data_mht-iii-53
# start Validation Reply Form
_vrf_PLAT975_mht-iii-53
;
PROBLEM: Check Calcd Resid. Dens. 0.55A From N2_2 2.10 eA-3
RESPONSE: There is underlying disorder of the organic molecules.
This disorder is indicated by the large and very
anisotropic thermal ellispoids. The complexity and the degree of this
disorder
prohibited building a model that could reproduce these effects
This residual is probably unresolved disorder.
;
_vrf_PLAT241_mht-iii-53
;
PROBLEM: High MainMol Ueq as Compared to Neighbors of C8_3 Check
RESPONSE: A qualitative examination of the thermal ellipsoids
of this sample suggests underlying disorder associated with packing
defects in the crystal. The complexity and the degree of this disorder
prohibited building a model that could reproduce these effects.
;
_vrf_PLAT430_mht-iii-53
;
PROBLEM: Short Inter D...A Contact O2_2 ..O1_4 . 2.78 Ang.
RESPONSE: This is a real contact in the crystal.
The nitro groups interact with each other in many modes;
described in the paper.
;
# end Validation Reply Form
_audit_creation_date 2018-10-20
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number '2018/3'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Bruker (2013). SAINT-Plus V8.34A Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2016). APEX2 Version 2016.5-1. Bruker AXS Inc., Madison, Wisconsin, USA. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Krause, L., Herbst-Irmer, R., Sheldrick, G. M., and Stalke, D., J. Appl. Cryst. (2015). 48, 1907-1913. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790; Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984; Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580 Petricek,V., Dusek,M. & Palatinus,L.(2006). Jana2006. The crystallographic computing system. Institute of Physics, Praha, Czech Republic. Rigaku Oxford Diffraction, (2015), CrysAlisPro Software system, version 1.171.39.20a, Rigaku Corporation, Oxford, UK. Sheldrick, G.M. (2015). Acta Cryst. (2015). A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. (2015). C71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. Spek, A. L. (2015). Acta Cryst. C71, 9-18.
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '(I4 Pb), 2(C8 H11 N2 O2)'
_chemical_formula_sum 'C16 H22 I4 N4 O4 Pb'
_chemical_formula_weight 1049.16
_chemical_melting_point ?
_chemical_oxdiff_formula 'C180 I32 N12 O8 Pb8 '
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'
'I' 'I' -0.4742 1.8119 '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'
'Pb' 'Pb' -3.3944 10.1111
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system 'monoclinic'
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 21.0976(4)
_cell_length_b 19.8255(3)
_cell_length_c 12.6149(2)
_cell_angle_alpha 90
_cell_angle_beta 98.2252(17)
_cell_angle_gamma 90
_cell_volume 5222.17(16)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 32454
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 33.7420
_cell_measurement_theta_min 1.9140
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 11.218
_exptl_absorpt_correction_T_max 0.908
_exptl_absorpt_correction_T_min 0.408
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 2.669
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 3776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -4 -5 0.0476
-1 4 5 0.0476
0 -5 2 0.0438
0 5 -2 0.0438
1 0 0 0.0095
-1 0 0 0.0095
0 -5 -1 0.0488
0 5 1 0.0488
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max 0.099
_exptl_crystal_size_mid 0.088
_exptl_crystal_size_min 0.019
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0066 -3.9919 -4.9978 0.0079 0.0035 0.3151
-1.0066 3.9919 4.9978 -0.0079 -0.0035 -0.3151
0.0126 -5.0048 1.9973 0.1969 0.0749 -0.0252
-0.0126 5.0048 -1.9973 -0.1969 -0.0749 0.0252
1.0009 0.0013 -0.0006 0.0145 -0.0308 -0.0007
-1.0009 -0.0013 0.0006 -0.0145 0.0308 0.0007
0.0106 -5.0000 -1.0004 0.1223 0.0632 0.1275
-0.0106 5.0000 1.0004 -0.1223 -0.0632 -0.1275
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0476
_diffrn_reflns_av_unetI/netI 0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 90640
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 29.575
_diffrn_reflns_theta_min 1.928
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 100(2)
_diffrn_detector HyPix
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w -2.00 80.00 0.50 25.00 -- 15.69 38.00 -60.00 164
2 \w 57.00 85.00 0.50 25.00 -- 15.69 0.00 -30.00 56
3 \w 4.00 34.00 0.50 25.00 -- 15.69 57.00-150.00 60
4 \w -34.00 -1.00 0.50 25.00 -- 15.69 0.00 -30.00 66
5 \w -24.00 5.00 0.50 25.00 -- 15.69 -57.00-120.00 58
6 \w -56.00 34.00 0.50 25.00 -- 15.69 -57.00-150.00 180
7 \w -24.00 59.00 0.50 25.00 -- -15.84 38.00-180.00 166
8 \w -59.00 34.00 0.50 25.00 -- 15.69 -38.00 -60.00 186
9 \w -86.00 -32.00 0.50 25.00 -- -15.84 -57.00 60.00 108
10 \w -89.00 -21.00 0.50 25.00 -- -15.84 -57.00-180.00 136
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0144901000
_diffrn_orient_matrix_UB_12 -0.0293935000
_diffrn_orient_matrix_UB_13 0.0248131000
_diffrn_orient_matrix_UB_21 -0.0307133000
_diffrn_orient_matrix_UB_22 -0.0134875000
_diffrn_orient_matrix_UB_23 0.0038903000
_diffrn_orient_matrix_UB_31 -0.0007337000
_diffrn_orient_matrix_UB_32 -0.0153028000
_diffrn_orient_matrix_UB_33 -0.0509651000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_current 1.0
_diffrn_source_type 'PhotonJet (Mo) X-ray Source'
_diffrn_source_voltage 50
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 11561
_reflns_number_total 14658
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 30.44
_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 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 3.260
_refine_diff_density_min -2.533
_refine_diff_density_rms 0.238
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 555
_refine_ls_number_reflns 14658
_refine_ls_number_restraints 603
_refine_ls_R_factor_all 0.0704
_refine_ls_R_factor_gt 0.0521
_refine_ls_restrained_S_all 1.032
_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^)+(0.0421P)^2^+85.4699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1129
_refine_ls_wR_factor_ref 0.1208
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
N2_4-C8_4
1.48 with sigma of 0.005
C8_1-C7_1
1.52 with sigma of 0.005
N1_3-C1_3
1.47 with sigma of 0.005
Pb1-I2B \\sim Pb1-I2A
with sigma of 0.005
Pb2-I4A \\sim Pb2-I4B
with sigma of 0.002
O2_4-N1_4 \\sim O1_4-N1_4
with sigma of 0.002
C6_2-C1_2 \\sim C2_2-C1_2
with sigma of 0.002
C3_2-C2_2 \\sim C6_2-C5_2
with sigma of 0.002
C5_2-C4_2 \\sim C4_2-C3_2
with sigma of 0.002
3. Restrained planarity
C2_3, C1_3, C6_3, C5_3, C4_3, C3_3, N1_3
with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
I4A \\sim I4B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
I7B \\sim I7A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(I7B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C6_4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1_2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1_1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1_3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(I8A) = Uanis(I8B)
Uanis(I2A) = Uanis(I2B)
5. Rigid body (RIGU) restrains
Pb2, I4A
with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
O1_4, N1_4, O2_4, C1_4, C2_4, C6_4, C3_4, C5_4, C4_4, C7_4, C8_4, N2_4
with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
C7_2, O1_2, N1_2, O2_2, C1_2, C2_2, C6_2, C3_2, C5_2, C4_2, C8_2, N2_2
with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
C7_1, O1_1, N1_1, O2_1, C1_1, C2_1, C6_1, C3_1, C5_1, C4_1, C8_1, N2_1
with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
C1_3, O1_3, N1_3, O2_3, C2_3, C6_3, C3_3, C5_3, C4_3, C7_3, C8_3, N2_3
with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
6. Same fragment restrains
{O1_2, O2_2, N1_2, N2_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2}
{O1_3, O2_3, N1_3, N2_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3}
{O1_4, O2_4, N1_4, N2_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4, C8_4}
as
{O1_1, O2_1, N1_1, N2_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1} sigma
for 1-2: 0.002 1-3: 0.004
7. Others
Sof(I8B)=Sof(I4A)=Sof(I7B)=Sof(I2B)=1-FVAR(1)
Sof(I2A)=Sof(I8A)=Sof(I7A)=Sof(I4B)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B),
C7(H7A,H7B), C8(H8A,H8B)
8.b Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2),
C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6)
8.c Idealised Me refined as rotating group:
N2(H2A,H2B,H2C), N2(H2A,H2B,H2C), N2(H2A,H2B,H2C), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
I1 I 0.62079(3) 0.59502(3) 0.99335(5) 0.04032(15) Uani 1 1 d . . . . .
I8B I 0.81514(8) 0.16864(8) 0.53886(15) 0.0389(2) Uani 0.4076(13) 1 d . . . A 2
I3 I 0.47827(3) 0.47757(4) 0.74536(4) 0.04070(15) Uani 1 1 d . . . . .
I5 I 0.56080(3) 0.35279(3) 0.49787(6) 0.04766(17) Uani 1 1 d . . . . .
I6 I 0.78379(4) 0.37647(3) 0.50661(6) 0.0540(2) Uani 1 1 d . . . . .
Pb1 Pb 0.500000 0.500000 1.000000 0.02431(9) Uani 1 2 d DS T P . .
Pb2 Pb 0.500000 0.500000 0.500000 0.02238(9) Uani 1 2 d DS TU P . .
Pb3 Pb 0.69303(2) 0.25864(2) 0.52252(2) 0.02703(7) Uani 1 1 d . . . . .
I2A I 0.41670(8) 0.63569(7) 0.98525(15) 0.0348(3) Uani 0.5924(13) 1 d D . . A 1
I4A I 0.64063(9) 0.5509(2) 0.5705(3) 0.0408(8) Uani 0.4076(13) 1 d D U . A 1
I7B I 0.67603(14) 0.27640(13) 0.7732(2) 0.0445(5) Uani 0.4076(13) 1 d . U . A 2
I8A I 0.79559(5) 0.15395(6) 0.58059(10) 0.0389(2) Uani 0.5924(13) 1 d . . . A 1
I7A I 0.69130(11) 0.25220(8) 0.77454(13) 0.0487(4) Uani 0.5924(13) 1 d . U . A 1
I2B I 0.40070(12) 0.62166(11) 0.9621(2) 0.0348(3) Uani 0.4076(13) 1 d D . . A 2
I4B I 0.63170(7) 0.56370(14) 0.59626(18) 0.0343(4) Uani 0.5924(13) 1 d D U . A 2
O1_1 O 0.8387(5) 0.6923(6) 0.9924(8) 0.099(3) Uani 1 1 d D U . . .
O2_1 O 0.8057(4) 0.7692(5) 1.0914(6) 0.077(2) Uani 1 1 d D U . . .
N1_1 N 0.8008(4) 0.7333(4) 1.0142(6) 0.0623(16) Uani 1 1 d D U . . .
N2_1 N 0.5175(5) 0.6721(4) 0.7741(8) 0.0580(19) Uani 1 1 d D U . . .
H2A_1 H 0.514621 0.650985 0.711296 0.070 Uiso 1 1 calc GR . . . .
H2B_1 H 0.484995 0.659595 0.807578 0.070 Uiso 1 1 calc GR . . . .
H2C_1 H 0.554312 0.661252 0.814050 0.070 Uiso 1 1 calc GR . . . .
C1_1 C 0.7421(4) 0.7420(5) 0.9355(7) 0.0642(14) Uani 1 1 d D U . . .
C2_1 C 0.6974(4) 0.7874(5) 0.9555(7) 0.0545(15) Uani 1 1 d D U . . .
H2_1 H 0.703976 0.812441 1.018399 0.065 Uiso 1 1 calc R . . . .
C3_1 C 0.6435(4) 0.7967(5) 0.8857(6) 0.0537(15) Uani 1 1 d D U . . .
H3_1 H 0.612907 0.827502 0.901360 0.064 Uiso 1 1 calc R . . . .
C4_1 C 0.6334(4) 0.7600(4) 0.7889(6) 0.0547(11) Uani 1 1 d D U . . .
C5_1 C 0.6815(4) 0.7136(5) 0.7710(7) 0.0557(16) Uani 1 1 d D U . . .
H5_1 H 0.676601 0.688127 0.708395 0.067 Uiso 1 1 calc R . . . .
C6_1 C 0.7343(4) 0.7058(5) 0.8436(7) 0.0604(18) Uani 1 1 d D U . . .
H6_1 H 0.765770 0.675295 0.830528 0.072 Uiso 1 1 calc R . . . .
C7_1 C 0.5747(4) 0.7692(5) 0.7139(6) 0.0581(11) Uani 1 1 d D U . . .
H7A_1 H 0.578504 0.744441 0.648781 0.070 Uiso 1 1 calc R . . . .
H7B_1 H 0.570336 0.816643 0.695310 0.070 Uiso 1 1 calc R . . . .
C8_1 C 0.5150(4) 0.7463(4) 0.7562(9) 0.0571(15) Uani 1 1 d D U . . .
H8A_1 H 0.511501 0.769262 0.823080 0.069 Uiso 1 1 calc R . . . .
H8B_1 H 0.477566 0.757665 0.705273 0.069 Uiso 1 1 calc R . . . .
O1_2 O 1.0292(5) 0.6067(9) 0.9098(10) 0.155(5) Uani 1 1 d D U . . .
O2_2 O 0.9991(6) 0.6464(9) 0.7520(10) 0.153(4) Uani 1 1 d D U . . .
N1_2 N 0.9908(5) 0.6166(7) 0.8316(8) 0.120(3) Uani 1 1 d D U . . .
N2_2 N 0.6514(4) 0.4414(7) 0.7926(10) 0.102(3) Uani 1 1 d D U . . .
H2A_2 H 0.635159 0.462480 0.732576 0.123 Uiso 1 1 calc GR . . . .
H2B_2 H 0.623052 0.442231 0.838579 0.123 Uiso 1 1 calc GR . . . .
H2C_2 H 0.660086 0.398759 0.777812 0.123 Uiso 1 1 calc GR . . . .
C1_2 C 0.9293(4) 0.5797(6) 0.8257(10) 0.0980(18) Uani 1 1 d D U . . .
C2_2 C 0.8805(4) 0.5958(6) 0.7481(9) 0.084(2) Uani 1 1 d D U . . .
H2_2 H 0.885234 0.631388 0.701886 0.101 Uiso 1 1 calc R . . . .
C3_2 C 0.8252(5) 0.5607(7) 0.7370(12) 0.117(3) Uani 1 1 d D U . . .
H3_2 H 0.790521 0.574637 0.687917 0.141 Uiso 1 1 calc R . . . .
C4_2 C 0.8202(5) 0.5028(6) 0.8004(10) 0.117(2) Uani 1 1 d D U . . .
C5_2 C 0.8683(6) 0.4938(7) 0.8893(11) 0.114(3) Uani 1 1 d D U . . .
H5_2 H 0.862509 0.462620 0.942143 0.136 Uiso 1 1 calc R . . . .
C6_2 C 0.9226(5) 0.5304(6) 0.8974(9) 0.092(2) Uani 1 1 d D U . . .
H6_2 H 0.955761 0.521700 0.952706 0.110 Uiso 1 1 calc R . . . .
C7_2 C 0.7648(4) 0.4584(6) 0.7784(11) 0.113(2) Uani 1 1 d D U . . .
H7A_2 H 0.778352 0.412379 0.795053 0.136 Uiso 1 1 calc R . . . .
H7B_2 H 0.748550 0.460409 0.702557 0.136 Uiso 1 1 calc R . . . .
C8_2 C 0.7113(5) 0.4759(7) 0.8411(10) 0.108(3) Uani 1 1 d D U . . .
H8A_2 H 0.722575 0.461715 0.914976 0.130 Uiso 1 1 calc R . . . .
H8B_2 H 0.704719 0.524315 0.840192 0.130 Uiso 1 1 calc R . . . .
O1_3 O 1.0357(8) 0.5588(10) 0.5821(13) 0.242(6) Uani 1 1 d D U . . .
O2_3 O 1.1138(5) 0.5554(5) 0.7118(8) 0.103(3) Uani 1 1 d D U . . .
N1_3 N 1.0627(4) 0.5379(5) 0.6657(8) 0.147(3) Uani 1 1 d D U . . .
N2_3 N 0.8838(6) 0.2119(6) 0.8317(11) 0.102(3) Uani 1 1 d D U . . .
H2A_3 H 0.856685 0.188040 0.785871 0.122 Uiso 1 1 calc GR . . . .
H2B_3 H 0.865552 0.221855 0.889154 0.122 Uiso 1 1 calc GR . . . .
H2C_3 H 0.919192 0.187933 0.851508 0.122 Uiso 1 1 calc GR . . . .
C1_3 C 1.0343(3) 0.4778(4) 0.7108(5) 0.0919(18) Uani 1 1 d D U . . .
C2_3 C 1.0654(4) 0.4494(4) 0.8011(6) 0.0742(18) Uani 1 1 d D U . . .
H2_3 H 1.103887 0.467899 0.833356 0.089 Uiso 1 1 calc R . . . .
C3_3 C 1.0414(4) 0.3948(4) 0.8449(7) 0.082(2) Uani 1 1 d D U . . .
H3_3 H 1.063362 0.375910 0.907019 0.098 Uiso 1 1 calc R . . . .
C4_3 C 0.9830(4) 0.3662(5) 0.7968(7) 0.102(3) Uani 1 1 d D U . . .
C5_3 C 0.9523(5) 0.3975(5) 0.7028(8) 0.086(2) Uani 1 1 d D U . . .
H5_3 H 0.913678 0.380242 0.668518 0.103 Uiso 1 1 calc R . . . .
C6_3 C 0.9783(4) 0.4521(4) 0.6622(7) 0.087(3) Uani 1 1 d D U . . .
H6_3 H 0.957553 0.472183 0.600161 0.105 Uiso 1 1 calc R . . . .
C7_3 C 0.9545(8) 0.3106(8) 0.8492(11) 0.144(3) Uani 1 1 d D U . . .
H7A_3 H 0.938531 0.327824 0.912287 0.173 Uiso 1 1 calc R . . . .
H7B_3 H 0.987677 0.277832 0.872902 0.173 Uiso 1 1 calc R . . . .
C8_3 C 0.9006(11) 0.2755(10) 0.7793(15) 0.196(5) Uani 1 1 d D U . . .
H8A_3 H 0.863526 0.304836 0.767484 0.235 Uiso 1 1 calc R . . . .
H8B_3 H 0.913541 0.265236 0.710241 0.235 Uiso 1 1 calc R . . . .
O1_4 O 0.9546(7) 0.7532(7) 0.3758(13) 0.176(5) Uani 1 1 d D U . . .
O2_4 O 0.9839(6) 0.6840(7) 0.5051(11) 0.148(4) Uani 1 1 d D U . . .
N1_4 N 0.9484(5) 0.7040(6) 0.4289(10) 0.109(3) Uani 1 1 d D U . . .
N2_4 N 0.6805(8) 0.4368(6) 0.2630(16) 0.147(6) Uani 1 1 d D U . . .
H2A_4 H 0.649630 0.437195 0.206982 0.177 Uiso 1 1 calc GR . . . .
H2B_4 H 0.663940 0.446771 0.322145 0.177 Uiso 1 1 calc GR . . . .
H2C_4 H 0.698232 0.395988 0.269674 0.177 Uiso 1 1 calc GR . . . .
C1_4 C 0.8911(5) 0.6619(5) 0.3948(8) 0.085(2) Uani 1 1 d D U . . .
C2_4 C 0.8788(5) 0.6086(6) 0.4558(9) 0.093(3) Uani 1 1 d D U . . .
H2_4 H 0.908171 0.596913 0.515156 0.112 Uiso 1 1 calc R . . . .
C3_4 C 0.8247(5) 0.5723(6) 0.4317(9) 0.088(2) Uani 1 1 d D U . . .
H3_4 H 0.816321 0.536532 0.475339 0.106 Uiso 1 1 calc R . . . .
C4_4 C 0.7807(5) 0.5885(5) 0.3402(8) 0.0901(17) Uani 1 1 d D U . . .
C5_4 C 0.7979(5) 0.6410(5) 0.2743(8) 0.082(2) Uani 1 1 d D U . . .
H5_4 H 0.772289 0.650352 0.209643 0.099 Uiso 1 1 calc R . . . .
C6_4 C 0.8511(6) 0.6777(7) 0.3046(10) 0.1026(19) Uani 1 1 d D U . . .
H6_4 H 0.860513 0.714169 0.263207 0.123 Uiso 1 1 calc R . . . .
C7_4 C 0.7221(5) 0.5493(5) 0.3134(10) 0.0926(17) Uani 1 1 d D U . . .
H7A_4 H 0.689392 0.577969 0.274532 0.111 Uiso 1 1 calc R . . . .
H7B_4 H 0.707066 0.535380 0.379166 0.111 Uiso 1 1 calc R . . . .
C8_4 C 0.7301(6) 0.4876(6) 0.2467(12) 0.097(3) Uani 1 1 d D U . . .
H8A_4 H 0.725973 0.499920 0.171634 0.116 Uiso 1 1 calc R . . . .
H8B_4 H 0.772452 0.468568 0.267472 0.116 Uiso 1 1 calc 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
I1 0.0499(4) 0.0349(3) 0.0403(3) -0.0060(2) 0.0203(3) -0.0107(3)
I8B 0.0360(5) 0.0337(5) 0.0466(6) 0.0041(4) 0.0046(4) 0.0078(4)
I3 0.0466(3) 0.0620(4) 0.0140(2) -0.0038(2) 0.0061(2) -0.0152(3)
I5 0.0482(4) 0.0300(3) 0.0616(4) -0.0037(3) -0.0031(3) 0.0130(3)
I6 0.0741(5) 0.0312(3) 0.0639(4) -0.0100(3) 0.0346(4) -0.0206(3)
Pb1 0.0386(2) 0.01832(17) 0.01633(17) 0.00090(14) 0.00493(15) 0.00483(16)
Pb2 0.0272(2) 0.02420(18) 0.01482(16) -0.00292(14) -0.00021(14) 0.00317(15)
Pb3 0.03655(17) 0.02407(14) 0.01912(13) 0.00255(10) -0.00066(11) -0.00272(12)
I2A 0.0407(9) 0.0195(6) 0.0428(9) 0.0051(5) 0.0008(6) 0.0063(5)
I4A 0.0562(14) 0.0351(14) 0.0260(15) 0.0023(9) -0.0115(9) -0.0150(11)
I7B 0.0698(12) 0.0484(12) 0.0150(7) 0.0015(9) 0.0056(7) 0.0064(10)
I8A 0.0360(5) 0.0337(5) 0.0466(6) 0.0041(4) 0.0046(4) 0.0078(4)
I7A 0.0946(13) 0.0381(8) 0.0136(5) 0.0009(6) 0.0082(6) 0.0008(7)
I2B 0.0407(9) 0.0195(6) 0.0428(9) 0.0051(5) 0.0008(6) 0.0063(5)
I4B 0.0337(6) 0.0394(11) 0.0259(10) 0.0039(6) -0.0085(5) -0.0123(6)
O1_1 0.090(2) 0.112(4) 0.088(3) -0.025(3) -0.011(2) 0.031(3)
O2_1 0.077(3) 0.079(4) 0.071(2) -0.004(2) 0.001(2) 0.009(3)
N1_1 0.0673(17) 0.059(3) 0.0612(18) 0.0104(19) 0.0109(16) -0.0039(18)
N2_1 0.065(4) 0.063(3) 0.048(5) 0.009(3) 0.012(4) -0.0119(18)
C1_1 0.0688(16) 0.062(2) 0.0621(16) 0.0061(14) 0.0097(12) -0.0013(14)
C2_1 0.0637(17) 0.048(3) 0.0533(17) 0.0149(19) 0.0145(15) -0.0096(18)
C3_1 0.0631(17) 0.048(3) 0.0521(18) 0.0152(18) 0.0154(15) -0.0102(19)
C4_1 0.0623(16) 0.051(2) 0.0530(17) 0.0135(15) 0.0154(14) -0.0096(14)
C5_1 0.0623(18) 0.050(3) 0.0567(17) 0.0127(19) 0.0163(15) -0.0101(19)
C6_1 0.0652(19) 0.057(3) 0.0603(17) 0.009(2) 0.0132(16) -0.005(2)
C7_1 0.0628(16) 0.061(3) 0.0526(18) 0.0120(16) 0.0152(14) -0.0076(15)
C8_1 0.0628(16) 0.063(3) 0.047(3) 0.008(3) 0.0129(18) -0.0114(18)
O1_2 0.108(3) 0.216(12) 0.136(4) 0.057(6) -0.005(3) -0.034(5)
O2_2 0.113(4) 0.205(9) 0.134(4) 0.053(4) -0.008(3) -0.039(5)
N1_2 0.102(2) 0.134(5) 0.120(3) 0.021(3) 0.006(2) -0.008(3)
N2_2 0.095(2) 0.117(7) 0.092(6) 0.065(4) 0.005(3) 0.021(3)
C1_2 0.0943(19) 0.101(2) 0.100(2) -0.0015(17) 0.0164(15) 0.0083(15)
C2_2 0.090(2) 0.081(4) 0.084(3) -0.019(3) 0.025(2) 0.019(2)
C3_2 0.101(2) 0.117(4) 0.129(5) 0.026(4) 0.000(3) -0.001(2)
C4_2 0.099(2) 0.118(3) 0.131(4) 0.028(3) 0.003(2) 0.002(2)
C5_2 0.094(3) 0.118(5) 0.126(4) 0.025(4) 0.008(3) 0.006(3)
C6_2 0.087(2) 0.095(4) 0.097(3) -0.006(3) 0.025(2) 0.019(2)
C7_2 0.096(2) 0.116(3) 0.124(4) 0.028(3) 0.006(2) 0.005(2)
C8_2 0.095(3) 0.115(6) 0.110(5) 0.057(5) 0.001(3) 0.024(3)
O1_3 0.209(6) 0.262(7) 0.214(5) 0.139(6) -0.107(5) -0.143(6)
O2_3 0.101(3) 0.112(4) 0.095(5) 0.002(4) 0.006(3) -0.012(3)
N1_3 0.129(3) 0.151(4) 0.145(4) 0.050(3) -0.032(3) -0.046(3)
N2_3 0.083(6) 0.138(4) 0.087(7) 0.024(5) 0.019(5) -0.013(4)
C1_3 0.089(2) 0.094(2) 0.092(2) -0.0034(16) 0.0121(15) 0.0026(15)
C2_3 0.075(2) 0.077(3) 0.075(2) -0.021(2) 0.027(2) 0.020(2)
C3_3 0.081(3) 0.086(3) 0.082(3) -0.013(3) 0.020(2) 0.013(2)
C4_3 0.096(3) 0.107(4) 0.099(4) 0.007(3) 0.004(3) -0.005(3)
C5_3 0.085(3) 0.089(3) 0.085(3) -0.008(3) 0.016(3) 0.007(3)
C6_3 0.086(2) 0.089(3) 0.087(3) -0.008(3) 0.016(3) 0.006(3)
C7_3 0.125(5) 0.162(4) 0.131(4) 0.050(3) -0.028(3) -0.045(4)
C8_3 0.199(6) 0.209(5) 0.151(6) 0.091(5) -0.071(5) -0.108(5)
O1_4 0.173(5) 0.153(5) 0.179(6) 0.059(5) -0.050(5) -0.063(5)
O2_4 0.147(4) 0.133(6) 0.152(5) 0.034(5) -0.026(4) -0.039(4)
N1_4 0.119(3) 0.097(4) 0.111(4) -0.003(3) 0.009(3) -0.008(3)
N2_4 0.149(7) 0.101(4) 0.205(14) -0.060(6) 0.073(9) -0.018(4)
C1_4 0.098(2) 0.072(3) 0.089(2) -0.024(2) 0.028(2) 0.015(2)
C2_4 0.105(3) 0.082(3) 0.094(3) -0.016(3) 0.020(3) 0.007(2)
C3_4 0.101(3) 0.075(3) 0.090(3) -0.020(3) 0.023(2) 0.011(2)
C4_4 0.101(2) 0.081(3) 0.091(3) -0.017(2) 0.023(2) 0.010(2)
C5_4 0.093(2) 0.072(3) 0.088(3) -0.023(2) 0.031(2) 0.020(2)
C6_4 0.109(2) 0.097(2) 0.103(2) -0.0043(16) 0.0163(15) -0.0006(16)
C7_4 0.101(2) 0.079(3) 0.099(4) -0.013(2) 0.020(2) 0.011(2)
C8_4 0.100(4) 0.084(3) 0.105(7) -0.020(4) 0.010(4) 0.014(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
I1 Pb1 3.1797(6) . ?
I8B Pb3 3.1162(16) . ?
I3 Pb1 3.2102(5) . ?
I3 Pb2 3.2240(5) . ?
I5 Pb2 3.1896(6) . ?
I5 Pb3 3.3340(7) . ?
I6 Pb3 3.0453(7) . ?
Pb1 I2A 3.2041(14) . ?
Pb1 I2A 3.2040(14) 3_667 ?
Pb1 I2B 3.186(2) 3_667 ?
Pb1 I2B 3.186(2) . ?
Pb2 I4A 3.1398(15) . ?
Pb2 I4A 3.1399(15) 3_666 ?
Pb2 I4B 3.1343(10) 3_666 ?
Pb2 I4B 3.1343(10) . ?
Pb3 I2A 3.3535(15) 2_646 ?
Pb3 I7B 3.253(3) . ?
Pb3 I7B 3.190(2) 4_565 ?
Pb3 I8A 3.0122(11) . ?
Pb3 I7A 3.1306(17) 4_565 ?
Pb3 I7A 3.1872(17) . ?
Pb3 I2B 3.381(2) 2_646 ?
O1_1 N1_1 1.200(5) . ?
O2_1 N1_1 1.199(5) . ?
N1_1 C1_1 1.482(5) . ?
N2_1 C8_1 1.489(5) . ?
C1_1 C2_1 1.352(6) . ?
C1_1 C6_1 1.353(6) . ?
C2_1 C3_1 1.348(7) . ?
C3_1 C4_1 1.411(7) . ?
C4_1 C5_1 1.411(7) . ?
C4_1 C7_1 1.458(10) . ?
C5_1 C6_1 1.348(7) . ?
C7_1 C8_1 1.508(5) . ?
O1_2 N1_2 1.200(5) . ?
O2_2 N1_2 1.200(5) . ?
N1_2 C1_2 1.482(5) . ?
N2_2 C8_2 1.490(5) . ?
C1_2 C2_2 1.353(6) . ?
C1_2 C6_2 1.352(6) . ?
C2_2 C3_2 1.349(7) . ?
C3_2 C4_2 1.412(7) . ?
C4_2 C5_2 1.412(7) . ?
C4_2 C7_2 1.458(10) . ?
C5_2 C6_2 1.348(7) . ?
C7_2 C8_2 1.508(5) . ?
O1_3 N1_3 1.200(5) . ?
O2_3 N1_3 1.201(5) . ?
N1_3 C1_3 1.482(5) . ?
N2_3 C8_3 1.489(5) . ?
C1_3 C2_3 1.353(6) . ?
C1_3 C6_3 1.352(6) . ?
C2_3 C3_3 1.347(7) . ?
C3_3 C4_3 1.412(7) . ?
C4_3 C5_3 1.411(7) . ?
C4_3 C7_3 1.458(10) . ?
C5_3 C6_3 1.348(7) . ?
C7_3 C8_3 1.507(5) . ?
O1_4 N1_4 1.200(5) . ?
O2_4 N1_4 1.199(5) . ?
N1_4 C1_4 1.482(5) . ?
N2_4 C8_4 1.489(5) . ?
C1_4 C2_4 1.353(6) . ?
C1_4 C6_4 1.352(6) . ?
C2_4 C3_4 1.348(7) . ?
C3_4 C4_4 1.411(7) . ?
C4_4 C5_4 1.411(7) . ?
C4_4 C7_4 1.459(10) . ?
C5_4 C6_4 1.347(7) . ?
C7_4 C8_4 1.508(5) . ?
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
Pb1 I3 Pb2 157.22(2) . . ?
Pb2 I5 Pb3 147.53(3) . . ?
I1 Pb1 I1 180.0 3_667 . ?
I1 Pb1 I3 86.794(16) 3_667 . ?
I1 Pb1 I3 93.206(16) . . ?
I1 Pb1 I3 93.205(16) 3_667 3_667 ?
I1 Pb1 I3 86.794(16) . 3_667 ?
I1 Pb1 I2A 86.33(3) . . ?
I1 Pb1 I2A 93.67(3) 3_667 . ?
I1 Pb1 I2A 86.33(3) 3_667 3_667 ?
I1 Pb1 I2A 93.67(3) . 3_667 ?
I1 Pb1 I2B 93.43(5) . . ?
I1 Pb1 I2B 93.43(5) 3_667 3_667 ?
I1 Pb1 I2B 86.57(5) . 3_667 ?
I1 Pb1 I2B 86.57(5) 3_667 . ?
I3 Pb1 I3 180.00(2) 3_667 . ?
I2A Pb1 I3 93.42(4) 3_667 3_667 ?
I2A Pb1 I3 93.42(4) . . ?
I2A Pb1 I3 86.58(4) 3_667 . ?
I2A Pb1 I3 86.58(4) . 3_667 ?
I2A Pb1 I2A 180.00(6) 3_667 . ?
I2B Pb1 I3 92.40(6) 3_667 . ?
I2B Pb1 I3 87.60(6) . . ?
I2B Pb1 I2B 180.00(9) 3_667 . ?
I3 Pb2 I3 180.0 . 3_666 ?
I5 Pb2 I3 89.681(19) 3_666 3_666 ?
I5 Pb2 I3 89.682(19) . . ?
I5 Pb2 I3 90.318(19) . 3_666 ?
I5 Pb2 I3 90.318(19) 3_666 . ?
I5 Pb2 I5 180.0 3_666 . ?
I4A Pb2 I3 91.76(7) 3_666 3_666 ?
I4A Pb2 I3 91.77(7) . . ?
I4A Pb2 I3 88.23(7) 3_666 . ?
I4A Pb2 I3 88.24(7) . 3_666 ?
I4A Pb2 I5 86.09(8) 3_666 3_666 ?
I4A Pb2 I5 86.09(8) . . ?
I4A Pb2 I5 93.91(8) 3_666 . ?
I4A Pb2 I5 93.91(8) . 3_666 ?
I4A Pb2 I4A 180.00(12) . 3_666 ?
I4B Pb2 I3 85.62(5) . . ?
I4B Pb2 I3 94.38(5) 3_666 . ?
I4B Pb2 I5 92.10(5) . . ?
I4B Pb2 I5 87.90(5) 3_666 . ?
I4B Pb2 I4B 180.0 3_666 . ?
I8B Pb3 I5 178.26(4) . . ?
I8B Pb3 I7B 101.70(6) . . ?
I5 Pb3 I2A 80.75(3) . 2_646 ?
I5 Pb3 I2B 88.09(5) . 2_646 ?
I6 Pb3 I8B 85.52(4) . . ?
I6 Pb3 I5 95.16(2) . . ?
I6 Pb3 I2A 173.52(3) . 2_646 ?
I6 Pb3 I7B 97.98(5) . . ?
I6 Pb3 I7B 94.88(5) . 4_565 ?
I6 Pb3 I7A 84.51(4) . 4_565 ?
I6 Pb3 I7A 101.16(4) . . ?
I6 Pb3 I2B 176.65(5) . 2_646 ?
I2A Pb3 I2B 8.47(4) 2_646 2_646 ?
I7B Pb3 I5 93.18(6) 4_565 . ?
I7B Pb3 I5 79.80(5) . . ?
I7B Pb3 I7B 165.83(10) 4_565 . ?
I8A Pb3 I5 166.14(3) . . ?
I8A Pb3 I6 96.20(3) . . ?
I8A Pb3 I2A 88.58(3) . 2_646 ?
I8A Pb3 I7B 93.74(6) . 4_565 ?
I8A Pb3 I7A 80.80(4) . . ?
I8A Pb3 I7A 95.80(4) . 4_565 ?
I8A Pb3 I2B 80.70(5) . 2_646 ?
I7A Pb3 I5 93.16(4) 4_565 . ?
I7A Pb3 I5 89.23(4) . . ?
I7A Pb3 I2A 83.90(5) . 2_646 ?
I7A Pb3 I2A 90.67(5) 4_565 2_646 ?
I7A Pb3 I7B 163.50(5) . 4_565 ?
I7A Pb3 I7B 10.42(4) 4_565 4_565 ?
I7A Pb3 I7A 173.63(2) 4_565 . ?
I7A Pb3 I2B 94.52(6) 4_565 2_646 ?
I7A Pb3 I2B 79.66(6) . 2_646 ?
Pb1 I2A Pb3 169.29(6) . 2_656 ?
Pb3 I7B Pb3 157.28(9) 4_566 . ?
Pb3 I7A Pb3 177.90(7) 4_566 . ?
Pb1 I2B Pb3 167.69(9) . 2_656 ?
O1_1 N1_1 C1_1 116.5(6) . . ?
O2_1 N1_1 O1_1 127.3(7) . . ?
O2_1 N1_1 C1_1 116.2(6) . . ?
C2_1 C1_1 N1_1 119.4(5) . . ?
C2_1 C1_1 C6_1 120.7(7) . . ?
C6_1 C1_1 N1_1 120.0(5) . . ?
C3_1 C2_1 C1_1 121.0(7) . . ?
C2_1 C3_1 C4_1 120.2(7) . . ?
C3_1 C4_1 C5_1 116.9(8) . . ?
C3_1 C4_1 C7_1 120.4(6) . . ?
C5_1 C4_1 C7_1 122.7(6) . . ?
C6_1 C5_1 C4_1 120.6(7) . . ?
C5_1 C6_1 C1_1 120.6(7) . . ?
C4_1 C7_1 C8_1 114.0(5) . . ?
N2_1 C8_1 C7_1 109.7(5) . . ?
O1_2 N1_2 C1_2 116.3(6) . . ?
O2_2 N1_2 O1_2 127.3(8) . . ?
O2_2 N1_2 C1_2 115.7(6) . . ?
C2_2 C1_2 N1_2 119.3(5) . . ?
C6_2 C1_2 N1_2 119.8(5) . . ?
C6_2 C1_2 C2_2 120.9(7) . . ?
C3_2 C2_2 C1_2 120.7(7) . . ?
C2_2 C3_2 C4_2 119.6(7) . . ?
C3_2 C4_2 C5_2 116.7(8) . . ?
C3_2 C4_2 C7_2 120.4(6) . . ?
C5_2 C4_2 C7_2 122.7(6) . . ?
C6_2 C5_2 C4_2 120.0(7) . . ?
C5_2 C6_2 C1_2 120.4(7) . . ?
C4_2 C7_2 C8_2 113.7(6) . . ?
N2_2 C8_2 C7_2 109.5(6) . . ?
O1_3 N1_3 O2_3 127.3(8) . . ?
O1_3 N1_3 C1_3 116.7(6) . . ?
O2_3 N1_3 C1_3 115.5(6) . . ?
C2_3 C1_3 N1_3 118.9(5) . . ?
C6_3 C1_3 N1_3 120.3(5) . . ?
C6_3 C1_3 C2_3 120.8(7) . . ?
C3_3 C2_3 C1_3 121.0(7) . . ?
C2_3 C3_3 C4_3 120.1(7) . . ?
C3_3 C4_3 C7_3 119.9(6) . . ?
C5_3 C4_3 C3_3 117.0(8) . . ?
C5_3 C4_3 C7_3 122.9(6) . . ?
C6_3 C5_3 C4_3 120.5(7) . . ?
C5_3 C6_3 C1_3 120.6(7) . . ?
C4_3 C7_3 C8_3 114.2(5) . . ?
N2_3 C8_3 C7_3 109.8(6) . . ?
O1_4 N1_4 C1_4 116.5(6) . . ?
O2_4 N1_4 O1_4 127.6(8) . . ?
O2_4 N1_4 C1_4 115.9(6) . . ?
C2_4 C1_4 N1_4 119.3(5) . . ?
C6_4 C1_4 N1_4 119.8(5) . . ?
C6_4 C1_4 C2_4 120.9(7) . . ?
C3_4 C2_4 C1_4 120.9(7) . . ?
C2_4 C3_4 C4_4 120.0(7) . . ?
C3_4 C4_4 C5_4 117.1(8) . . ?
C3_4 C4_4 C7_4 120.3(6) . . ?
C5_4 C4_4 C7_4 122.5(6) . . ?
C6_4 C5_4 C4_4 120.3(7) . . ?
C5_4 C6_4 C1_4 120.5(7) . . ?
C4_4 C7_4 C8_4 113.7(5) . . ?
N2_4 C8_4 C7_4 109.5(6) . . ?
_shelx_res_file
;
TITL MHT-III-53 in P2(1)/c
mht-iii-53.res
created by SHELXL-2018/3 at 15:13:33 on 20-Oct-2018
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 21.097616 19.825465 12.614931 90 98.2252 90
ZERR 8 0.000427 0.000343 0.000197 0 0.0017 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H I N O Pb
UNIT 128 176 32 32 32 8
DFIX_4 1.48 0.005 N2 C8
DFIX_1 1.52 0.005 C8 C7
DFIX_3 1.47 0.005 N1 C1
SADI 0.005 Pb1 I2B Pb1 I2A
SADI 0.002 Pb2 I4A Pb2 I4B
SADI_4 0.002 O2 N1 O1 N1
SADI_2 0.002 C6 C1 C2 C1
SADI_2 0.002 C3 C2 C6 C5
SADI_2 0.002 C5 C4 C4 C3
FLAT_3 0.002 C2 C1 C6 C5 C4 C3 N1
SIMU 0.004 0.008 2 I4A I4B
SIMU 0.004 0.008 2 I7b I7a
RIGU 0.0002 0.0002 Pb2 I4A
RIGU_4 0.0001 0.0001 O1 N1 O2 C1 C2 C6 C3 C5 C4 C7 C8 N2
RIGU_2 0.0001 0.0001 C7 O1 N1 O2 C1 C2 C6 C3 C5 C4 C8 N2
RIGU_1 0.0001 0.0001 C7 O1 N1 O2 C1 C2 C6 C3 C5 C4 C8 N2
RIGU_3 0.0001 0.0001 C1 O1 N1 O2 C2 C6 C3 C5 C4 C7 C8 N2
ISOR 0.002 0.004 I7b
ISOR_4 0.002 0.004 C6
ISOR_2 0.002 0.004 C1
ISOR_1 0.002 0.004 C1
ISOR_3 0.002 0.004 C1
EADP I8a I8b
EADP I2A I2B
SAME_4NPE 0.002 0.004 O1 > C8
L.S. 9
PLAN 20
list 4
fmap 2
acta
SHEL 20 0.72
OMIT 7 0 2
OMIT 1 3 1
OMIT 8 0 2
REM
REM
REM
WGHT 0.042100 85.469902
FVAR 0.07848 0.59237
I1 3 0.620786 0.595020 0.993346 11.00000 0.04988 0.03489 =
0.04026 -0.00602 0.02033 -0.01065
PART 2
I8B 3 0.815135 0.168638 0.538855 -21.00000 0.03596 0.03370 =
0.04660 0.00412 0.00464 0.00783
PART 0
I3 3 0.478269 0.477565 0.745357 11.00000 0.04658 0.06199 =
0.01403 -0.00382 0.00607 -0.01525
I5 3 0.560801 0.352790 0.497870 11.00000 0.04818 0.03000 =
0.06158 -0.00371 -0.00314 0.01301
I6 3 0.783789 0.376466 0.506610 11.00000 0.07409 0.03120 =
0.06387 -0.00999 0.03456 -0.02057
PB1 6 0.500000 0.500000 1.000000 10.50000 0.03855 0.01832 =
0.01633 0.00090 0.00493 0.00483
PB2 6 0.500000 0.500000 0.500000 10.50000 0.02717 0.02420 =
0.01482 -0.00292 -0.00021 0.00317
PB3 6 0.693029 0.258636 0.522521 11.00000 0.03655 0.02407 =
0.01912 0.00255 -0.00066 -0.00272
PART 1
I2A 3 0.416701 0.635689 0.985249 21.00000 0.04066 0.01947 =
0.04282 0.00515 0.00081 0.00627
I4A 3 0.640626 0.550944 0.570509 -21.00000 0.05618 0.03512 =
0.02595 0.00229 -0.01147 -0.01497
PART 0
PART 2
I7B 3 0.676029 0.276404 0.773219 -21.00000 0.06985 0.04841 =
0.01497 0.00151 0.00562 0.00644
PART 0
PART 1
I8A 3 0.795594 0.153948 0.580593 21.00000 0.03596 0.03370 =
0.04660 0.00412 0.00464 0.00783
I7A 3 0.691298 0.252197 0.774544 21.00000 0.09459 0.03807 =
0.01364 0.00087 0.00821 0.00078
PART 0
PART 2
I2B 3 0.400700 0.621660 0.962142 -21.00000 0.04066 0.01947 =
0.04282 0.00515 0.00081 0.00627
I4B 3 0.631696 0.563699 0.596264 21.00000 0.03375 0.03939 =
0.02593 0.00387 -0.00854 -0.01235
RESI 4NPE 1
PART 0
O1 5 0.838695 0.692268 0.992433 11.00000 0.08990 0.11220 =
0.08762 -0.02474 -0.01116 0.03086
O2 5 0.805660 0.769221 1.091432 11.00000 0.07726 0.07935 =
0.07098 -0.00380 0.00066 0.00943
N1 4 0.800792 0.733322 1.014164 11.00000 0.06731 0.05897 =
0.06118 0.01040 0.01090 -0.00386
N2 4 0.517474 0.672071 0.774084 11.00000 0.06474 0.06275 =
0.04775 0.00870 0.01240 -0.01187
AFIX 137
H2A 2 0.514621 0.650985 0.711296 11.00000 -1.20000
H2B 2 0.484995 0.659595 0.807578 11.00000 -1.20000
H2C 2 0.554312 0.661252 0.814050 11.00000 -1.20000
AFIX 0
C1 1 0.742132 0.742032 0.935472 11.00000 0.06884 0.06161 =
0.06209 0.00614 0.00966 -0.00126
C2 1 0.697424 0.787354 0.955490 11.00000 0.06371 0.04834 =
0.05331 0.01485 0.01452 -0.00965
AFIX 43
H2 2 0.703976 0.812441 1.018399 11.00000 -1.20000
AFIX 0
C3 1 0.643524 0.796732 0.885703 11.00000 0.06307 0.04793 =
0.05207 0.01522 0.01541 -0.01017
AFIX 43
H3 2 0.612907 0.827502 0.901360 11.00000 -1.20000
AFIX 0
C4 1 0.633408 0.759999 0.788943 11.00000 0.06230 0.05079 =
0.05304 0.01348 0.01543 -0.00961
C5 1 0.681467 0.713583 0.770956 11.00000 0.06228 0.05043 =
0.05666 0.01267 0.01630 -0.01010
AFIX 43
H5 2 0.676601 0.688127 0.708395 11.00000 -1.20000
AFIX 0
C6 1 0.734338 0.705829 0.843633 11.00000 0.06515 0.05691 =
0.06031 0.00900 0.01324 -0.00530
AFIX 43
H6 2 0.765770 0.675295 0.830528 11.00000 -1.20000
AFIX 0
C7 1 0.574734 0.769228 0.713880 11.00000 0.06281 0.06108 =
0.05257 0.01202 0.01517 -0.00757
AFIX 23
H7A 2 0.578504 0.744441 0.648781 11.00000 -1.20000
H7B 2 0.570336 0.816643 0.695310 11.00000 -1.20000
AFIX 0
C8 1 0.514955 0.746325 0.756228 11.00000 0.06277 0.06272 =
0.04741 0.00824 0.01290 -0.01137
AFIX 23
H8A 2 0.511501 0.769262 0.823080 11.00000 -1.20000
H8B 2 0.477566 0.757665 0.705273 11.00000 -1.20000
AFIX 0
RESI 4NPE 2
O1 5 1.029172 0.606725 0.909842 11.00000 0.10789 0.21613 =
0.13574 0.05721 -0.00491 -0.03399
O2 5 0.999098 0.646422 0.751966 11.00000 0.11335 0.20536 =
0.13413 0.05273 -0.00784 -0.03894
N1 4 0.990781 0.616587 0.831567 11.00000 0.10227 0.13376 =
0.11973 0.02096 0.00561 -0.00802
N2 4 0.651367 0.441364 0.792636 11.00000 0.09491 0.11713 =
0.09184 0.06512 0.00519 0.02061
AFIX 137
H2A 2 0.635159 0.462480 0.732576 11.00000 -1.20000
H2B 2 0.623052 0.442231 0.838579 11.00000 -1.20000
H2C 2 0.660086 0.398759 0.777812 11.00000 -1.20000
AFIX 0
C1 1 0.929259 0.579699 0.825728 11.00000 0.09431 0.10091 =
0.09963 -0.00146 0.01640 0.00831
C2 1 0.880528 0.595775 0.748109 11.00000 0.08971 0.08115 =
0.08427 -0.01860 0.02533 0.01877
AFIX 43
H2 2 0.885234 0.631388 0.701886 11.00000 -1.20000
AFIX 0
C3 1 0.825187 0.560726 0.737009 11.00000 0.10118 0.11654 =
0.12931 0.02593 0.00021 -0.00129
AFIX 43
H3 2 0.790521 0.574637 0.687917 11.00000 -1.20000
AFIX 0
C4 1 0.820196 0.502786 0.800368 11.00000 0.09881 0.11800 =
0.13071 0.02784 0.00297 0.00235
C5 1 0.868300 0.493782 0.889265 11.00000 0.09436 0.11809 =
0.12599 0.02465 0.00752 0.00573
AFIX 43
H5 2 0.862509 0.462620 0.942143 11.00000 -1.20000
AFIX 0
C6 1 0.922635 0.530398 0.897432 11.00000 0.08708 0.09457 =
0.09664 -0.00577 0.02484 0.01885
AFIX 43
H6 2 0.955761 0.521700 0.952706 11.00000 -1.20000
AFIX 0
C7 1 0.764780 0.458389 0.778417 11.00000 0.09601 0.11583 =
0.12442 0.02792 0.00626 0.00461
AFIX 23
H7A 2 0.778352 0.412379 0.795053 11.00000 -1.20000
H7B 2 0.748550 0.460409 0.702557 11.00000 -1.20000
AFIX 0
C8 1 0.711302 0.475883 0.841086 11.00000 0.09549 0.11450 =
0.11049 0.05680 0.00150 0.02413
AFIX 23
H8A 2 0.722575 0.461715 0.914976 11.00000 -1.20000
H8B 2 0.704719 0.524315 0.840192 11.00000 -1.20000
AFIX 0
RESI 4NPE 3
O1 5 1.035687 0.558843 0.582066 11.00000 0.20897 0.26177 =
0.21433 0.13878 -0.10739 -0.14325
O2 5 1.113800 0.555406 0.711791 11.00000 0.10118 0.11197 =
0.09478 0.00234 0.00608 -0.01207
N1 4 1.062689 0.537869 0.665745 11.00000 0.12928 0.15149 =
0.14475 0.05029 -0.03220 -0.04583
N2 4 0.883826 0.211933 0.831725 11.00000 0.08308 0.13780 =
0.08737 0.02448 0.01908 -0.01332
AFIX 137
H2A 2 0.856685 0.188040 0.785871 11.00000 -1.20000
H2B 2 0.865552 0.221855 0.889154 11.00000 -1.20000
H2C 2 0.919192 0.187933 0.851508 11.00000 -1.20000
AFIX 0
C1 1 1.034330 0.477832 0.710813 11.00000 0.08914 0.09409 =
0.09215 -0.00339 0.01211 0.00258
C2 1 1.065390 0.449434 0.801073 11.00000 0.07535 0.07686 =
0.07535 -0.02116 0.02745 0.01989
AFIX 43
H2 2 1.103887 0.467899 0.833356 11.00000 -1.20000
AFIX 0
C3 1 1.041417 0.394820 0.844915 11.00000 0.08096 0.08564 =
0.08162 -0.01286 0.02034 0.01307
AFIX 43
H3 2 1.063362 0.375910 0.907019 11.00000 -1.20000
AFIX 0
C4 1 0.983025 0.366220 0.796763 11.00000 0.09621 0.10718 =
0.09944 0.00747 0.00392 -0.00528
C5 1 0.952254 0.397466 0.702754 11.00000 0.08479 0.08851 =
0.08539 -0.00823 0.01628 0.00739
AFIX 43
H5 2 0.913678 0.380242 0.668518 11.00000 -1.20000
AFIX 0
C6 1 0.978306 0.452060 0.662178 11.00000 0.08569 0.08925 =
0.08745 -0.00755 0.01611 0.00646
AFIX 43
H6 2 0.957553 0.472183 0.600161 11.00000 -1.20000
AFIX 0
C7 1 0.954544 0.310622 0.849192 11.00000 0.12502 0.16177 =
0.13137 0.05013 -0.02776 -0.04491
AFIX 23
H7A 2 0.938531 0.327824 0.912287 11.00000 -1.20000
H7B 2 0.987677 0.277832 0.872902 11.00000 -1.20000
AFIX 0
C8 1 0.900644 0.275472 0.779252 11.00000 0.19898 0.20934 =
0.15121 0.09141 -0.07051 -0.10751
AFIX 23
H8A 2 0.863526 0.304836 0.767484 11.00000 -1.20000
H8B 2 0.913541 0.265236 0.710241 11.00000 -1.20000
AFIX 0
RESI 4NPE 4
O1 5 0.954613 0.753152 0.375841 11.00000 0.17339 0.15349 =
0.17948 0.05896 -0.04986 -0.06281
O2 5 0.983877 0.684038 0.505131 11.00000 0.14691 0.13253 =
0.15170 0.03395 -0.02595 -0.03908
N1 4 0.948359 0.704025 0.428883 11.00000 0.11911 0.09653 =
0.11050 -0.00327 0.00869 -0.00757
N2 4 0.680494 0.436779 0.263019 11.00000 0.14939 0.10105 =
0.20544 -0.05953 0.07268 -0.01797
AFIX 137
H2A 2 0.649630 0.437195 0.206982 11.00000 -1.20000
H2B 2 0.663940 0.446771 0.322145 11.00000 -1.20000
H2C 2 0.698232 0.395988 0.269674 11.00000 -1.20000
AFIX 0
C1 1 0.891056 0.661868 0.394828 11.00000 0.09807 0.07229 =
0.08863 -0.02353 0.02822 0.01512
C2 1 0.878831 0.608619 0.455809 11.00000 0.10521 0.08170 =
0.09387 -0.01596 0.02001 0.00654
AFIX 43
H2 2 0.908171 0.596913 0.515156 11.00000 -1.20000
AFIX 0
C3 1 0.824674 0.572297 0.431683 11.00000 0.10147 0.07529 =
0.08994 -0.01991 0.02327 0.01143
AFIX 43
H3 2 0.816321 0.536532 0.475339 11.00000 -1.20000
AFIX 0
C4 1 0.780652 0.588533 0.340198 11.00000 0.10075 0.08141 =
0.09085 -0.01665 0.02338 0.00982
C5 1 0.797858 0.641026 0.274318 11.00000 0.09270 0.07155 =
0.08786 -0.02256 0.03055 0.01984
AFIX 43
H5 2 0.772289 0.650352 0.209643 11.00000 -1.20000
AFIX 0
C6 1 0.851127 0.677692 0.304632 11.00000 0.10886 0.09681 =
0.10257 -0.00427 0.01632 -0.00062
AFIX 43
H6 2 0.860513 0.714169 0.263207 11.00000 -1.20000
AFIX 0
C7 1 0.722062 0.549321 0.313354 11.00000 0.10075 0.07919 =
0.09936 -0.01346 0.01964 0.01075
AFIX 23
H7A 2 0.689392 0.577969 0.274532 11.00000 -1.20000
H7B 2 0.707066 0.535380 0.379166 11.00000 -1.20000
AFIX 0
C8 1 0.730138 0.487593 0.246723 11.00000 0.09965 0.08408 =
0.10458 -0.02006 0.01041 0.01366
AFIX 23
H8A 2 0.725973 0.499920 0.171634 11.00000 -1.20000
H8B 2 0.772452 0.468568 0.267472 11.00000 -1.20000
AFIX 0
HKLF 4
REM MHT-III-53 in P2(1)/c
REM wR2 = 0.1208, GooF = S = 1.025, Restrained GooF = 1.032 for all data
REM R1 = 0.0521 for 11561 Fo > 4sig(Fo) and 0.0704 for all 14658 data
REM 555 parameters refined using 603 restraints
END
WGHT 0.0421 85.4813
REM Highest difference peak 3.260, deepest hole -2.533, 1-sigma level 0.238
Q1 1 0.7367 0.4984 0.8554 11.00000 0.05 3.26
Q2 1 0.6551 0.2467 0.7634 11.00000 0.05 2.82
Q3 1 0.7194 0.4396 0.7710 11.00000 0.05 2.71
Q4 1 0.4682 0.5098 0.7418 11.00000 0.05 2.65
Q5 1 0.5480 0.3661 0.5417 11.00000 0.05 2.44
Q6 1 0.5910 0.6049 0.9651 11.00000 0.05 2.39
Q7 1 0.8023 0.5271 0.8437 11.00000 0.05 2.30
Q8 1 0.7628 0.3799 0.4653 11.00000 0.05 2.09
Q9 1 1.1130 0.4967 0.7844 11.00000 0.05 2.03
Q10 1 0.8102 0.1440 0.5411 11.00000 0.05 2.01
Q11 1 1.1616 0.4895 0.8546 11.00000 0.05 2.00
Q12 1 0.5018 0.4747 0.7418 11.00000 0.05 1.95
Q13 1 0.4315 0.6270 1.0189 11.00000 0.05 1.94
Q14 1 0.6447 0.4234 0.7609 11.00000 0.05 1.93
Q15 1 0.8966 0.2661 0.8391 11.00000 0.05 1.81
Q16 1 0.8034 0.3793 0.5190 11.00000 0.05 1.78
Q17 1 0.8236 0.1917 0.5284 11.00000 0.05 1.73
Q18 1 0.5906 0.3699 0.4990 11.00000 0.05 1.65
Q19 1 0.7505 0.5037 0.2365 11.00000 0.05 1.49
Q20 1 1.0255 0.3561 0.8436 11.00000 0.05 1.41
;
_shelx_res_checksum 90688
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-8 -2 18 13.2312 8.18957 10
8 2 -18 23.5232 7.43345 6
-7 -2 18 2.44884 6.35939 1
-7 2 18-4.78637 6.77187 10
-7 -2 18-0.65230 7.50987 10
7 2 -18 10.1959 7.11840 6
-6 2 18 7.61403 7.10021 10
-6 -2 18 0.64486 7.42405 10
6 -2 -18-8.39864 7.51684 6
-6 -2 18-0.48838 6.28883 1
6 2 -18-3.75096 6.95218 6
-5 2 18 22.4360 7.51815 10
5 -2 -18 7.49424 7.15157 6
-5 -2 18 4.44940 7.81802 10
5 2 -18 9.15400 6.92008 6
-5 -2 18 16.0490 6.49240 1
-4 2 18 44.5044 7.71516 10
4 -2 -18 15.9729 7.09159 6
-4 -2 18 28.1678 7.56267 10
4 2 -18 23.2668 7.14498 6
-4 -2 18 27.6352 7.02915 1
-3 -2 18 9.71334 6.36866 1
3 -2 -18 2.59863 6.85967 6
-3 2 18-1.65072 6.89391 10
-3 -2 18-2.47247 7.30779 10
3 2 -18 5.25846 6.26083 6
-2 -2 18-6.80599 5.97221 1
2 -2 -18-0.63491 7.03018 6
-2 2 18-6.47419 6.59093 10
-2 -2 18-4.27923 7.53679 10
2 2 -18-1.14336 6.48585 6
-1 2 18 13.7285 6.75033 10
-1 -2 18 8.43069 7.43052 10
1 2 -18 6.69688 6.04597 6
-1 -2 18 9.75534 6.18395 1
0 -2 18 23.5177 6.76019 1
0 2 18 16.5006 6.70583 10
0 -2 18 18.3865 7.30107 10
0 2 -18 17.4386 6.30869 6
1 2 18 19.6884 6.73589 10
1 -2 18 20.4645 7.72800 10
-1 2 -18 20.2322 6.47418 6
1 -2 18 26.0386 6.96347 1
2 -2 18 20.7562 6.97312 1
2 -2 18 19.5237 7.31607 10
2 2 18 31.6946 7.84294 3
3 -2 18 6.78157 6.91483 10
3 2 18 19.6537 7.77100 3
3 -2 18 10.9280 6.50507 1
4 -2 18 2.79109 7.29498 10
4 -2 18 8.50864 6.43627 1
5 -2 18 28.7673 7.68501 10
-13 -3 18-9.75438 7.67505 1
-12 -3 18 9.57474 7.02723 1
11 3 -18 2.78047 7.46612 6
-11 -3 18 2.62555 6.82987 1
10 3 -18-15.5857 8.09030 6
-10 -3 18 10.9006 7.09667 1
-9 -3 18 2.05644 6.45476 1
-9 3 18 7.32535 7.24750 10
-9 -3 18 4.08841 7.66441 10
9 3 -18 9.24285 7.16100 6
-8 -3 18 9.70116 6.81853 1
-8 3 18 22.7064 7.63530 10
-8 -3 18 3.37214 8.11908 10
8 3 -18-0.64399 7.24721 6
-7 -3 18 7.11929 6.33707 1
-7 3 18-9.93803 6.75860 10
7 3 -18-5.03148 7.10337 6
-6 3 18 4.00300 6.69879 10
-6 -3 18 8.57341 7.80132 10
6 3 -18 7.99532 7.14510 6
-6 -3 18 11.6365 6.42224 1
-5 3 18 25.7415 7.07985 10
-5 -3 18 18.1908 7.66414 10
5 3 -18 19.2763 7.15314 6
-5 -3 18 14.1370 6.94545 1
-4 3 18 3.83301 6.74974 10
-4 -3 18 5.78090 7.37923 10
4 3 -18-2.94967 6.97387 6
-4 -3 18-4.53754 6.38259 1
-3 -3 18 3.02949 6.48645 1
-3 3 18 13.3290 6.80239 10
-3 -3 18 7.62113 7.24051 10
3 3 -18 9.84172 6.89052 6
-2 3 18-3.64445 6.45275 10
-2 -3 18 3.14055 7.30636 10
2 3 -18 3.97490 6.24348 6
-2 -3 18-1.51613 6.34228 1
-1 3 18 4.58092 6.45850 10
-1 -3 18 12.3998 7.53323 10
1 3 -18 6.66490 6.51713 6
-1 -3 18 3.04489 6.54932 1
0 -3 18-10.1834 6.72069 1
0 -3 18 0.61263 7.34367 10
0 3 -18-1.63327 6.47595 6
1 -3 18 2.41449 7.05023 10
1 3 18-9.02707 7.51241 3
-1 3 -18 3.19983 5.94389 6
1 -3 18 5.10635 6.49790 1
2 -3 18 16.6316 7.30655 10
2 -3 18 9.74834 6.71785 1
2 3 18 9.35562 6.85420 3
3 -3 18 6.44432 6.98033 10
3 3 18-4.51808 7.35251 3
3 -3 18-0.51675 7.04332 1
4 -3 18 4.64451 7.07077 10
4 3 18 13.3634 7.82570 3
5 -3 18 6.32383 6.97268 10
6 -3 18-6.25598 7.86956 10
-12 -4 18 57.9885 8.41681 1
-11 -4 18 40.5619 7.65679 1
10 4 -18 3.34445 7.65371 6
-10 -4 18 5.34646 6.81688 1
-9 -4 18-2.65223 6.63409 1
-9 4 18 7.17684 6.84261 10
9 4 -18 4.56906 6.96014 6
-8 -4 18 1.05674 6.55883 1
-8 4 18 25.1349 7.45996 10
-8 -4 18 1.37497 7.88995 10
8 4 -18 15.9438 7.32050 6
-7 4 18 10.2533 7.18943 10
-7 -4 18 24.4865 8.06111 10
-7 -4 18 23.6806 6.99708 1
7 4 -18 29.9249 7.43854 6
-6 4 18 26.1373 7.31201 10
-6 -4 18 8.73894 7.85467 10
6 4 -18 11.6058 6.84509 6
-6 -4 18 15.7342 6.66221 1
-5 4 18 8.14658 6.92516 10
-5 -4 18-1.32966 7.52676 10
5 4 -18 12.5817 6.81262 6
-5 -4 18 0.52336 6.29881 1
-4 -4 18 6.81105 6.80336 1
-4 4 18-5.30303 6.94253 10
-4 -4 18-7.90153 7.81540 10
4 4 -18-4.69987 6.57762 6
-3 -4 18 18.3497 6.78371 1
-3 4 18 21.6269 7.21520 10
-3 -4 18 26.0847 7.77787 10
3 4 -18 23.1093 7.11135 6
-2 4 18 26.6100 7.00753 10
-2 -4 18 34.1996 8.15493 10
2 4 -18 37.4635 7.57896 6
-2 -4 18 26.2681 7.20922 1
-1 -4 18 21.6169 7.24819 1
-1 -4 18 5.09660 7.54956 10
1 4 -18 17.3103 6.77690 6
0 -4 18 0.63088 7.50281 10
0 4 -18 9.32644 6.52467 6
0 -4 18-2.11111 6.69375 1
1 -4 18 4.77085 6.74651 1
1 -4 18-9.96341 7.49257 10
1 4 18 5.90411 6.69783 3
-1 4 -18 11.3372 6.48357 6
2 -4 18 0.61347 7.33796 10
-2 4 -18 0.52976 6.12431 6
2 4 18-5.50480 7.86282 3
2 -4 18 6.38870 6.77476 1
3 -4 18 15.1506 7.58971 10
3 4 18 30.4841 8.44985 3
4 -4 18 38.4858 8.25725 10
4 4 18 38.2621 8.22746 3
5 -4 18-0.59648 7.45922 10
-10 -5 18-2.75475 7.05941 1
-9 -5 18 2.19115 7.01832 1
-9 5 18-1.17225 7.29069 10
9 5 -18 1.94438 7.25587 6
-8 -5 18 16.9222 6.89574 1
-8 5 18 2.28081 7.03656 10
8 5 -18 28.5502 7.50462 6
-7 5 18 11.1125 7.35933 10
7 5 -18 9.30928 6.98285 6
-7 -5 18 2.17327 6.66507 1
-6 5 18 3.78652 6.51138 10
-6 -5 18 15.0785 8.10518 10
6 5 -18 10.3740 6.81991 6
-6 -5 18-1.62740 6.87083 1
-5 5 18 2.63517 6.62689 10
-5 -5 18 4.75915 7.82811 10
5 5 -18 1.79560 6.46027 6
-5 -5 18 5.95469 6.78273 1
-4 -5 18 9.20922 6.65408 1
-4 5 18 1.53837 6.57079 10
-4 -5 18 11.4640 8.00414 10
4 5 -18-5.89010 6.66742 6
-3 -5 18-0.66857 8.09090 10
3 5 -18 12.1689 6.87895 6
-3 -5 18 0.54194 6.44632 1
-2 -5 18-1.98681 7.90673 10
2 5 -18-3.42398 6.78663 6
-2 -5 18-1.63072 6.85808 1
-1 -5 18 7.08325 6.86201 1
-1 -5 18 13.7734 7.82537 10
1 5 -18 14.6178 6.87896 6
0 -5 18 14.2831 7.40402 10
0 5 18 17.8426 7.12820 3
0 5 -18-0.55464 6.34134 6
0 -5 18 13.0936 6.83152 1
1 -5 18 13.1506 7.18654 1
1 -5 18 1.92266 7.63819 10
1 5 18-5.79607 6.88126 3
-1 5 -18 10.9064 6.68749 6
2 -5 18-1.65511 6.88968 1
2 -5 18-5.69529 7.67369 10
-2 5 -18-10.7177 6.99482 6
2 5 18-2.40654 6.88542 3
3 -5 18 6.89075 7.52195 10
3 -5 18-12.2031 7.56033 1
3 5 18 8.76177 7.25006 3
4 5 18 20.1905 7.74698 3
-9 -6 18 49.6803 8.25042 1
-8 6 18-0.55668 7.15629 10
-8 -6 18-2.25022 7.14633 1
8 6 -18 1.26856 7.00592 6
-7 6 18 4.33164 6.84288 10
7 6 -18-4.98193 7.21430 6
-7 -6 18 4.48718 6.74815 1
-6 6 18-4.20516 6.45602 10
6 6 -18 4.28804 6.87320 6
-6 -6 18 6.15089 6.81709 1
-5 -6 18 32.4295 7.64825 1
5 6 -18 27.7317 7.71754 6
-4 -6 18 46.4733 8.01711 1
4 6 -18 29.0101 7.43868 6
-3 -6 18 36.2924 8.75931 10
3 6 -18 31.5471 7.50489 6
-3 -6 18 22.3924 7.36457 1
-2 -6 18 24.7022 7.55123 1
-2 -6 18 29.8510 8.14972 10
2 6 -18 12.6616 6.95149 6
-1 -6 18 16.8368 8.33218 10
-1 -6 18 10.6884 7.07783 1
1 6 -18 16.4244 6.98691 6
0 6 -18 5.04834 6.89790 6
0 -6 18 15.7935 7.28365 1
1 6 18 25.0357 7.54977 3
-1 6 -18 22.6794 7.09585 6
1 -6 18 29.4472 7.52626 1
-2 6 -18 17.4473 6.79176 6
2 6 18 16.5670 7.40619 3
2 -6 18 12.5203 7.34861 1
3 6 18-4.31880 7.55099 3
4 6 18 3.21525 7.52682 3
-8 7 18-3.80370 7.17164 10
7 7 -18-18.8093 8.23370 6
6 7 -18 14.1639 7.44124 6
-6 -7 18 15.5423 7.05002 1
-5 -7 18-2.87870 6.93981 1
5 7 -18 1.81986 6.66985 6
-4 -7 18 6.34334 7.00990 1
4 7 -18 10.1550 6.73791 6
3 7 -18 7.06858 7.02623 6
-3 -7 18 12.1210 7.47685 1
-2 -7 18-13.9004 7.70583 1
2 7 -18 2.90924 6.97589 6
1 7 -18-7.46857 6.92667 6
-1 -7 18-0.57997 7.09841 1
0 7 -18 19.3105 6.82709 6
-1 7 -18 14.0798 6.66277 6
-2 7 -18 39.0663 7.77661 6
2 7 18 40.1495 8.02788 3
-3 7 -18 4.41499 6.90892 6
3 7 18 15.8140 7.66668 3
4 7 18-0.63480 7.39927 3
5 8 -18-7.95997 7.51142 6
4 8 -18-3.62400 7.07009 6
3 8 -18 13.1296 7.49051 6
2 8 -18 27.1178 7.53603 6
1 8 -18 27.5045 7.69616 6
0 8 -18-4.64283 7.12952 6
-1 8 -18-9.20884 7.25550 6
-2 8 -18 31.3983 7.34726 6
-3 8 -18 51.5818 8.41386 6
10 9 -18-7.48422 8.15732 5
9 9 -18 10.3872 8.22171 5
8 9 -18 2.19679 7.75058 5
7 9 -18 5.78162 6.93695 5
2 9 -18 3.60372 6.82844 6
1 9 -18 3.57751 6.74963 6
0 9 -18 6.51914 6.99578 6
-1 9 -18-4.69718 7.14641 6
-2 9 -18-14.0346 7.71995 6
-3 9 -18 8.13249 7.12684 6
9 10 -18 12.1522 8.82701 5
8 10 -18 13.6059 8.40045 5
7 10 -18 13.4228 8.43489 5
8 11 -18-4.69559 7.66710 5
7 11 -18 10.8227 7.73282 5
8 0 -19 1.46968 7.19775 6
7 0 -19 15.0475 7.46993 6
6 0 -19-0.70278 7.52966 6
5 0 -19-4.11825 7.54812 6
-4 0 19 11.7346 7.64220 10
4 0 -19-1.34399 6.80800 6
-3 0 19-9.71889 7.84218 10
-2 0 19-17.9004 8.32454 10
-1 0 19 5.84858 7.40688 10
0 0 19 1.14991 7.10031 10
8 1 -19-6.41534 7.49151 6
7 -1 -19-1.48152 7.00005 6
7 1 -19-4.19776 7.62218 6
6 -1 -19-7.22547 7.64963 6
6 1 -19-3.41009 7.62056 6
5 -1 -19-12.7505 8.30776 6
-5 1 19-4.28060 7.41382 10
5 1 -19 9.37746 7.41592 6
4 -1 -19-5.54569 6.71254 6
-4 1 19-0.60051 7.55087 10
4 1 -19-5.87171 7.30530 6
-3 1 19-1.76626 7.40163 10
3 1 -19 0.63754 6.79756 6
-2 1 19-8.67222 7.43840 10
-1 1 19-0.56586 7.22531 10
-9 -2 19 4.60093 6.82255 1
-8 -2 19 14.6792 6.62454 1
-7 -2 19 6.53927 6.54379 1
7 2 -19-15.6993 8.55238 6
-6 -2 19 11.5427 6.32197 1
-6 2 19 7.90436 7.54658 10
6 2 -19 14.7025 7.27432 6
-5 2 19-5.95550 7.34131 10
-5 -2 19 4.51056 6.58190 1
5 2 -19 5.23290 6.80224 6
-4 2 19-2.91409 7.18531 10
4 2 -19 10.8914 7.33032 6
-3 2 19-1.14259 7.35638 10
3 2 -19 0.62949 6.67892 6
-7 -3 19 12.0110 7.04483 1
-6 -3 19 2.08560 6.66901 1
-6 3 19-0.59240 7.47367 10
6 3 -19 1.97466 7.06936 6
-5 3 19-0.57862 7.47563 10
5 3 -19-9.01538 7.35124 6
-5 -3 19 10.9143 6.84731 1
-4 3 19-5.64247 7.31583 10
4 3 -19-2.52978 6.81059 6
-4 -3 19-5.71577 6.82576 1
3 3 -19 8.67329 6.81198 6
-3 -3 19-4.15784 6.78167 1
-2 -3 19 4.16653 6.98189 1
2 3 -19 1.82187 6.52304 6
-1 -3 19 5.75010 7.09573 1
-7 4 19 8.81218 7.16856 10
-6 4 19 6.90610 7.61020 10
5 4 -19 14.0398 7.36338 6
4 4 -19-3.75436 7.33922 6
3 4 -19 3.07608 7.25910 6
2 4 -19 0.60382 7.13805 6
1 4 -19 4.15237 6.83071 6
3 5 -19 1.84141 7.29937 6
2 5 -19 10.8929 7.24858 6
1 5 -19 5.34554 6.78295 6
1 6 -19-4.80915 7.46589 6
0 6 -19-2.95485 7.24544 6
0 0 0 0.00 0.00 0
TITL MHT-III-53 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 21.097616 19.825465 12.614931 90.0000 98.2252 90.0000
ZERR 1.00 0.000427 0.000343 0.000197 0.0000 0.0017 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C N O I Pb
UNIT 180.00 12.00 8.00 32.00 8.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 18132
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id MHT-III-53
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.235
_oxdiff_exptl_absorpt_empirical_full_min 0.860