90.5(5) . . ?
N2 Ir1 N3 100.9(7) . . ?
N3 Ir1 Cl1 91.9(5) . . ?
C2 Ir1 Cl1 95.1(6) . . ?
C2 Ir1 N1 79.6(7) . . ?
C2 Ir1 N2 80.2(6) . . ?
C2 Ir1 N3 172.9(8) . . ?
C2 Ir1 C25 92.1(8) . . ?
C25 Ir1 Cl1 172.5(6) . . ?
C25 Ir1 N1 89.9(7) . . ?
C25 Ir1 N2 92.7(7) . . ?
C25 Ir1 N3 80.8(7) . . ?
C7 N1 Ir1 115.8(11) . . ?
C7 N1 C15 120.6(14) . . ?
C15 N1 Ir1 123.7(12) . . ?
C16 N2 Ir1 114.8(13) . . ?
C16 N2 C24 121.7(18) . . ?
C24 N2 Ir1 123.5(14) . . ?
C31 N3 Ir1 112.6(13) . . ?
C35 N3 Ir1 127.0(15) . . ?
C35 N3 C31 120.4(19) . . ?
C2 C1 C7 111.0(15) . . ?
C6 C1 C2 116.2(17) . . ?
C6 C1 C7 132.6(18) . . ?
C1 C2 Ir1 119.1(13) . . ?
C1 C2 C3 124.8(17) . . ?
C3 C2 Ir1 116.0(14) . . ?
C2 C3 C4 116(2) . . ?
C2 C3 C16 115(2) . . ?
C4 C3 C16 129(2) . . ?
C5 C4 C3 119(2) . . ?
C4 C5 C6 123(2) . . ?
C1 C6 C5 121(2) . . ?
N1 C7 C1 114.0(15) . . ?
N1 C7 C8 119.2(15) . . ?
C8 C7 C1 126.8(15) . . ?
C9 C8 C7 123.9(17) . . ?
C13 C8 C7 118.9(16) . . ?
C13 C8 C9 117.1(17) . . ?
C10 C9 C8 122(2) . . ?
C9 C10 C11 120.0(19) . . ?
C12 C11 C10 118.2(19) . . ?
C11 C12 C13 121.6(19) . . ?
C8 C13 C12 121.2(17) . . ?
C14 C13 C8 118.9(16) . . ?
C14 C13 C12 119.8(17) . . ?
C15 C14 C13 120.7(17) . . ?
C14 C15 N1 121.7(17) . . ?
N2 C16 C3 113.6(19) . . ?
N2 C16 C17 117.9(18) . . ?
C17 C16 C3 128(2) . . ?
C18 C17 C16 121.9(19) . . ?
C18 C17 C22 117.7(18) . . ?
C22 C17 C16 120.4(18) . . ?
C19 C18 C17 121(2) . . ?
C20 C19 C18 121(2) . . ?
C19 C20 C21 119(2) . . ?
C22 C21 C20 122(2) . . ?
C21 C22 C17 118.9(19) . . ?
C21 C22 C23 123.7(19) . . ?
C23 C22 C17 117.4(18) . . ?
C24 C23 C22 119.0(18) . . ?
N2 C24 C23 122.4(19) . . ?
C26 C25 Ir1 128.0(17) . . ?
C26 C25 C30 120(2) . . ?
C30 C25 Ir1 111.7(15) . . ?
C25 C26 C27 121(2) . . ?
C26 C27 C28 119(2) . . ?
C29 C28 C27 122(2) . . ?
C28 C29 C30 119(2) . . ?
C25 C30 C31 118.7(18) . . ?
C29 C30 C25 118.4(19) . . ?
C29 C30 C31 122.8(18) . . ?
N3 C31 C30 116.0(16) . . ?
N3 C31 C32 117.6(19) . . ?
C32 C31 C30 126(2) . . ?
C33 C32 C31 120(2) . . ?
C34 C33 C32 121(2) . . ?
C33 C34 C35 115(2) . . ?
N3 C35 C34 125(2) . . ?
N4 Ir2 Cl2 90.2(4) 2_565 . ?
N4 Ir2 Cl2 90.2(4) . . ?
N4 Ir2 N4 160.5(8) . 2_565 ?
N4 Ir2 N5 99.7(4) 2_565 . ?
N4 Ir2 N5 99.7(4) . . ?
N5 Ir2 Cl2 92.5(6) . . ?
C36 Ir2 Cl2 92.7(9) . . ?
C36 Ir2 N4 80.3(4) . 2_565 ?
C36 Ir2 N4 80.3(4) . . ?
C36 Ir2 N5 174.8(11) . . ?
C36 Ir2 C49 97.0(12) . . ?
C49 Ir2 Cl2 170.3(9) . . ?
C49 Ir2 N4 91.4(5) . . ?
C49 Ir2 N4 91.4(5) . 2_565 ?
C49 Ir2 N5 77.7(10) . . ?
C40 N4 Ir2 116.3(11) . . ?
C40 N4 C48 118.0(15) . . ?
C48 N4 Ir2 125.5(12) . . ?
C55 N5 Ir2 116.0(16) . . ?
C59 N5 Ir2 126.5(19) . . ?
C59 N5 C55 117(2) . . ?
C37 C36 Ir2 116.8(12) . . ?
C37 C36 Ir2 116.8(12) 2_565 . ?
C37 C36 C37 124(2) 2_565 . ?
C36 C37 C40 111.7(16) . . ?
C38 C37 C36 115.5(17) . . ?
C38 C37 C40 132.7(16) . . ?
C39 C38 C37 122.1(19) . . ?
C38 C39 C38 121(3) 2_565 . ?
N4 C40 C37 112.8(15) . . ?
N4 C40 C41 121.8(18) . . ?
C41 C40 C37 125.3(17) . . ?
C40 C41 C42 125(2) . . ?
C40 C41 C46 118.4(19) . . ?
C46 C41 C42 116.8(19) . . ?
C43 C42 C41 122(2) . . ?
C44 C43 C42 118(2) . . ?
C43 C44 C45 125(3) . . ?
C44 C45 C46 117(2) . . ?
C41 C46 C45 120(2) . . ?
C41 C46 C47 118.9(17) . . ?
C47 C46 C45 121.3(19) . . ?
C48 C47 C46 119.0(18) . . ?
C47 C48 N4 123.2(18) . . ?
C50 C49 Ir2 127(2) . . ?
C54 C49 Ir2 118(2) . . ?
C54 C49 C50 114(3) . . ?
C51 C50 C49 123(3) . . ?
C52 C51 C50 120(3) . . ?
C51 C52 C53 120(3) . . ?
C52 C53 C54 121(2) . . ?
C49 C54 C53 122(3) . . ?
C49 C54 C55 116(3) . . ?
C53 C54 C55 121(2) . . ?
N5 C55 C54 112(2) . . ?
N5 C55 C56 123(2) . . ?
C56 C55 C54 126(2) . . ?
C57 C56 C55 120(3) . . ?
C56 C57 C58 119(3) . . ?
C59 C58 C57 119(3) . . ?
N5 C59 C58 122(3) . . ?
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_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.
;
_shelxl_version_number 2013-2
_iucr_refine_instructions_details
;
TITL 08srv423 in Im
CELL 0.71073 10.6873 32.019 14.1789 90 104.476 90
ZERR 6 0.0011 0.004 0.0019 0 0.013 0
LATT -2
SYMM +X,-Y,+Z
SFAC C H N O Cl Ir
UNIT 220 186 18 14 6 6
EQIV $1 +X,2-Y,+Z
DFIX 0.96 C4 H4 C6 H6 C9 H9 C18 H18
L.S. 7
PLAN 6
TEMP -153
RTAB D-A O1 O4
RTAB D-A O2 O4
RTAB D-A O3 O4
RTAB D-A O1 O1_$1
RTAB D-A O3 O3_$1
RIGU C25 > C35 N3
RIGU N1 N2 C2 > C15
RIGU C49 > C59 N5
RIGU N4 C36 > C48
BOND
fmap 2
acta 49.976
OMIT 0 2 0
REM I:/andrei/papers/Williams/08srv423/08srv423.hkl
WGHT 0.0326
FVAR 0.10674
Ir1 6 0.40808 0.80159 0.13800 11.00000 0.02455 0.01925 0.03305 =
0.00009 0.00157 0.00071
Cl1 5 0.18568 0.80618 0.15690 11.00000 0.03206 0.03422 0.05034 =
0.00061 0.00785 0.00386
N1 3 0.35109 0.83264 0.00849 11.00000 0.02125 0.02013 0.03451 =
0.00477 0.00392 0.00610
N2 3 0.44673 0.75268 0.23581 11.00000 0.01760 0.03563 0.04683 =
0.00369 0.00026 0.00792
N3 3 0.47000 0.85468 0.23502 11.00000 0.03823 0.02624 0.04360 =
0.00279 0.00394 -0.00424
C1 1 0.34434 0.76259 -0.05209 11.00000 0.04085 0.01973 0.02895 =
-0.00294 0.00556 -0.00145
C2 1 0.37360 0.75475 0.04785 11.00000 0.02359 0.01854 0.03628 =
-0.01089 -0.00033 0.00096
C3 1 0.38918 0.71456 0.09044 11.00000 0.03176 0.02273 0.04496 =
-0.00355 -0.00444 0.00286
C4 1 0.38764 0.68078 0.02497 11.00000 0.04257 0.02439 0.04489 =
-0.00333 -0.00271 0.00315
H4 2 0.39936 0.65196 0.04436 11.00000 -1.20000
C5 1 0.36565 0.68873 -0.07180 11.00000 0.10073 0.02095 0.04018 =
-0.00795 0.00155 0.00368
AFIX 3
H5 2 0.36404 0.66573 -0.11558 11.00000 -1.20000
AFIX 0
C6 1 0.34460 0.72884 -0.11066 11.00000 0.08408 0.01904 0.05273 =
-0.00216 0.02260 0.01650
H6 2 0.35836 0.73816 -0.17126 11.00000 -1.20000
C7 1 0.32782 0.80849 -0.07256 11.00000 0.01784 0.02749 0.03298 =
0.00119 0.00515 0.00376
C8 1 0.28597 0.82808 -0.16719 11.00000 0.02267 0.02565 0.03595 =
0.00309 0.00228 -0.00117
C9 1 0.25509 0.80588 -0.25606 11.00000 0.05779 0.03136 0.03805 =
-0.00155 0.00106 -0.00747
H9 2 0.22777 0.77776 -0.24850 11.00000 -1.20000
C10 1 0.21395 0.82606 -0.34496 11.00000 0.06155 0.03963 0.03319 =
0.00067 -0.00722 -0.01409
AFIX 3
H10 2 0.19474 0.81013 -0.40420 11.00000 -1.20000
AFIX 0
C11 1 0.20457 0.87066 -0.34851 11.00000 0.05867 0.03703 0.03943 =
0.00161 -0.00183 -0.01124
AFIX 3
H11 2 0.17907 0.88529 -0.40937 11.00000 -1.20000
AFIX 0
C12 1 0.23339 0.89220 -0.26217 11.00000 0.03485 0.02540 0.04171 =
0.00443 -0.00227 -0.01441
AFIX 3
H12 2 0.22495 0.92205 -0.26234 11.00000 -1.20000
AFIX 0
C13 1 0.27274 0.87162 -0.17236 11.00000 0.01044 0.02449 0.04171 =
0.00107 0.00221 -0.00162
C14 1 0.30087 0.89462 -0.08634 11.00000 0.02493 0.01800 0.04153 =
0.00089 0.00069 -0.00008
AFIX 3
H14 2 0.28721 0.92429 -0.08879 11.00000 -1.20000
AFIX 0
C15 1 0.33937 0.87531 0.00105 11.00000 0.03113 0.01958 0.04205 =
-0.00073 0.00466 0.00888
AFIX 3
H15 2 0.36202 0.89205 0.05897 11.00000 -1.20000
AFIX 0
C16 1 0.42115 0.71428 0.19546 11.00000 0.03159 0.02665 0.02826 =
-0.00145 0.00818 0.00711
C17 1 0.42603 0.67929 0.25970 11.00000 0.03105 0.02475 0.03884 =
-0.00203 0.02107 -0.00406
C18 1 0.37861 0.63912 0.22455 11.00000 0.03589 0.03025 0.04428 =
0.01597 -0.00474 0.00393
H18 2 0.33563 0.63223 0.15857 11.00000 -1.20000
C19 1 0.39398 0.60486 0.28707 11.00000 0.03419 0.03668 0.06469 =
-0.00887 0.01993 -0.00692
AFIX 3
H19 2 0.36490 0.57791 0.26082 11.00000 -1.20000
AFIX 0
C20 1 0.45032 0.60883 0.38377 11.00000 0.03263 0.02807 0.06490 =
0.01098 0.00881 -0.00315
AFIX 3
H20 2 0.46564 0.58463 0.42506 11.00000 -1.20000
AFIX 0
C21 1 0.49361 0.64851 0.42117 11.00000 0.03500 0.03942 0.05622 =
0.01547 0.00586 0.00065
AFIX 3
H21 2 0.52466 0.65124 0.49054 11.00000 -1.20000
AFIX 0
C22 1 0.47824 0.68397 0.36202 11.00000 0.01977 0.03396 0.04100 =
0.00126 0.00192 -0.00002
C23 1 0.51441 0.72479 0.39755 11.00000 0.03899 0.03426 0.03082 =
-0.00422 -0.00525 -0.00469
AFIX 3
H23 2 0.55810 0.72852 0.46495 11.00000 -1.20000
AFIX 0
C24 1 0.48888 0.75796 0.33368 11.00000 0.04606 0.03035 0.04476 =
-0.01223 0.02499 -0.01178
AFIX 3
H24 2 0.49999 0.78559 0.36091 11.00000 -1.20000
AFIX 0
C25 1 0.59592 0.80538 0.13012 11.00000 0.02867 0.02752 0.02035 =
0.01884 0.00391 0.00058
C26 1 0.65650 0.78165 0.07773 11.00000 0.03709 0.03643 0.04178 =
0.01392 0.01737 0.00774
AFIX 3
H26 2 0.60971 0.75928 0.03948 11.00000 -1.20000
AFIX 0
C27 1 0.78537 0.78892 0.07881 11.00000 0.03500 0.04823 0.06013 =
0.02657 0.01725 0.01011
AFIX 3
H27 2 0.82825 0.77116 0.04228 11.00000 -1.20000
AFIX 0
C28 1 0.84841 0.82399 0.13025 11.00000 0.03270 0.05968 0.05889 =
0.02330 0.01002 0.00472
AFIX 3
H28 2 0.93699 0.82922 0.13064 11.00000 -1.20000
AFIX 0
C29 1 0.79103 0.84906 0.18180 11.00000 0.03503 0.05505 0.05570 =
0.01623 0.00715 -0.00438
AFIX 3
H29 2 0.83516 0.87266 0.21674 11.00000 -1.20000
AFIX 0
C30 1 0.66163 0.84087 0.18451 11.00000 0.03290 0.03370 0.03323 =
0.01472 0.00208 -0.00458
C31 1 0.59305 0.86593 0.24086 11.00000 0.03491 0.02781 0.03454 =
0.01424 -0.00005 -0.00321
C32 1 0.64509 0.89852 0.30451 11.00000 0.06282 0.05037 0.05564 =
-0.00749 0.00417 -0.01811
AFIX 3
H32 2 0.73508 0.90550 0.31634 11.00000 -1.20000
AFIX 0
C33 1 0.56849 0.92046 0.35224 11.00000 0.07906 0.05019 0.06189 =
-0.01205 0.01222 -0.01856
AFIX 3
H33 2 0.60319 0.94322 0.39487 11.00000 -1.20000
AFIX 0
C34 1 0.44385 0.90973 0.34265 11.00000 0.07839 0.03667 0.04895 =
-0.00786 0.01282 -0.00907
AFIX 3
H34 2 0.38807 0.92566 0.37250 11.00000 -1.20000
AFIX 0
C35 1 0.40075 0.87535 0.28289 11.00000 0.04806 0.03346 0.04473 =
-0.00133 0.00684 0.00193
AFIX 3
H35 2 0.31356 0.86662 0.27873 11.00000 -1.20000
AFIX 0
Ir2 6 0.09205 0.50000 0.36159 10.50000 0.02682 0.01574 0.02717 =
0.00000 0.00269 0.00000
Cl2 5 0.31990 0.50000 0.35475 10.50000 0.02657 0.02051 0.04476 =
0.00000 0.00767 0.00000
N4 3 0.08169 0.56281 0.33651 11.00000 0.02211 0.01872 0.03745 =
-0.00059 0.00096 -0.00220
N5 3 0.14236 0.50000 0.51708 10.50000 0.03419 0.02685 0.02075 =
0.00000 -0.00290 0.00000
C36 1 0.02966 0.50000 0.22018 10.50000 0.03755 0.02774 0.03425 =
0.00000 0.00921 0.00000
C37 1 -0.00888 0.53943 0.17452 11.00000 0.02272 0.02434 0.02779 =
0.00512 0.00929 -0.00118
C38 1 -0.08803 0.53741 0.07868 11.00000 0.04396 0.03263 0.03308 =
0.00434 0.00261 -0.00259
AFIX 3
H38 2 -0.11489 0.56273 0.04307 11.00000 -1.20000
AFIX 0
C39 1 -0.12950 0.50000 0.03385 10.50000 0.07866 0.02920 0.04141 =
0.00000 -0.01451 0.00000
AFIX 43
H39 2 -0.18760 0.50000 -0.02897 10.50000 -1.20000
AFIX 0
C40 1 0.03971 0.57496 0.24154 11.00000 0.04037 0.02010 0.03970 =
0.00412 0.00086 0.00317
C41 1 0.04932 0.61645 0.21278 11.00000 0.03048 0.02106 0.06452 =
0.01116 0.00963 0.00541
C42 1 0.03456 0.62958 0.11509 11.00000 0.05233 0.03642 0.06513 =
0.02138 0.00591 0.00078
AFIX 3
H42 2 0.01776 0.60864 0.06503 11.00000 -1.20000
AFIX 0
C43 1 0.04697 0.67076 0.09045 11.00000 0.04114 0.04188 0.07963 =
0.02822 0.00300 0.00141
AFIX 3
H43 2 0.02986 0.67976 0.02382 11.00000 -1.20000
AFIX 0
C44 1 0.07342 0.69896 0.16278 11.00000 0.06203 0.04392 0.09206 =
0.02472 0.00797 -0.00380
AFIX 3
H44 2 0.08577 0.72755 0.14674 11.00000 -1.20000
AFIX 0
C45 1 0.09312 0.69028 0.25845 11.00000 0.04884 0.02608 0.08932 =
0.01314 0.00857 -0.00301
AFIX 3
H45 2 0.11313 0.71185 0.30700 11.00000 -1.20000
AFIX 0
C46 1 0.08738 0.64707 0.28558 11.00000 0.02537 0.02751 0.07126 =
0.00271 0.01309 -0.00461
C47 1 0.12057 0.63457 0.38435 11.00000 0.03050 0.01819 0.06524 =
-0.00825 0.00563 -0.00732
AFIX 3
H47 2 0.14046 0.65486 0.43577 11.00000 -1.20000
AFIX 0
C48 1 0.12149 0.59328 0.40586 11.00000 0.04412 0.02205 0.04410 =
-0.00817 -0.00053 -0.00782
AFIX 3
H48 2 0.15489 0.58450 0.47212 11.00000 -1.20000
AFIX 0
C49 1 -0.07788 0.50000 0.39106 10.50000 0.05295 0.01618 0.03090 =
0.00000 0.00368 0.00000
C50 1 -0.20469 0.50000 0.32132 10.50000 0.04782 0.02266 0.03058 =
0.00000 0.00254 0.00000
AFIX 3
H50 2 -0.20724 0.50000 0.25316 10.50000 -1.20000
AFIX 0
C51 1 -0.32139 0.50000 0.34925 10.50000 0.04910 0.00716 0.04246 =
0.00000 0.00694 0.00000
AFIX 3
H51 2 -0.40196 0.50000 0.30051 10.50000 -1.20000
AFIX 0
C52 1 -0.32054 0.50000 0.44487 10.50000 0.04604 0.01802 0.04305 =
0.00000 0.00854 0.00000
AFIX 3
H52 2 -0.39868 0.50000 0.46670 10.50000 -1.20000
AFIX 0
C53 1 -0.20098 0.50000 0.51610 10.50000 0.04317 0.02921 0.03910 =
0.00000 0.00755 0.00000
AFIX 3
H53 2 -0.19495 0.50000 0.58480 10.50000 -1.20000
AFIX 0
C54 1 -0.08250 0.50000 0.48795 10.50000 0.03814 0.00459 0.03123 =
0.00000 0.00072 0.00000
C55 1 0.04153 0.50000 0.56000 10.50000 0.03814 0.00579 0.02741 =
0.00000 0.00227 -0.00000
C56 1 0.05849 0.50000 0.65907 10.50000 0.04126 0.04093 0.02394 =
0.00000 -0.00075 0.00000
AFIX 3
H56 2 -0.01506 0.50000 0.68654 10.50000 -1.20000
AFIX 0
C57 1 0.18019 0.50000 0.71866 10.50000 0.04720 0.04682 0.02972 =
0.00000 -0.00171 0.00000
AFIX 3
H57 2 0.19266 0.50000 0.78813 10.50000 -1.20000
AFIX 0
C58 1 0.28558 0.50000 0.67646 10.50000 0.04292 0.05728 0.02337 =
0.00000 -0.00714 0.00000
AFIX 3
H58 2 0.37236 0.50000 0.71676 10.50000 -1.20000
AFIX 0
C59 1 0.26262 0.50000 0.57598 10.50000 0.03254 0.03596 0.02459 =
0.00000 -0.00489 0.00000
AFIX 3
H59 2 0.33667 0.50000 0.54917 10.50000 -1.20000
AFIX 0
O1 4 0.13372 0.95866 0.22920 11.00000 0.15447 0.08435 0.11747 =
-0.04413 0.00122 0.02606
C60 1 0.08454 0.93306 0.14383 11.00000 0.13327 0.06001 0.07382 =
0.02405 0.04801 0.02825
AFIX 3
H60a 2 0.05357 0.95096 0.08668 11.00000 -1.50000
H60b 2 0.01305 0.91589 0.15385 11.00000 -1.50000
H60c 2 0.15367 0.91491 0.13340 11.00000 -1.50000
AFIX 0
O2 4 0.12253 0.83930 0.34122 11.00000 0.09185 0.11599 0.13796 =
-0.03086 0.03808 -0.01344
AFIX 3
H2 2 0.11411 0.83318 0.28235 11.00000 -1.50000
AFIX 0
C61 1 0.20496 0.80665 0.40430 11.00000 0.24835 0.15159 0.05736 =
0.03189 0.05063 -0.01898
AFIX 3
H61a 2 0.27865 0.79967 0.37773 11.00000 -1.50000
H61b 2 0.15334 0.78149 0.40601 11.00000 -1.50000
H61c 2 0.23652 0.81765 0.47053 11.00000 -1.50000
AFIX 0
O3 4 -0.09203 0.95712 0.45553 10.50000 0.15384 0.04543 0.09008 =
-0.02018 0.01874 -0.03570
C62 1 -0.12403 0.94967 0.54285 10.50000 0.09812
AFIX 3
H62a 2 -0.19223 0.96962 0.54651 10.50000 -1.50000
H62b 2 -0.04915 0.95408 0.59808 10.50000 -1.50000
H62c 2 -0.15634 0.92114 0.54502 10.50000 -1.50000
AFIX 0
O4 4 0.10780 0.92251 0.39227 11.00000 0.41038 0.09340 0.09562 =
0.00644 -0.00263 -0.02785
HKLF 4
END
;
#===END
_database_code_depnum_ccdc_archive 'CCDC 937443'