# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full 'Dalton Trans.'
#TrackingRef '- 6a.cif'
#==============================================================================
_journal_coden_Cambridge 0222
_journal_volume ?
_journal_page_first ?
_journal_year ?
_publ_contact_author_name 'Dr Oliver Reiser'
_publ_contact_author_email Oliver.Reiser@chemie.uni-regensburg.de
_publ_section_title
;
Palladium(II)- and
Platinum(II)phenyl-2,6-bis(oxazole) pincer complexes:
Syntheses, crystal structures, and photophysical properties
;
# 0. AUDIT DETAILS
_audit_creation_date 'Feb 14 10:27:15 2005'
_audit_creation_method 'PLATON
option'
_audit_update_record
;
?
2011-04-07 # Formatted by publCIF
;
_publ_section_exptl_refinement
;
The data were collected at 173 K using an Oxford Cryosystems Cooler (Cosier &
Glazer, 1986). The structure was solved by direct methods (SIR97) and
refined by full-matrix anisotropic least squares (SHELXL97). The
H-atoms were calculated geometrically and a riding model was used during
refinement process.
;
# Insert blank lines between references
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J.
Appl. Cryst. 26, 343--350.
Cosier, J. & Glazer, A. M. (1986). J. Appl. Cryst. 19, 105--107.
Flack, H. D. (1983). Acta Cryst. A39, 876--881.
L. J. Farrugia, J. Appl. Cryst (1997). 30, 565.
Sheldrick, G.M. SHELXL97. Program for crystal structure refinement.
University of G\\"ottingen, Germany, 1997.
Sheldrick, G.M. SHELXS97. Program for Crystal Structure solution.
University of G\\"ottingen, Germany, 1997.
Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194--201.
Spek, A. L. (1990). Acta Cryst. A46 C-34.
STOE (1998). IPDSsoftware, version 2.89, STOE & CIE GmbH, Darmstadt,
Germany.
Wilson, A. J. C. (1992). International Tables for Crystallography, Volume C,
Kluwer Academic Publishers, Dordrecht, The Netherlands.
;
_publ_section_acknowledgements
;
(type here to add acknowledgements)
;
_publ_section_figure_captions
;
View of the title compound with the atom numbering scheme. Displacement
ellipsoids for non-H atoms are drawn at the 50% probability level.
;
loop_
_publ_author_name
'Gang Xu'
'Qunli Luo'
S.Eibauer
A.Rausch
S.Stempfhuber
M.Zabel
H.Yersin
O.Reiser
#===============================================================================
data_e027
_database_code_depnum_ccdc_archive 'CCDC 630898'
#TrackingRef '- 6a.cif'
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
; ?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C16 H15 Br N2 O4 Pd'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural 'C16 H15 Br N2 O4 Pd'
_chemical_formula_sum 'C16 H15 Br N2 O4 Pd'
_chemical_formula_iupac ?
_chemical_formula_weight 485.62
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+z
_cell_length_a 7.5601(8)
_cell_length_b 9.3101(6)
_cell_length_c 24.686(3)
_cell_angle_alpha 90
_cell_angle_beta 90.828(12)
_cell_angle_gamma 90
_cell_volume 1737.4(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 173
_cell_measurement_reflns_used 8000
_cell_measurement_theta_min 3.18
_cell_measurement_theta_max 25.87
_cell_special_details
;
Cell parameters were determined by indexing 8000 reflections with
I/sigma limit 6.0.
;
_exptl_crystal_description prism
_exptl_crystal_colour 'light yellow'
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.08
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.857
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 952
_exptl_absorpt_coefficient_mu 3.390
_exptl_crystal_density_meas_temp ?
# Permitted for :
# analytical 'analytical from crystal shape'
# Example: de Meulenaer&Tompa: ABST
# cylinder 'cylindrical'
# gaussian 'Gaussian from crystal shape'
# Example: PLATON/ABSG
# integration 'integration from crystal shape'
# multi-scan 'symmetry-related measurements'
# Example: SADABS, MULABS
# none 'no absorption corr. applied'
# numerical 'numerical from crystal shape'
# psi-scan 'psi-scan corrections'
# Example: PLATON/ABSP
# refdelf 'refined from delta-F'
# Example: SHELXA, DIFABS, DELABS
# sphere 'spherical'
# Example: PLATON/ABSS
_exptl_absorpt_correction_type analytical
# Example: '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_process_details
'analytical from crystal shape (X-SHAPE, X-RED. STOE, 1996)'
_exptl_absorpt_correction_T_min 0.4459
_exptl_absorpt_correction_T_max 0.7642
loop_
_exptl_crystal_face_index_h_
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 2 0.0280
2 1 -1 0.1114
0 -1 3 0.1823
1 0 -2 0.0580
-2 0 -1 0.0315
-2 1 2 0.1452
-2 -1 -2 0.0679
1 1 9 0.1192
1 -1 -2 0.1332
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
Data were collected applying an imaging plate system (STOE) with the
following measurement parameters:
Detector distance [mm] 70
Phi movement mode Oscillation
Phi incr. [degrees] 0.8
Number of exposures 368
Irradiation / exposure [min] 1.00
For a detailed description of the method see: Sheldrick, G.M., Paulus, E.
Vertesy, L. & Hahn, F. (1995) Acta Cryst. B51, 89-98.
;
_diffrn_ambient_temperature 173(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'STOE-IPDS diffractometer'
_diffrn_measurement_method rotation
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
# number of measured reflections (redundant set)
_diffrn_reflns_number 19590
_diffrn_reflns_av_R_equivalents 0.0360
_diffrn_reflns_av_sigmaI/netI 0.0211
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_theta_min 3.18
_diffrn_reflns_theta_max 25.87
_diffrn_reflns_theta_full 25.87
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_reduction_process
; ?
;
# number of unique reflections
_reflns_number_total 3360
# number of observed reflections (> n sig(I))
_reflns_number_gt 2905
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'STOE (1998)'
_computing_cell_refinement 'STOE (1998)'
_computing_data_reduction 'STOE (1998)'
_computing_structure_solution 'SIR-97 (Altomare, 1993)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 1990)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
Refinement on F^2 for ALL reflections except those
flagged by the user for potential systematic errors.
Weighted R-factors wR and all goodnesses 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
observed criterion of F^2 > 2sigma(F^2) is used only
for calculating -R-factor-obs etc. and is not
relevant to the choice of reflections for refinement.
R-factors based on F^2 are statistically about twice
as large as those based on F, and R-factors based on
ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
# Permitted for _refine_ls_hydrogen_treatment :
# refall - refined all H parameters
# refxyz - refined H coordinates only
# refU - refined H U only
# noref - no refinement of H parameters
# constr - H parameters constrained
# mixed - some constrained, some independent
# undef - H-atom parameters not defined
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack .
_refine_ls_number_reflns 3360
_refine_ls_number_parameters 217
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0272
_refine_ls_R_factor_gt 0.0226
_refine_ls_wR_factor_ref 0.0571
_refine_ls_wR_factor_gt 0.0560
_refine_ls_goodness_of_fit_ref 0.969
_refine_ls_restrained_S_all 0.969
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.680
_refine_diff_density_min -0.290
_refine_diff_density_rms 0.089
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd Uani 0.84700(2) 0.88931(2) 0.63640(1) 1.000 0.0192(1) . .
Br1 Br Uani 0.94583(4) 0.90258(3) 0.73389(1) 1.000 0.0420(1) . .
O1 O Uani 0.9117(2) 1.24553(17) 0.54083(6) 1.000 0.0244(5) . .
O2 O Uani 1.0448(2) 1.44383(18) 0.57572(7) 1.000 0.0289(5) . .
O3 O Uani 0.61774(19) 0.51294(17) 0.58508(6) 1.000 0.0230(5) . .
O4 O Uani 0.5823(2) 0.32940(18) 0.64407(6) 1.000 0.0268(5) . .
N1 N Uani 0.9141(2) 1.09112(19) 0.60945(7) 1.000 0.0214(5) . .
N2 N Uani 0.7485(2) 0.6830(2) 0.63412(7) 1.000 0.0220(5) . .
C1 C Uani 0.9941(3) 1.2180(2) 0.62779(9) 1.000 0.0231(6) . .
C2 C Uani 0.9913(3) 1.3102(2) 0.58531(9) 1.000 0.0233(6) . .
C3 C Uani 0.8682(3) 1.1123(2) 0.55843(9) 1.000 0.0222(6) . .
C4 C Uani 0.7836(3) 0.9980(2) 0.52737(9) 1.000 0.0223(6) . .
C5 C Uani 0.7645(3) 0.8785(2) 0.56092(9) 1.000 0.0207(6) . .
C6 C Uani 0.6865(3) 0.7511(2) 0.54204(9) 1.000 0.0214(6) . .
C7 C Uani 0.6240(3) 0.7440(3) 0.48837(9) 1.000 0.0242(7) . .
C8 C Uani 0.6437(3) 0.8637(3) 0.45505(9) 1.000 0.0264(7) . .
C9 C Uani 0.7232(3) 0.9905(3) 0.47344(9) 1.000 0.0244(7) . .
C10 C Uani 0.6841(3) 0.6478(2) 0.58607(9) 1.000 0.0204(6) . .
C11 C Uani 0.6443(3) 0.4618(2) 0.63732(9) 1.000 0.0229(6) . .
C12 C Uani 0.7251(3) 0.5642(3) 0.66802(9) 1.000 0.0236(6) . .
C13 C Uani 1.1593(3) 1.5027(3) 0.61837(10) 1.000 0.0289(7) . .
C14 C Uani 1.2195(3) 1.6484(3) 0.59920(12) 1.000 0.0361(8) . .
C15 C Uani 0.5940(4) 0.2776(3) 0.70009(10) 1.000 0.0344(8) . .
C16 C Uani 0.5070(4) 0.1329(3) 0.70192(12) 1.000 0.0382(8) . .
H1 H Uiso 1.04110 1.23590 0.66300 1.000 0.0280 calc R
H7 H Uiso 0.56920 0.65910 0.47490 1.000 0.0290 calc R
H8 H Uiso 0.60160 0.85890 0.41860 1.000 0.0320 calc R
H9 H Uiso 0.73620 1.07020 0.44980 1.000 0.0290 calc R
H12 H Uiso 0.75910 0.55670 0.70510 1.000 0.0280 calc R
H13A H Uiso 1.26240 1.43910 0.62480 1.000 0.0350 calc R
H13B H Uiso 1.09350 1.51190 0.65260 1.000 0.0350 calc R
H14A H Uiso 1.28250 1.63790 0.56500 1.000 0.0540 calc R
H14B H Uiso 1.29870 1.69110 0.62650 1.000 0.0540 calc R
H14C H Uiso 1.11630 1.71070 0.59360 1.000 0.0540 calc R
H15A H Uiso 0.53330 0.34510 0.72460 1.000 0.0410 calc R
H15B H Uiso 0.71940 0.26990 0.71190 1.000 0.0410 calc R
H16A H Uiso 0.38150 0.14260 0.69220 1.000 0.0570 calc R
H16B H Uiso 0.51860 0.09320 0.73860 1.000 0.0570 calc R
H16C H Uiso 0.56430 0.06830 0.67620 1.000 0.0570 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
Pd1 0.0227(1) 0.0175(1) 0.0173(1) -0.0003(1) -0.0016(1) -0.0012(1)
Br1 0.0642(2) 0.0370(2) 0.0242(2) 0.0012(1) -0.0171(1) -0.0061(1)
O1 0.0285(8) 0.0202(8) 0.0244(8) 0.0025(7) -0.0006(6) -0.0018(6)
O2 0.0339(9) 0.0206(8) 0.0320(9) 0.0033(7) -0.0032(7) -0.0041(7)
O3 0.0241(8) 0.0216(8) 0.0233(8) 0.0008(7) -0.0020(6) -0.0029(6)
O4 0.0306(8) 0.0217(8) 0.0281(8) 0.0031(7) -0.0016(6) -0.0051(7)
N1 0.0241(9) 0.0189(10) 0.0211(9) 0.0002(8) 0.0015(7) -0.0003(7)
N2 0.0235(9) 0.0202(10) 0.0224(9) 0.0002(8) -0.0007(7) -0.0015(8)
C1 0.0247(10) 0.0193(11) 0.0252(11) -0.0033(9) -0.0001(9) -0.0003(9)
C2 0.0235(10) 0.0205(11) 0.0260(11) -0.0018(10) 0.0006(8) 0.0000(9)
C3 0.0227(10) 0.0198(11) 0.0240(11) 0.0013(9) 0.0019(8) -0.0009(9)
C4 0.0221(10) 0.0228(11) 0.0220(11) 0.0003(9) 0.0009(8) 0.0012(9)
C5 0.0209(10) 0.0233(11) 0.0179(10) -0.0010(9) -0.0007(8) 0.0017(8)
C6 0.0211(10) 0.0218(11) 0.0212(11) -0.0016(9) 0.0016(8) 0.0001(8)
C7 0.0245(11) 0.0247(12) 0.0232(11) -0.0047(9) -0.0016(9) -0.0024(9)
C8 0.0274(11) 0.0321(13) 0.0195(11) -0.0020(10) -0.0026(9) 0.0014(9)
C9 0.0273(11) 0.0247(12) 0.0213(11) 0.0041(9) 0.0020(9) 0.0012(9)
C10 0.0194(10) 0.0188(11) 0.0230(11) -0.0012(9) 0.0003(8) -0.0004(8)
C11 0.0217(10) 0.0227(12) 0.0242(11) 0.0034(9) 0.0016(8) 0.0000(9)
C12 0.0260(11) 0.0221(11) 0.0227(11) 0.0016(9) 0.0012(9) -0.0005(9)
C13 0.0257(11) 0.0238(12) 0.0372(13) -0.0004(11) -0.0014(10) -0.0037(9)
C14 0.0287(12) 0.0242(13) 0.0554(17) 0.0005(12) 0.0029(11) -0.0024(10)
C15 0.0439(14) 0.0315(14) 0.0277(13) 0.0047(11) 0.0020(11) -0.0049(11)
C16 0.0442(15) 0.0313(14) 0.0394(15) 0.0109(12) 0.0084(12) -0.0035(11)
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All su's are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Br1 2.5125(4) . . yes
Pd1 N1 2.0591(18) . . yes
Pd1 N2 2.0605(18) . . yes
Pd1 C5 1.959(2) . . yes
O1 C2 1.383(3) . . yes
O1 C3 1.356(2) . . yes
O2 C2 1.331(3) . . yes
O2 C13 1.460(3) . . yes
O3 C10 1.352(2) . . yes
O3 C11 1.387(3) . . yes
O4 C11 1.330(3) . . yes
O4 C15 1.466(3) . . yes
N1 C1 1.399(3) . . yes
N1 C3 1.316(3) . . yes
N2 C10 1.317(3) . . yes
N2 C12 1.400(3) . . yes
C1 C2 1.355(3) . . no
C3 C4 1.454(3) . . no
C4 C5 1.396(3) . . no
C4 C9 1.403(3) . . no
C5 C6 1.401(3) . . no
C6 C7 1.402(3) . . no
C6 C10 1.452(3) . . no
C7 C8 1.394(4) . . no
C8 C9 1.398(4) . . no
C11 C12 1.358(3) . . no
C13 C14 1.509(4) . . no
C15 C16 1.500(4) . . no
C1 H1 0.9490 . . no
C7 H7 0.9503 . . no
C8 H8 0.9511 . . no
C9 H9 0.9500 . . no
C12 H12 0.9497 . . no
C13 H13A 0.9898 . . no
C13 H13B 0.9904 . . no
C14 H14A 0.9802 . . no
C14 H14B 0.9793 . . no
C14 H14C 0.9804 . . no
C15 H15A 0.9898 . . no
C15 H15B 0.9904 . . no
C16 H16A 0.9795 . . no
C16 H16B 0.9808 . . no
C16 H16C 0.9800 . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pd1 N1 101.15(5) . . . yes
Br1 Pd1 N2 100.04(5) . . . yes
Br1 Pd1 C5 178.73(7) . . . yes
N1 Pd1 N2 158.81(7) . . . yes
N1 Pd1 C5 79.40(7) . . . yes
N2 Pd1 C5 79.41(7) . . . yes
C2 O1 C3 104.40(16) . . . yes
C2 O2 C13 113.66(19) . . . yes
C10 O3 C11 104.68(16) . . . yes
C11 O4 C15 113.98(18) . . . yes
Pd1 N1 C1 140.63(14) . . . yes
Pd1 N1 C3 112.52(13) . . . yes
C1 N1 C3 106.85(17) . . . yes
Pd1 N2 C10 112.66(14) . . . yes
Pd1 N2 C12 140.26(15) . . . yes
C10 N2 C12 107.07(18) . . . yes
N1 C1 C2 106.41(19) . . . yes
O1 C2 O2 113.32(18) . . . yes
O1 C2 C1 109.91(17) . . . yes
O2 C2 C1 136.8(2) . . . yes
O1 C3 N1 112.44(18) . . . yes
O1 C3 C4 127.38(19) . . . yes
N1 C3 C4 120.17(18) . . . yes
C3 C4 C5 108.60(19) . . . no
C3 C4 C9 132.2(2) . . . no
C5 C4 C9 119.2(2) . . . no
Pd1 C5 C4 119.29(15) . . . yes
Pd1 C5 C6 119.11(15) . . . yes
C4 C5 C6 121.6(2) . . . no
C5 C6 C7 119.3(2) . . . no
C5 C6 C10 108.75(19) . . . no
C7 C6 C10 132.0(2) . . . no
C6 C7 C8 118.9(2) . . . no
C7 C8 C9 122.2(2) . . . no
C4 C9 C8 118.9(2) . . . no
O3 C10 N2 112.31(18) . . . yes
O3 C10 C6 127.61(19) . . . yes
N2 C10 C6 120.07(18) . . . yes
O3 C11 O4 112.84(18) . . . yes
O3 C11 C12 109.63(18) . . . yes
O4 C11 C12 137.5(2) . . . yes
N2 C12 C11 106.31(19) . . . yes
O2 C13 C14 106.8(2) . . . yes
O4 C15 C16 107.7(2) . . . yes
N1 C1 H1 126.79 . . . no
C2 C1 H1 126.80 . . . no
C6 C7 H7 120.61 . . . no
C8 C7 H7 120.54 . . . no
C7 C8 H8 118.91 . . . no
C9 C8 H8 118.91 . . . no
C4 C9 H9 120.59 . . . no
C8 C9 H9 120.54 . . . no
N2 C12 H12 126.84 . . . no
C11 C12 H12 126.85 . . . no
O2 C13 H13A 110.39 . . . no
O2 C13 H13B 110.35 . . . no
C14 C13 H13A 110.34 . . . no
C14 C13 H13B 110.32 . . . no
H13A C13 H13B 108.60 . . . no
C13 C14 H14A 109.45 . . . no
C13 C14 H14B 109.47 . . . no
C13 C14 H14C 109.45 . . . no
H14A C14 H14B 109.47 . . . no
H14A C14 H14C 109.46 . . . no
H14B C14 H14C 109.53 . . . no
O4 C15 H15A 110.22 . . . no
O4 C15 H15B 110.24 . . . no
C16 C15 H15A 110.15 . . . no
C16 C15 H15B 110.14 . . . no
H15A C15 H15B 108.44 . . . no
C15 C16 H16A 109.48 . . . no
C15 C16 H16B 109.44 . . . no
C15 C16 H16C 109.48 . . . no
H16A C16 H16B 109.53 . . . no
H16A C16 H16C 109.48 . . . no
H16B C16 H16C 109.41 . . . no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 Pd1 N1 C1 1.9(2) . . . . no
N2 Pd1 N1 C1 -178.92(19) . . . . no
C5 Pd1 N1 C1 -179.3(2) . . . . no
Br1 Pd1 N1 C3 -177.71(13) . . . . no
N2 Pd1 N1 C3 1.5(3) . . . . no
C5 Pd1 N1 C3 1.13(15) . . . . no
Br1 Pd1 N2 C10 179.26(14) . . . . no
N1 Pd1 N2 C10 0.1(3) . . . . no
C5 Pd1 N2 C10 0.42(15) . . . . no
Br1 Pd1 N2 C12 0.1(2) . . . . no
N1 Pd1 N2 C12 -179.1(2) . . . . no
C5 Pd1 N2 C12 -178.8(2) . . . . no
N2 Pd1 C5 C4 179.31(19) . . . . no
N1 Pd1 C5 C6 179.63(19) . . . . no
N1 Pd1 C5 C4 -0.83(17) . . . . no
N2 Pd1 C5 C6 -0.24(17) . . . . no
C3 O1 C2 C1 -0.2(2) . . . . no
C2 O1 C3 N1 0.1(2) . . . . no
C2 O1 C3 C4 -178.8(2) . . . . no
C3 O1 C2 O2 179.69(18) . . . . no
C13 O2 C2 C1 11.4(4) . . . . no
C13 O2 C2 O1 -168.45(17) . . . . no
C2 O2 C13 C14 175.44(19) . . . . no
C10 O3 C11 O4 178.59(18) . . . . no
C10 O3 C11 C12 -0.3(2) . . . . no
C11 O3 C10 N2 0.0(2) . . . . no
C11 O3 C10 C6 -178.5(2) . . . . no
C15 O4 C11 C12 3.7(4) . . . . no
C11 O4 C15 C16 175.7(2) . . . . no
C15 O4 C11 O3 -174.72(19) . . . . no
C1 N1 C3 O1 0.0(2) . . . . no
Pd1 N1 C3 C4 -1.3(3) . . . . no
C1 N1 C3 C4 179.0(2) . . . . no
Pd1 N1 C1 C2 -179.66(16) . . . . no
C3 N1 C1 C2 -0.1(2) . . . . no
Pd1 N1 C3 O1 179.69(13) . . . . no
C10 N2 C12 C11 -0.4(2) . . . . no
C12 N2 C10 C6 178.9(2) . . . . no
Pd1 N2 C10 C6 -0.6(3) . . . . no
Pd1 N2 C12 C11 178.82(16) . . . . no
Pd1 N2 C10 O3 -179.23(13) . . . . no
C12 N2 C10 O3 0.2(2) . . . . no
N1 C1 C2 O2 -179.7(2) . . . . no
N1 C1 C2 O1 0.1(3) . . . . no
N1 C3 C4 C9 -179.5(2) . . . . no
O1 C3 C4 C9 -0.6(4) . . . . no
N1 C3 C4 C5 0.7(3) . . . . no
O1 C3 C4 C5 179.5(2) . . . . no
C3 C4 C5 C6 179.9(2) . . . . no
C9 C4 C5 Pd1 -179.50(17) . . . . no
C3 C4 C9 C8 -179.2(2) . . . . no
C5 C4 C9 C8 0.7(3) . . . . no
C3 C4 C5 Pd1 0.4(3) . . . . no
C9 C4 C5 C6 0.0(3) . . . . no
C4 C5 C6 C10 -179.5(2) . . . . no
C4 C5 C6 C7 -0.9(3) . . . . no
Pd1 C5 C6 C10 0.0(3) . . . . no
Pd1 C5 C6 C7 178.69(17) . . . . no
C5 C6 C7 C8 0.9(3) . . . . no
C7 C6 C10 O3 0.4(4) . . . . no
C5 C6 C10 N2 0.4(3) . . . . no
C5 C6 C10 O3 178.8(2) . . . . no
C10 C6 C7 C8 179.2(2) . . . . no
C7 C6 C10 N2 -178.1(2) . . . . no
C6 C7 C8 C9 -0.2(3) . . . . no
C7 C8 C9 C4 -0.6(4) . . . . no
O3 C11 C12 N2 0.4(2) . . . . no
O4 C11 C12 N2 -178.0(2) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Pd1 C14 3.726(3) . 1_545 no
Pd1 C16 3.806(3) . 1_565 no
Pd1 H14C 2.8441 . 1_545 no
Pd1 H16C 2.8932 . 1_565 no
Br1 N1 3.5431(18) . . no
Br1 N2 3.5163(18) . . no
Br1 H1 2.9816 . 2_746 no
Br1 H12 3.0342 . 2_756 no
Br1 H13B 3.0001 . 2_746 no
Br1 H15B 3.1023 . 2_756 no
O1 N1 2.222(2) . . no
O2 C10 3.336(3) . 1_565 no
O2 C11 3.412(3) . 1_565 no
O3 C2 3.397(3) . 1_545 no
O3 C14 3.287(3) . 1_445 no
O4 C1 3.311(3) . 1_545 no
O3 H14A 2.8260 . 1_445 no
O3 H7 2.5874 . 3_666 no
O4 H13A 2.6618 . 1_445 no
O4 H8 2.7088 . 3_666 no
N1 Br1 3.5431(18) . . no
N1 O1 2.222(2) . . no
N1 C4 2.403(3) . . no
N1 C5 2.568(3) . . no
N2 Br1 3.5163(18) . . no
N2 C5 2.569(3) . . no
N2 C6 2.400(3) . . no
C1 O4 3.311(3) . 1_565 no
C1 C11 3.496(3) . 1_565 no
C1 C15 3.578(4) . 1_565 no
C1 C8 3.524(3) . 3_776 no
C2 O3 3.397(3) . 1_565 no
C2 C11 3.259(3) . 1_565 no
C2 C8 3.363(3) . 3_776 no
C2 C7 3.489(3) . 3_776 no
C3 C4 3.554(3) . 3_776 no
C3 C9 3.339(3) . 3_776 no
C4 C3 3.554(3) . 3_776 no
C4 C4 3.558(3) . 3_776 no
C4 C8 3.510(3) . 3_676 no
C5 C3 2.315(3) . . no
C5 C10 2.319(3) . . no
C5 N1 2.568(3) . . no
C5 N2 2.569(3) . . no
C7 C2 3.489(3) . 3_776 no
C8 C1 3.524(3) . 3_776 no
C8 C2 3.363(3) . 3_776 no
C8 C4 3.510(3) . 3_676 no
C8 C9 3.577(3) . 3_676 no
C9 C8 3.577(3) . 3_676 no
C9 C3 3.339(3) . 3_776 no
C10 O2 3.336(3) . 1_545 no
C10 C14 3.532(3) . 1_445 no
C11 O2 3.412(3) . 1_545 no
C11 C2 3.259(3) . 1_545 no
C11 C1 3.496(3) . 1_545 no
C12 C13 3.567(3) . 1_545 no
C13 C12 3.567(3) . 1_565 no
C14 C10 3.532(3) . 1_665 no
C14 O3 3.287(3) . 1_665 no
C14 Pd1 3.726(3) . 1_565 no
C15 C1 3.578(4) . 1_545 no
C16 Pd1 3.806(3) . 1_545 no
C1 H15B 2.9970 . 1_565 no
C1 H13B 2.9006 . . no
C1 H13A 2.8916 . . no
C10 H14A 3.0743 . 1_445 no
C11 H13A 2.9069 . 1_445 no
C12 H15B 2.9469 . . no
C12 H13B 2.8583 . 1_545 no
C12 H15A 2.8763 . . no
C12 H16B 2.9839 . 2_656 no
C13 H1 2.8654 . . no
C14 H9 2.9070 . 3_786 no
C15 H12 2.8846 . . no
C16 H8 3.0759 . 3_666 no
H1 C13 2.8654 . . no
H1 Br1 2.9816 . 2_756 no
H7 O3 2.5874 . 3_666 no
H8 O4 2.7088 . 3_666 no
H8 C16 3.0759 . 3_666 no
H9 C14 2.9070 . 3_786 no
H9 H14C 2.5665 . 3_786 no
H12 C15 2.8846 . . no
H12 Br1 3.0342 . 2_746 no
H12 H16B 2.5572 . 2_656 no
H13A O4 2.6618 . 1_665 no
H13A C1 2.8916 . . no
H13A C11 2.9069 . 1_665 no
H13B C1 2.9006 . . no
H13B C12 2.8583 . 1_565 no
H13B Br1 3.0001 . 2_756 no
H14A O3 2.8260 . 1_665 no
H14A C10 3.0743 . 1_665 no
H14C Pd1 2.8441 . 1_565 no
H14C H9 2.5665 . 3_786 no
H15A C12 2.8763 . . no
H15A H16B 2.5149 . 2_656 no
H15B C1 2.9970 . 1_545 no
H15B C12 2.9469 . . no
H15B Br1 3.1023 . 2_746 no
H16B C12 2.9839 . 2_646 no
H16B H12 2.5572 . 2_646 no
H16B H15A 2.5149 . 2_646 no
H16C Pd1 2.8932 . 1_545 no
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
_geom_hbond_publ_flag
C7 H7 O3 0.9500 2.5900 3.501(3) 161.00 3_666 yes
#===END
# Attachment '- 6c.cif'
# CIF-file generated for Luo0426 Luo/Reiser
#==============================================================================
data_e121
_database_code_depnum_ccdc_archive 'CCDC 817026'
#TrackingRef '- 6c.cif'
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
; ?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C16 H13 Br N2 O5 Pd'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural 'C16 H13 Br N2 O5 Pd'
_chemical_formula_sum 'C16 H13 Br N2 O5 Pd'
_chemical_formula_iupac ?
_chemical_formula_weight 499.60
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
_cell_length_a 9.6564(11)
_cell_length_b 10.0610(12)
_cell_length_c 10.5897(12)
_cell_angle_alpha 107.986(13)
_cell_angle_beta 112.136(12)
_cell_angle_gamma 100.062(13)
_cell_volume 855.5(2)
_cell_formula_units_Z 2
_cell_measurement_temperature 173
_cell_measurement_reflns_used 8000
_cell_measurement_theta_min 2.41
_cell_measurement_theta_max 27.93
_cell_special_details
;
Cell parameters were determined by indexing 8000 reflections with
I/sigma limit 6.0.
;
_exptl_crystal_description prism
_exptl_crystal_colour 'yellow to orange'
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.14
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.939
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 488
_exptl_absorpt_coefficient_mu 3.449
_exptl_crystal_density_meas_temp ?
# Permitted for :
# analytical 'analytical from crystal shape'
# Example: de Meulenaer&Tompa: ABST
# cylinder 'cylindrical'
# gaussian 'Gaussian from crystal shape'
# Example: PLATON/ABSG
# integration 'integration from crystal shape'
# multi-scan 'symmetry-related measurements'
# Example: SADABS, MULABS
# none 'no absorption corr. applied'
# numerical 'numerical from crystal shape'
# psi-scan 'psi-scan corrections'
# Example: PLATON/ABSP
# refdelf 'refined from delta-F'
# Example: SHELXA, DIFABS, DELABS
# sphere 'spherical'
# Example: PLATON/ABSS
_exptl_absorpt_correction_type analytical
# Example: '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_process_details
'analytical from crystal shape (X-SHAPE, X-RED. STOE, 1996)'
_exptl_absorpt_correction_T_min 0.3711
_exptl_absorpt_correction_T_max 0.7039
loop_
_exptl_crystal_face_index_h_
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 3 0.0382
0 -3 -1 0.0734
1 1 -2 0.1694
-1 1 1 0.1313
1 -2 2 0.1349
0 3 1 0.0721
-1 2 -3 0.0887
-1 -1 3 0.1173
2 -1 -3 0.1573
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
Data were collected applying an imaging plate system (STOE) with the
following measurement parameters:
Detector distance [mm] 60
Phi movement mode Oscillation
Phi incr. [degrees] 1.4
Number of exposures 190
Irradiation / exposure [min] 4.00
For a detailed description of the method see: Sheldrick, G.M., Paulus, E.
Vertesy, L. & Hahn, F. (1995) Acta Cryst. B51, 89-98.
;
_diffrn_ambient_temperature 173(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'STOE-IPDS diffractometer'
_diffrn_measurement_method rotation
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
# number of measured reflections (redundant set)
_diffrn_reflns_number 10880
_diffrn_reflns_av_R_equivalents 0.0326
_diffrn_reflns_av_sigmaI/netI 0.0270
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 2.41
_diffrn_reflns_theta_max 27.93
_diffrn_reflns_theta_full 27.93
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measured_fraction_theta_full 0.919
_diffrn_reflns_reduction_process
; ?
;
# number of unique reflections
_reflns_number_total 3756
# number of observed reflections (> n sig(I))
_reflns_number_gt 3258
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'STOE (1998)'
_computing_cell_refinement 'STOE (1998)'
_computing_data_reduction 'STOE (1998)'
_computing_structure_solution 'SIR-97 (Altomare, 1993)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 2003)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
Refinement on F^2 for ALL reflections except those
flagged by the user for potential systematic errors.
Weighted R-factors wR and all goodnesses 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
observed criterion of F^2 > 2sigma(F^2) is used only
for calculating -R-factor-obs etc. and is not
relevant to the choice of reflections for refinement.
R-factors based on F^2 are statistically about twice
as large as those based on F, and R-factors based on
ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
# Permitted for _refine_ls_hydrogen_treatment :
# refall - refined all H parameters
# refxyz - refined H coordinates only
# refU - refined H U only
# noref - no refinement of H parameters
# constr - H parameters constrained
# mixed - some constrained, some independent
# undef - H-atom parameters not defined
_refine_ls_hydrogen_treatment ' constr'
_refine_ls_extinction_method none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack .
_refine_ls_number_reflns 3756
_refine_ls_number_parameters 226
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0293
_refine_ls_R_factor_gt 0.0238
_refine_ls_wR_factor_ref 0.0596
_refine_ls_wR_factor_gt 0.0580
_refine_ls_goodness_of_fit_ref 0.963
_refine_ls_restrained_S_all 0.963
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.466
_refine_diff_density_min -0.376
_refine_diff_density_rms 0.070
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd Uani 0.26087(2) 0.44111(2) 0.45582(2) 1.000 0.0339(1) . .
Br1 Br Uani 0.22659(4) 0.16727(3) 0.37439(3) 1.000 0.0529(1) . .
O1 O Uani 0.4075(2) 0.7356(2) 0.2933(2) 1.000 0.0513(6) . .
O2 O Uani 0.4737(4) 0.3490(3) 0.0563(3) 1.000 0.0805(10) . .
O3 O Uani 0.3694(3) 0.2551(2) 0.1779(2) 1.000 0.0571(7) . .
O4 O Uani 0.1141(2) 0.55672(19) 0.7779(2) 1.000 0.0461(6) . .
O5 O Uani 0.0410(3) 0.3860(2) 0.8594(2) 1.000 0.0557(7) . .
N1 N Uani 0.3496(2) 0.5316(2) 0.3326(2) 1.000 0.0383(6) . .
N2 N Uani 0.1783(3) 0.4365(2) 0.6067(2) 1.000 0.0389(6) . .
C1 C Uani 0.2621(3) 0.6452(2) 0.5348(3) 1.000 0.0383(7) . .
C2 C Uani 0.3107(3) 0.7446(3) 0.4814(3) 1.000 0.0419(7) . .
C3 C Uani 0.3073(3) 0.8892(3) 0.5347(3) 1.000 0.0500(9) . .
C4 C Uani 0.2501(4) 0.9293(3) 0.6392(4) 1.000 0.0563(10) . .
C5 C Uani 0.1983(4) 0.8300(3) 0.6926(3) 1.000 0.0509(9) . .
C6 C Uani 0.2069(3) 0.6875(3) 0.6413(3) 1.000 0.0417(7) . .
C7 C Uani 0.3571(3) 0.6721(3) 0.3702(3) 1.000 0.0414(7) . .
C8 C Uani 0.4374(4) 0.6273(3) 0.2021(3) 1.000 0.0532(9) . .
C9 C Uani 0.4030(3) 0.5020(3) 0.2230(3) 1.000 0.0440(8) . .
C10 C Uani 0.4196(3) 0.3623(3) 0.1433(3) 1.000 0.0470(8) . .
C11 C Uani 0.3748(4) 0.1109(3) 0.1036(4) 1.000 0.0652(11) . .
C12 C Uani 0.1651(3) 0.5620(3) 0.6767(3) 1.000 0.0396(7) . .
C13 C Uani 0.0938(3) 0.4137(3) 0.7672(3) 1.000 0.0441(8) . .
C14 C Uani 0.1329(3) 0.3376(3) 0.6637(3) 1.000 0.0420(8) . .
C15 C Uani 0.0237(4) 0.2364(3) 0.8516(3) 1.000 0.0514(9) . .
C16 C Uani -0.0287(4) 0.2231(4) 0.9652(4) 1.000 0.0616(11) . .
H3A H Uiso 0.34300 0.95860 0.50060 1.000 0.0600 calc R
H4A H Uiso 0.24630 1.02700 0.67500 1.000 0.0680 calc R
H5A H Uiso 0.15810 0.85880 0.76230 1.000 0.0610 calc R
H8A H Uiso 0.47620 0.63840 0.13450 1.000 0.0640 calc R
H11A H Uiso 0.28420 0.06050 0.00350 1.000 0.0780 calc R
H11B H Uiso 0.37040 0.05240 0.16160 1.000 0.0780 calc R
H11C H Uiso 0.47340 0.12190 0.09530 1.000 0.0780 calc R
H14A H Uiso 0.13020 0.23760 0.63540 1.000 0.0500 calc R
H15A H Uiso 0.12590 0.21800 0.87350 1.000 0.0620 calc R
H15B H Uiso -0.05590 0.16290 0.75010 1.000 0.0620 calc R
H16A H Uiso 0.05080 0.29670 1.06500 1.000 0.0740 calc R
H16B H Uiso -0.04050 0.12360 0.96290 1.000 0.0740 calc R
H16C H Uiso -0.13040 0.24050 0.94170 1.000 0.0740 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
Pd1 0.0392(1) 0.0293(1) 0.0365(1) 0.0150(1) 0.0193(1) 0.0114(1)
Br1 0.0774(2) 0.0352(1) 0.0624(2) 0.0228(1) 0.0441(2) 0.0227(1)
O1 0.0576(11) 0.0502(10) 0.0581(11) 0.0332(9) 0.0309(10) 0.0150(8)
O2 0.125(2) 0.0765(16) 0.0840(17) 0.0401(14) 0.0825(18) 0.0401(15)
O3 0.0748(14) 0.0472(10) 0.0619(12) 0.0207(9) 0.0461(12) 0.0182(9)
O4 0.0577(11) 0.0394(9) 0.0490(10) 0.0167(8) 0.0333(10) 0.0163(8)
O5 0.0778(14) 0.0488(10) 0.0578(12) 0.0239(9) 0.0471(12) 0.0196(9)
N1 0.0400(11) 0.0388(10) 0.0386(10) 0.0188(8) 0.0189(9) 0.0114(8)
N2 0.0458(11) 0.0344(9) 0.0404(10) 0.0164(8) 0.0233(10) 0.0121(8)
C1 0.0389(12) 0.0304(10) 0.0437(13) 0.0148(9) 0.0175(11) 0.0113(9)
C2 0.0414(13) 0.0344(11) 0.0481(14) 0.0201(10) 0.0172(12) 0.0106(9)
C3 0.0508(15) 0.0354(12) 0.0603(17) 0.0242(12) 0.0195(14) 0.0120(11)
C4 0.0624(18) 0.0335(12) 0.0694(19) 0.0199(12) 0.0259(17) 0.0200(12)
C5 0.0575(16) 0.0389(13) 0.0551(16) 0.0135(11) 0.0282(15) 0.0186(11)
C6 0.0437(13) 0.0344(11) 0.0454(13) 0.0148(10) 0.0207(12) 0.0120(10)
C7 0.0423(13) 0.0399(12) 0.0444(13) 0.0239(10) 0.0186(12) 0.0097(9)
C8 0.0576(17) 0.0588(16) 0.0541(16) 0.0320(14) 0.0313(15) 0.0148(13)
C9 0.0413(13) 0.0523(14) 0.0399(13) 0.0216(11) 0.0199(12) 0.0111(10)
C10 0.0441(14) 0.0565(15) 0.0408(13) 0.0221(12) 0.0207(12) 0.0113(11)
C11 0.078(2) 0.0473(16) 0.070(2) 0.0153(14) 0.0420(19) 0.0176(14)
C12 0.0419(13) 0.0368(11) 0.0388(12) 0.0123(9) 0.0204(11) 0.0117(9)
C13 0.0523(15) 0.0398(12) 0.0454(13) 0.0173(10) 0.0285(13) 0.0137(10)
C14 0.0509(14) 0.0386(12) 0.0438(13) 0.0196(10) 0.0269(12) 0.0145(10)
C15 0.0604(17) 0.0500(15) 0.0476(14) 0.0228(12) 0.0281(14) 0.0143(12)
C16 0.0659(19) 0.0699(19) 0.0588(18) 0.0334(16) 0.0359(17) 0.0151(15)
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All su's are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Br1 2.5382(5) . . yes
Pd1 N1 2.138(2) . . yes
Pd1 N2 2.045(2) . . yes
Pd1 C1 1.959(2) . . yes
O1 C7 1.349(4) . . yes
O1 C8 1.369(4) . . yes
O2 C10 1.204(5) . . yes
O3 C10 1.314(4) . . yes
O3 C11 1.442(4) . . yes
O4 C12 1.348(4) . . yes
O4 C13 1.381(4) . . yes
O5 C13 1.336(4) . . yes
O5 C15 1.458(4) . . yes
N1 C7 1.326(4) . . yes
N1 C9 1.412(4) . . yes
N2 C12 1.308(4) . . yes
N2 C14 1.402(4) . . yes
C1 C2 1.388(4) . . no
C1 C6 1.405(4) . . no
C2 C3 1.400(4) . . no
C2 C7 1.449(4) . . no
C3 C4 1.398(5) . . no
C4 C5 1.398(5) . . no
C5 C6 1.397(5) . . no
C6 C12 1.458(5) . . no
C8 C9 1.353(5) . . no
C9 C10 1.470(4) . . no
C13 C14 1.351(4) . . no
C15 C16 1.502(5) . . no
C3 H3A 0.9498 . . no
C4 H4A 0.9509 . . no
C5 H5A 0.9500 . . no
C8 H8A 0.9498 . . no
C11 H11A 0.9800 . . no
C11 H11B 0.9796 . . no
C11 H11C 0.9792 . . no
C14 H14A 0.9495 . . no
C15 H15A 0.9899 . . no
C15 H15B 0.9904 . . no
C16 H16A 0.9804 . . no
C16 H16B 0.9791 . . no
C16 H16C 0.9797 . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pd1 N1 111.11(6) . . . yes
Br1 Pd1 N2 90.94(6) . . . yes
Br1 Pd1 C1 169.58(9) . . . yes
N1 Pd1 N2 157.94(8) . . . yes
N1 Pd1 C1 78.89(10) . . . yes
N2 Pd1 C1 79.06(10) . . . yes
C7 O1 C8 104.9(2) . . . yes
C10 O3 C11 118.0(3) . . . yes
C12 O4 C13 104.3(2) . . . yes
C13 O5 C15 113.4(3) . . . yes
Pd1 N1 C7 110.04(17) . . . yes
Pd1 N1 C9 145.34(19) . . . yes
C7 N1 C9 104.6(2) . . . yes
Pd1 N2 C12 114.04(19) . . . yes
Pd1 N2 C14 139.0(2) . . . yes
C12 N2 C14 107.0(2) . . . yes
Pd1 C1 C2 120.3(2) . . . yes
Pd1 C1 C6 119.1(2) . . . yes
C2 C1 C6 120.6(3) . . . no
C1 C2 C3 120.3(3) . . . no
C1 C2 C7 109.4(3) . . . no
C3 C2 C7 130.3(3) . . . no
C2 C3 C4 118.6(3) . . . no
C3 C4 C5 122.0(3) . . . no
C4 C5 C6 118.6(3) . . . no
C1 C6 C5 120.0(3) . . . no
C1 C6 C12 108.5(3) . . . no
C5 C6 C12 131.5(3) . . . no
O1 C7 N1 113.5(2) . . . yes
O1 C7 C2 125.1(3) . . . yes
N1 C7 C2 121.4(3) . . . yes
O1 C8 C9 109.5(3) . . . yes
N1 C9 C8 107.6(3) . . . yes
N1 C9 C10 127.7(3) . . . yes
C8 C9 C10 124.8(3) . . . no
O2 C10 O3 124.3(3) . . . yes
O2 C10 C9 123.2(3) . . . yes
O3 C10 C9 112.6(3) . . . yes
O4 C12 N2 112.7(3) . . . yes
O4 C12 C6 128.1(3) . . . yes
N2 C12 C6 119.2(3) . . . yes
O4 C13 O5 113.2(2) . . . yes
O4 C13 C14 110.1(3) . . . yes
O5 C13 C14 136.6(3) . . . yes
N2 C14 C13 105.9(3) . . . yes
O5 C15 C16 107.7(3) . . . yes
C2 C3 H3A 120.75 . . . no
C4 C3 H3A 120.68 . . . no
C3 C4 H4A 119.01 . . . no
C5 C4 H4A 119.03 . . . no
C4 C5 H5A 120.71 . . . no
C6 C5 H5A 120.68 . . . no
O1 C8 H8A 125.24 . . . no
C9 C8 H8A 125.26 . . . no
O3 C11 H11A 109.44 . . . no
O3 C11 H11B 109.46 . . . no
O3 C11 H11C 109.45 . . . no
H11A C11 H11B 109.48 . . . no
H11A C11 H11C 109.54 . . . no
H11B C11 H11C 109.46 . . . no
N2 C14 H14A 127.06 . . . no
C13 C14 H14A 127.03 . . . no
O5 C15 H15A 110.15 . . . no
O5 C15 H15B 110.11 . . . no
C16 C15 H15A 110.21 . . . no
C16 C15 H15B 110.25 . . . no
H15A C15 H15B 108.43 . . . no
C15 C16 H16A 109.41 . . . no
C15 C16 H16B 109.42 . . . no
C15 C16 H16C 109.41 . . . no
H16A C16 H16B 109.52 . . . no
H16A C16 H16C 109.52 . . . no
H16B C16 H16C 109.54 . . . no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 Pd1 N1 C7 176.08(16) . . . . no
N2 Pd1 N1 C7 -2.1(3) . . . . no
C1 Pd1 N1 C7 -0.83(19) . . . . no
Br1 Pd1 N1 C9 -2.6(3) . . . . no
N2 Pd1 N1 C9 179.3(3) . . . . no
C1 Pd1 N1 C9 -179.5(3) . . . . no
Br1 Pd1 N2 C12 -176.3(2) . . . . no
N1 Pd1 N2 C12 2.0(4) . . . . no
C1 Pd1 N2 C12 0.8(2) . . . . no
Br1 Pd1 N2 C14 5.8(3) . . . . no
N1 Pd1 N2 C14 -175.9(2) . . . . no
C1 Pd1 N2 C14 -177.2(3) . . . . no
N1 Pd1 C1 C2 1.0(2) . . . . no
N2 Pd1 C1 C2 -179.5(3) . . . . no
N1 Pd1 C1 C6 178.4(2) . . . . no
N2 Pd1 C1 C6 -2.1(2) . . . . no
C8 O1 C7 N1 -1.4(3) . . . . no
C8 O1 C7 C2 -179.9(3) . . . . no
C7 O1 C8 C9 1.0(3) . . . . no
C11 O3 C10 C9 178.1(3) . . . . no
C11 O3 C10 O2 -2.0(5) . . . . no
C13 O4 C12 C6 -179.4(3) . . . . no
C12 O4 C13 O5 -179.3(2) . . . . no
C12 O4 C13 C14 0.5(3) . . . . no
C13 O4 C12 N2 -0.3(3) . . . . no
C15 O5 C13 C14 2.0(5) . . . . no
C15 O5 C13 O4 -178.3(2) . . . . no
C13 O5 C15 C16 177.4(3) . . . . no
C9 N1 C7 C2 179.8(3) . . . . no
C7 N1 C9 C10 179.6(3) . . . . no
C7 N1 C9 C8 -0.5(3) . . . . no
Pd1 N1 C9 C8 178.2(2) . . . . no
Pd1 N1 C7 C2 0.6(3) . . . . no
Pd1 N1 C7 O1 -178.02(18) . . . . no
Pd1 N1 C9 C10 -1.7(5) . . . . no
C9 N1 C7 O1 1.2(3) . . . . no
C14 N2 C12 C6 179.2(3) . . . . no
Pd1 N2 C12 C6 0.6(3) . . . . no
Pd1 N2 C14 C13 178.3(2) . . . . no
Pd1 N2 C12 O4 -178.50(18) . . . . no
C12 N2 C14 C13 0.2(3) . . . . no
C14 N2 C12 O4 0.1(3) . . . . no
Pd1 C1 C6 C5 -176.3(2) . . . . no
Pd1 C1 C2 C3 178.2(2) . . . . no
C6 C1 C2 C7 -178.3(3) . . . . no
Pd1 C1 C6 C12 2.9(3) . . . . no
C2 C1 C6 C12 -179.8(3) . . . . no
Pd1 C1 C2 C7 -1.0(3) . . . . no
C2 C1 C6 C5 1.0(4) . . . . no
C6 C1 C2 C3 0.9(4) . . . . no
C7 C2 C3 C4 177.2(3) . . . . no
C1 C2 C7 N1 0.2(4) . . . . no
C1 C2 C3 C4 -1.7(4) . . . . no
C3 C2 C7 O1 -0.4(5) . . . . no
C3 C2 C7 N1 -178.9(3) . . . . no
C1 C2 C7 O1 178.6(3) . . . . no
C2 C3 C4 C5 0.7(5) . . . . no
C3 C4 C5 C6 1.1(5) . . . . no
C4 C5 C6 C12 179.1(3) . . . . no
C4 C5 C6 C1 -2.0(5) . . . . no
C1 C6 C12 N2 -2.2(4) . . . . no
C5 C6 C12 O4 -4.1(5) . . . . no
C1 C6 C12 O4 176.8(3) . . . . no
C5 C6 C12 N2 176.9(3) . . . . no
O1 C8 C9 C10 179.6(3) . . . . no
O1 C8 C9 N1 -0.3(3) . . . . no
C8 C9 C10 O2 3.9(5) . . . . no
N1 C9 C10 O3 3.6(4) . . . . no
N1 C9 C10 O2 -176.2(3) . . . . no
C8 C9 C10 O3 -176.2(3) . . . . no
O5 C13 C14 N2 179.2(3) . . . . no
O4 C13 C14 N2 -0.4(3) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Pd1 O3 3.588(3) . . no
Pd1 C7 3.993(3) . 2_666 no
Pd1 Pd1 4.2136(6) . 2_666 no
Pd1 O3 3.945(2) . 2_666 no
Pd1 O4 3.542(2) . 2_566 no
Pd1 N1 3.486(2) . 2_666 no
Pd1 C5 4.177(4) . 2_566 no
Pd1 C6 4.095(3) . 2_566 no
Pd1 C10 3.777(3) . 2_666 no
Pd1 C8 4.046(3) . 2_666 no
Pd1 C9 3.501(3) . 2_666 no
Pd1 C12 3.804(3) . 2_566 no
Pd1 C13 4.150(3) . 2_566 no
Pd1 H16A 3.5049 . 1_554 no
Br1 O3 3.144(3) . . no
Br1 N2 3.286(2) . . no
Br1 C3 3.744(3) . 1_545 no
Br1 C11 3.601(4) . . no
Br1 C14 3.540(3) . . no
Br1 C7 3.595(3) . 2_666 no
Br1 H11B 3.1069 . . no
Br1 H14A 3.1572 . . no
Br1 H3A 2.9804 . 1_545 no
Br1 H15B 3.0388 . 2_556 no
O2 C8 3.222(5) . 2_665 no
O2 C12 3.298(5) . 2_666 no
O3 Pd1 3.945(2) . 2_666 no
O3 Br1 3.144(3) . . no
O3 N1 2.840(3) . . no
O3 Pd1 3.588(3) . . no
O3 C1 3.411(4) . 2_666 no
O4 C16 3.405(4) . 2_567 no
O4 Pd1 3.542(2) . 2_566 no
O2 H11C 2.4439 . . no
O2 H8A 2.7632 . . no
O2 H11A 2.9081 . . no
O2 H8A 2.2817 . 2_665 no
N1 O3 2.840(3) . . no
N1 C1 2.607(4) . . no
N1 C2 2.420(4) . . no
N1 Pd1 3.486(2) . 2_666 no
N2 Br1 3.286(2) . . no
N2 C1 2.550(3) . . no
N2 C6 2.387(4) . . no
N2 C6 3.359(4) . 2_566 no
C1 N1 2.607(4) . . no
C1 N2 2.550(3) . . no
C1 C7 2.316(4) . . no
C1 C12 2.324(4) . . no
C1 O3 3.411(4) . 2_666 no
C1 C13 3.496(4) . 2_566 no
C2 C13 3.495(4) . 2_566 no
C3 Br1 3.744(3) . 1_565 no
C5 C14 3.522(4) . 2_566 no
C5 Pd1 4.177(4) . 2_566 no
C6 C14 3.533(4) . 2_566 no
C6 Pd1 4.095(3) . 2_566 no
C6 N2 3.359(4) . 2_566 no
C7 Br1 3.595(3) . 2_666 no
C7 Pd1 3.993(3) . 2_666 no
C8 Pd1 4.046(3) . 2_666 no
C8 O2 3.222(5) . 2_665 no
C9 Pd1 3.501(3) . 2_666 no
C10 C12 3.546(4) . 2_666 no
C10 Pd1 3.777(3) . 2_666 no
C10 C15 3.571(5) . 1_554 no
C11 Br1 3.601(4) . . no
C12 C12 3.530(4) . 2_566 no
C12 Pd1 3.804(3) . 2_566 no
C12 C10 3.546(4) . 2_666 no
C12 O2 3.298(5) . 2_666 no
C13 C2 3.495(4) . 2_566 no
C13 Pd1 4.150(3) . 2_566 no
C13 C1 3.496(4) . 2_566 no
C14 C6 3.533(4) . 2_566 no
C14 C5 3.522(4) . 2_566 no
C15 C10 3.571(5) . 1_556 no
C16 O4 3.405(4) . 2_567 no
C3 H15B 2.8854 . 2_566 no
C5 H11A 3.0757 . 1_566 no
C5 H11C 2.9590 . 2_666 no
C6 H11C 3.0211 . 2_666 no
C10 H15A 2.8648 . 1_554 no
C14 H15B 2.8950 . . no
C14 H15A 2.8503 . . no
C15 H14A 2.8437 . . no
H3A Br1 2.9804 . 1_565 no
H5A H11A 2.3909 . 1_566 no
H8A O2 2.7632 . . no
H8A O2 2.2817 . 2_665 no
H11A O2 2.9081 . . no
H11A C5 3.0757 . 1_544 no
H11A H5A 2.3909 . 1_544 no
H11B Br1 3.1069 . . no
H11C O2 2.4439 . . no
H11C C5 2.9590 . 2_666 no
H11C C6 3.0211 . 2_666 no
H14A Br1 3.1572 . . no
H14A C15 2.8437 . . no
H15A C10 2.8648 . 1_556 no
H15A C14 2.8503 . . no
H15B C14 2.8950 . . no
H15B Br1 3.0388 . 2_556 no
H15B C3 2.8854 . 2_566 no
H16A Pd1 3.5049 . 1_556 no
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
_geom_hbond_publ_flag
C8 H8A O2 0.9500 2.2800 3.222(5) 171.00 2_665 yes
_vrf_PLAT029_e121
;
PROBLEM: diffrn_measured_fraction_theta_full Low ....... 0.92
RESPONSE:There is a missing cusp of data due to data collection by rotation
around the spindle axis only.
;
#===END
# Attachment '- 7a.cif'
# CIF-file generated for Luo Luo02013
#==============================================================================
data_e029a
_database_code_depnum_ccdc_archive 'CCDC 817027'
#TrackingRef '- 7a.cif'
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
; ?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C16 H15 Br N2 O4 Pt'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural ?
_chemical_formula_sum 'C16 H15 Br N2 O4 Pt'
_chemical_formula_iupac ?
_chemical_formula_weight 574.28
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pt Pt -1.7033 8.3905 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_Int_Tables_number 15
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,1/2-z
-x,-y,-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a 33.697(4)
_cell_length_b 5.2354(4)
_cell_length_c 19.994(2)
_cell_angle_alpha 90
_cell_angle_beta 96.702(14)
_cell_angle_gamma 90
_cell_volume 3503.2(6)
_cell_formula_units_Z 8
_cell_measurement_temperature 173
_cell_measurement_reflns_used 6831
_cell_measurement_theta_min 2.26
_cell_measurement_theta_max 25.87
_cell_special_details
;
Cell parameters were determined by indexing 6831 reflections with
I/sigma limit 6.0.
;
_exptl_crystal_description rod
_exptl_crystal_colour 'light yellow'
_exptl_crystal_size_max 0.480
_exptl_crystal_size_mid 0.120
_exptl_crystal_size_min 0.020
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.178
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 2160
_exptl_absorpt_coefficient_mu 10.313
_exptl_crystal_density_meas_temp ?
# Permitted for
# analytical 'analytical from crystal shape'
# Example: de Meulenaer&Tompa: ABST
# cylinder 'cylindrical'
# gaussian 'Gaussian from crystal shape'
# Example: PLATON/ABSG
# integration 'integration from crystal shape'
# multi-scan 'symmetry-related measurements'
# Example: SADABS, MULABS
# none 'no absorption corr. applied'
# numerical 'numerical from crystal shape'
# psi-scan 'psi-scan corrections'
# Example: PLATON/ABSP
# refdelf 'refined from delta-F'
# Example: SHELXA, DIFABS, DELABS
# sphere 'spherical'
# Example: PLATON/ABSS
_exptl_absorpt_correction_type numerical
# Example: '(North, Phillips & Mathews, 1968)'
_exptl_absorpt_process_details
'analytical from crystal shape (X-SHAPE, X-RED. STOE, 1996)'
_exptl_absorpt_correction_T_min 0.1554
_exptl_absorpt_correction_T_max 0.2564
loop_
_exptl_crystal_face_index_h_
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 -1 1 0.0921
-9 1 15 0.1250
15 1 -1 0.0715
-15 0 -1 0.0894
1 0 -8 0.1170
10 -11 15 0.1011
-10 3 3 0.1048
4 -3 -10 0.1118
5 7 -15 0.1196
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
Data were collected applying an imaging plate system (STOE) with the
following measurement parameters:
Detector distance [mm] 70
Phi movement mode Oscillation
Phi incr. [degrees] 1.0
Number of exposures 277
Irradiation / exposure [min] 6.00
For a detailed description of the method see: Sheldrick, G.M., Paulus, E.
Vertesy, L. & Hahn, F. (1995) Acta Cryst. B51, 89-98.
;
_diffrn_ambient_temperature 173(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'STOE-IPDS diffractometer'
_diffrn_measurement_method rotation
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
# number of measured reflections (redundant set)
_diffrn_reflns_number 6524
_diffrn_reflns_av_R_equivalents 0.0834
_diffrn_reflns_av_sigmaI/netI 0.0497
_diffrn_reflns_limit_h_min -40
_diffrn_reflns_limit_h_max 40
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 2.26
_diffrn_reflns_theta_max 25.87
_diffrn_reflns_theta_full 25.87
_diffrn_measured_fraction_theta_max 0.495
_diffrn_measured_fraction_theta_full 0.495
_diffrn_reflns_reduction_process
; ?
;
# number of unique reflections
_reflns_number_total 1688
# number of observed reflections (> n sig(I))
_reflns_number_gt 1450
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'STOE (1998)'
_computing_cell_refinement 'STOE (1998)'
_computing_data_reduction 'STOE (1998)'
_computing_structure_solution 'SIR-97 (Altomare, 1993)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 1990)'
#===============================================================================
# 8. REFINEMENT DATA
_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. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1035P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
# Permitted for _refine_ls_hydrogen_treatment :
# refall - refined all H parameters
# refxyz - refined H coordinates only
# refU - refined H U only
# noref - no refinement of H parameters
# constr - H parameters constrained
# mixed - some constrained, some independent
# undef - H-atom parameters not defined
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack .
_refine_ls_number_reflns 1688
_refine_ls_number_parameters 217
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0513
_refine_ls_R_factor_gt 0.0461
_refine_ls_wR_factor_ref 0.1272
_refine_ls_wR_factor_gt 0.1225
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_restrained_S_all 1.021
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 1.792
_refine_diff_density_min -1.567
_refine_diff_density_rms 0.204
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Pt1 Pt Uani 0.14236(1) 0.94609(8) 0.50458(2) 1.000 0.0320(2) . .
Br1 Br Uani 0.20858(5) 0.9491(3) 0.57516(8) 1.000 0.0533(5) . .
O1 O Uani 0.1222(3) 0.4111(16) 0.3566(4) 1.000 0.039(3) . .
O2 O Uani 0.1721(2) 0.1449(18) 0.3350(3) 1.000 0.044(3) . .
O3 O Uani 0.0610(3) 1.4671(16) 0.5544(4) 1.000 0.040(3) . .
O4 O Uani 0.0789(3) 1.7442(17) 0.6404(3) 1.000 0.043(3) . .
N1 N Uani 0.1490(3) 0.6537(18) 0.4404(4) 1.000 0.032(3) . .
N2 N Uani 0.1161(3) 1.239(2) 0.5487(4) 1.000 0.037(3) . .
C1 C Uani 0.0888(4) 0.937(2) 0.4526(6) 1.000 0.033(4) . .
C2 C Uani 0.0602(4) 1.110(2) 0.4680(5) 1.000 0.035(3) . .
C3 C Uani 0.0223(4) 1.103(2) 0.4320(5) 1.000 0.040(4) . .
C4 C Uani 0.0130(4) 0.919(2) 0.3840(6) 1.000 0.042(4) . .
C5 C Uani 0.0428(3) 0.742(3) 0.3691(5) 1.000 0.042(3) . .
C6 C Uani 0.0802(3) 0.751(3) 0.4026(4) 1.000 0.036(3) . .
C7 C Uani 0.1171(4) 0.604(3) 0.3998(6) 1.000 0.043(4) . .
C8 C Uani 0.1793(4) 0.488(2) 0.4253(5) 1.000 0.037(4) . .
C9 C Uani 0.1622(3) 0.330(2) 0.3732(5) 1.000 0.035(3) . .
C10 C Uani 0.2131(4) 0.067(3) 0.3489(7) 1.000 0.048(5) . .
C11 C Uani 0.2204(4) -0.123(3) 0.2927(5) 1.000 0.049(4) . .
C12 C Uani 0.0788(3) 1.273(2) 0.5237(4) 1.000 0.035(3) . .
C13 C Uani 0.1244(5) 1.423(2) 0.6002(6) 1.000 0.042(4) . .
C14 C Uani 0.0908(4) 1.552(2) 0.6025(6) 1.000 0.039(4) . .
C15 C Uani 0.1112(4) 1.841(3) 0.6914(5) 1.000 0.048(4) . .
C16 C Uani 0.0922(5) 2.030(3) 0.7319(6) 1.000 0.045(5) . .
H3A H Uiso 0.00280 1.22640 0.44080 1.000 0.0480 calc R
H4A H Uiso -0.01320 0.90920 0.36080 1.000 0.0510 calc R
H5A H Uiso 0.03640 0.61580 0.33540 1.000 0.0500 calc R
H8 H Uiso 0.20610 0.48310 0.44630 1.000 0.0450 calc R
H10A H Uiso 0.21790 -0.01580 0.39360 1.000 0.0580 calc R
H10B H Uiso 0.23110 0.21620 0.34830 1.000 0.0580 calc R
H11A H Uiso 0.20220 -0.26910 0.29390 1.000 0.0580 calc R
H11B H Uiso 0.21540 -0.03840 0.24890 1.000 0.0580 calc R
H11C H Uiso 0.24810 -0.18360 0.29980 1.000 0.0580 calc R
H13 H Uiso 0.14900 1.44780 0.62760 1.000 0.0500 calc R
H15A H Uiso 0.12280 1.69940 0.72010 1.000 0.0580 calc R
H15B H Uiso 0.13270 1.92160 0.66900 1.000 0.0580 calc R
H16A H Uiso 0.08110 2.16930 0.70280 1.000 0.0550 calc R
H16B H Uiso 0.07070 1.94770 0.75310 1.000 0.0550 calc R
H16C H Uiso 0.11210 2.09860 0.76690 1.000 0.0550 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
Pt1 0.0337(3) 0.0342(4) 0.0283(3) 0.0007(1) 0.0048(2) 0.0011(2)
Br1 0.0410(8) 0.0634(11) 0.0531(8) -0.0087(6) -0.0049(6) 0.0036(6)
O1 0.043(5) 0.050(6) 0.021(3) -0.003(3) -0.003(3) 0.016(4)
O2 0.038(4) 0.052(5) 0.039(4) -0.015(4) -0.002(3) 0.002(4)
O3 0.039(5) 0.040(5) 0.044(4) 0.001(3) 0.012(4) 0.004(4)
O4 0.050(5) 0.046(5) 0.035(4) 0.002(4) 0.010(3) 0.008(4)
N1 0.039(5) 0.031(5) 0.027(4) 0.002(3) 0.011(3) 0.002(4)
N2 0.045(5) 0.035(6) 0.030(4) 0.007(4) 0.003(3) -0.004(5)
C1 0.020(5) 0.040(8) 0.038(7) 0.007(5) 0.002(5) -0.003(4)
C2 0.041(6) 0.041(6) 0.025(4) 0.007(4) 0.011(4) -0.006(5)
C3 0.033(6) 0.049(8) 0.039(6) 0.003(5) 0.003(4) 0.010(5)
C4 0.041(7) 0.040(8) 0.046(6) 0.011(5) 0.008(5) 0.002(5)
C5 0.045(6) 0.044(7) 0.036(5) -0.002(5) 0.006(4) -0.001(6)
C6 0.040(6) 0.045(7) 0.022(4) -0.002(5) -0.003(4) 0.008(5)
C7 0.038(7) 0.052(8) 0.039(6) 0.004(5) 0.010(5) -0.004(6)
C8 0.043(7) 0.047(7) 0.023(5) 0.000(4) 0.012(4) 0.002(5)
C9 0.035(5) 0.030(6) 0.039(5) -0.001(4) 0.004(4) 0.003(5)
C10 0.029(6) 0.064(11) 0.051(7) -0.016(6) 0.003(5) 0.006(6)
C11 0.054(7) 0.050(8) 0.043(6) -0.014(6) 0.010(5) 0.002(7)
C12 0.036(5) 0.039(6) 0.030(4) 0.002(4) 0.009(4) 0.001(5)
C13 0.055(8) 0.041(8) 0.030(5) -0.009(4) 0.010(5) -0.003(6)
C14 0.049(8) 0.036(7) 0.033(6) -0.002(4) 0.013(5) -0.006(5)
C15 0.073(9) 0.049(8) 0.023(5) -0.003(5) 0.008(5) 0.005(7)
C16 0.051(9) 0.062(9) 0.022(6) -0.004(5) 0.000(6) 0.013(7)
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All su's are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 Br1 2.4973(17) . . yes
Pt1 N1 2.027(9) . . yes
Pt1 N2 2.024(10) . . yes
Pt1 C1 1.975(13) . . yes
O1 C7 1.353(16) . . yes
O1 C9 1.415(14) . . yes
O2 C9 1.301(13) . . yes
O2 C10 1.436(15) . . yes
O3 C12 1.362(13) . . yes
O3 C14 1.380(15) . . yes
O4 C14 1.349(14) . . yes
O4 C15 1.491(15) . . yes
N1 C7 1.296(16) . . yes
N1 C8 1.399(16) . . yes
N2 C12 1.310(14) . . yes
N2 C13 1.414(15) . . yes
C1 C2 1.383(17) . . no
C1 C6 1.401(17) . . no
C2 C3 1.391(18) . . no
C2 C12 1.483(14) . . no
C3 C4 1.370(15) . . no
C4 C5 1.423(18) . . no
C5 C6 1.357(14) . . no
C6 C7 1.469(19) . . no
C8 C9 1.401(15) . . no
C10 C11 1.54(2) . . no
C13 C14 1.32(2) . . no
C15 C16 1.47(2) . . no
C3 H3A 0.9500 . . no
C4 H4A 0.9500 . . no
C5 H5A 0.9500 . . no
C8 H8 0.9500 . . no
C10 H10A 0.9900 . . no
C10 H10B 0.9900 . . no
C11 H11A 0.9800 . . no
C11 H11B 0.9800 . . no
C11 H11C 0.9800 . . no
C13 H13 0.9500 . . no
C15 H15A 0.9900 . . no
C15 H15B 0.9900 . . no
C16 H16A 0.9800 . . no
C16 H16B 0.9800 . . no
C16 H16C 0.9800 . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pt1 N1 101.8(3) . . . yes
Br1 Pt1 N2 99.0(3) . . . yes
Br1 Pt1 C1 177.2(4) . . . yes
N1 Pt1 N2 159.2(4) . . . yes
N1 Pt1 C1 79.1(4) . . . yes
N2 Pt1 C1 80.1(4) . . . yes
C7 O1 C9 105.2(9) . . . yes
C9 O2 C10 113.9(9) . . . yes
C12 O3 C14 103.4(9) . . . yes
C14 O4 C15 113.4(10) . . . yes
Pt1 N1 C7 113.8(9) . . . yes
Pt1 N1 C8 137.9(8) . . . yes
C7 N1 C8 108.3(10) . . . yes
Pt1 N2 C12 112.7(7) . . . yes
Pt1 N2 C13 140.8(9) . . . yes
C12 N2 C13 106.6(10) . . . yes
Pt1 C1 C2 119.0(8) . . . yes
Pt1 C1 C6 119.5(9) . . . yes
C2 C1 C6 121.5(11) . . . no
C1 C2 C3 119.3(10) . . . no
C1 C2 C12 107.4(11) . . . no
C3 C2 C12 133.3(10) . . . no
C2 C3 C4 120.1(11) . . . no
C3 C4 C5 119.7(12) . . . no
C4 C5 C6 120.8(12) . . . no
C1 C6 C5 118.6(12) . . . no
C1 C6 C7 106.6(10) . . . no
C5 C6 C7 134.8(12) . . . no
O1 C7 N1 113.1(12) . . . yes
O1 C7 C6 125.9(11) . . . yes
N1 C7 C6 121.0(12) . . . yes
N1 C8 C9 106.2(10) . . . yes
O1 C9 O2 112.8(8) . . . yes
O1 C9 C8 107.2(9) . . . yes
O2 C9 C8 139.9(10) . . . yes
O2 C10 C11 105.9(10) . . . yes
O3 C12 N2 112.5(9) . . . yes
O3 C12 C2 126.7(10) . . . yes
N2 C12 C2 120.8(10) . . . yes
N2 C13 C14 106.0(12) . . . yes
O3 C14 O4 113.1(11) . . . yes
O3 C14 C13 111.5(10) . . . yes
O4 C14 C13 135.4(12) . . . yes
O4 C15 C16 106.0(11) . . . yes
C2 C3 H3A 120.00 . . . no
C4 C3 H3A 120.00 . . . no
C3 C4 H4A 120.00 . . . no
C5 C4 H4A 120.00 . . . no
C4 C5 H5A 120.00 . . . no
C6 C5 H5A 120.00 . . . no
N1 C8 H8 127.00 . . . no
C9 C8 H8 127.00 . . . no
O2 C10 H10A 111.00 . . . no
O2 C10 H10B 111.00 . . . no
C11 C10 H10A 111.00 . . . no
C11 C10 H10B 110.00 . . . no
H10A C10 H10B 109.00 . . . no
C10 C11 H11A 109.00 . . . no
C10 C11 H11B 110.00 . . . no
C10 C11 H11C 109.00 . . . no
H11A C11 H11B 109.00 . . . no
H11A C11 H11C 109.00 . . . no
H11B C11 H11C 110.00 . . . no
N2 C13 H13 127.00 . . . no
C14 C13 H13 127.00 . . . no
O4 C15 H15A 110.00 . . . no
O4 C15 H15B 110.00 . . . no
C16 C15 H15A 111.00 . . . no
C16 C15 H15B 111.00 . . . no
H15A C15 H15B 109.00 . . . no
C15 C16 H16A 110.00 . . . no
C15 C16 H16B 109.00 . . . no
C15 C16 H16C 110.00 . . . no
H16A C16 H16B 109.00 . . . no
H16A C16 H16C 109.00 . . . no
H16B C16 H16C 109.00 . . . no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 Pt1 N1 C7 176.6(8) . . . . no
N2 Pt1 N1 C7 -2.9(16) . . . . no
C1 Pt1 N1 C7 -0.7(9) . . . . no
Br1 Pt1 N1 C8 -5.6(11) . . . . no
N2 Pt1 N1 C8 174.9(10) . . . . no
C1 Pt1 N1 C8 177.1(11) . . . . no
Br1 Pt1 N2 C12 -176.1(7) . . . . no
N1 Pt1 N2 C12 3.4(15) . . . . no
C1 Pt1 N2 C12 1.2(8) . . . . no
Br1 Pt1 N2 C13 2.1(13) . . . . no
N1 Pt1 N2 C13 -178.5(11) . . . . no
C1 Pt1 N2 C13 179.4(13) . . . . no
N1 Pt1 C1 C2 179.8(10) . . . . no
N2 Pt1 C1 C2 -1.0(9) . . . . no
N1 Pt1 C1 C6 1.8(9) . . . . no
N2 Pt1 C1 C6 -179.0(10) . . . . no
C9 O1 C7 N1 0.7(14) . . . . no
C7 O1 C9 O2 -179.1(10) . . . . no
C7 O1 C9 C8 -1.7(12) . . . . no
C9 O1 C7 C6 -179.9(12) . . . . no
C10 O2 C9 O1 177.4(9) . . . . no
C10 O2 C9 C8 1.2(19) . . . . no
C9 O2 C10 C11 -172.1(10) . . . . no
C14 O3 C12 N2 -0.8(11) . . . . no
C12 O3 C14 C13 1.3(12) . . . . no
C12 O3 C14 O4 -178.6(9) . . . . no
C14 O3 C12 C2 179.3(10) . . . . no
C14 O4 C15 C16 -174.7(10) . . . . no
C15 O4 C14 O3 -178.7(9) . . . . no
C15 O4 C14 C13 1.5(19) . . . . no
C7 N1 C8 C9 -1.6(12) . . . . no
C8 N1 C7 O1 0.6(14) . . . . no
Pt1 N1 C7 O1 179.0(8) . . . . no
Pt1 N1 C8 C9 -179.5(8) . . . . no
Pt1 N1 C7 C6 -0.5(15) . . . . no
C8 N1 C7 C6 -178.9(11) . . . . no
C12 N2 C13 C14 0.8(13) . . . . no
C13 N2 C12 O3 0.0(12) . . . . no
Pt1 N2 C12 C2 -1.3(12) . . . . no
Pt1 N2 C12 O3 178.8(6) . . . . no
Pt1 N2 C13 C14 -177.5(9) . . . . no
C13 N2 C12 C2 180.0(9) . . . . no
Pt1 C1 C6 C7 -2.4(13) . . . . no
Pt1 C1 C2 C3 -179.4(8) . . . . no
C2 C1 C6 C7 179.8(11) . . . . no
Pt1 C1 C2 C12 0.7(12) . . . . no
C2 C1 C6 C5 -0.2(18) . . . . no
C6 C1 C2 C12 178.6(10) . . . . no
Pt1 C1 C6 C5 177.7(9) . . . . no
C6 C1 C2 C3 -1.5(17) . . . . no
C3 C2 C12 N2 -179.5(11) . . . . no
C3 C2 C12 O3 0.4(19) . . . . no
C1 C2 C3 C4 3.0(16) . . . . no
C12 C2 C3 C4 -177.1(11) . . . . no
C1 C2 C12 O3 -179.6(10) . . . . no
C1 C2 C12 N2 0.5(14) . . . . no
C2 C3 C4 C5 -2.7(17) . . . . no
C3 C4 C5 C6 1.0(18) . . . . no
C4 C5 C6 C1 0.5(18) . . . . no
C4 C5 C6 C7 -179.5(13) . . . . no
C5 C6 C7 N1 -178.2(13) . . . . no
C5 C6 C7 O1 2(2) . . . . no
C1 C6 C7 O1 -177.6(12) . . . . no
C1 C6 C7 N1 1.8(17) . . . . no
N1 C8 C9 O1 2.0(11) . . . . no
N1 C8 C9 O2 178.4(13) . . . . no
N2 C13 C14 O4 178.5(13) . . . . no
N2 C13 C14 O3 -1.3(13) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Pt1 C8 3.546(11) . 1_565 no
Pt1 C9 3.435(10) . 1_565 no
Pt1 C13 3.434(11) . 1_545 no
Pt1 C14 3.450(12) . 1_545 no
Br1 N1 3.524(9) . . no
Br1 N2 3.451(10) . . no
Br1 H8 2.9800 . 7_566 no
Br1 H10B 2.9700 . 7_566 no
Br1 H11C 3.0800 . 7_556 no
O1 C1 3.408(14) . 1_545 no
O2 C15 3.329(13) . 4_574 no
O2 C16 3.323(17) . 4_574 no
O3 C1 3.394(14) . 1_565 no
O1 H15A 2.7900 . 4_574 no
O2 H15A 2.7900 . 4_574 no
O2 H16C 2.6300 . 4_574 no
O3 H3A 2.6900 . 3_586 no
O4 H4A 2.8600 . 3_586 no
N1 Br1 3.524(9) . . no
N1 C1 2.548(16) . . no
N1 C6 2.408(14) . . no
N2 Br1 3.451(10) . . no
N2 C1 2.574(15) . . no
N2 C2 2.429(15) . . no
N2 H15B 2.9200 . 1_545 no
C1 O1 3.408(14) . 1_565 no
C1 O3 3.394(14) . 1_545 no
C1 N1 2.548(16) . . no
C1 N2 2.574(15) . . no
C1 C7 2.302(19) . . no
C1 C12 2.311(15) . . no
C2 C7 3.583(19) . 1_565 no
C3 C3 3.431(16) . 3_576 no
C5 C16 3.576(18) . 4_584 no
C6 C12 3.486(16) . 1_545 no
C7 C12 3.399(16) . 1_545 no
C7 C2 3.583(19) . 1_545 no
C8 Pt1 3.546(11) . 1_545 no
C9 Pt1 3.435(10) . 1_545 no
C12 C7 3.399(16) . 1_565 no
C12 C6 3.486(16) . 1_565 no
C13 Pt1 3.434(11) . 1_565 no
C14 Pt1 3.450(12) . 1_565 no
C15 O2 3.329(13) . 4_575 no
C16 O2 3.323(17) . 4_575 no
C16 C5 3.576(18) . 4_585 no
C5 H16B 3.0700 . 4_584 no
C7 H16C 3.0700 . 4_584 no
C8 H10A 3.0100 . 1_565 no
C8 H11A 3.1000 . 1_565 no
C8 H10B 2.8400 . . no
C8 H10A 3.0400 . . no
C9 H11A 3.0400 . 1_565 no
C10 H8 2.9500 . . no
C13 H15B 2.9600 . 1_545 no
C13 H15B 2.9500 . . no
C13 H15A 2.8100 . . no
C13 H16A 2.9700 . 1_545 no
C14 H16A 2.8800 . 1_545 no
C15 H13 2.8000 . . no
C16 H4A 3.0800 . 3_586 no
H3A O3 2.6900 . 3_586 no
H4A O4 2.8600 . 3_586 no
H4A C16 3.0800 . 3_586 no
H4A H16A 2.5200 . 3_586 no
H8 C10 2.9500 . . no
H8 Br1 2.9800 . 7_566 no
H10A C8 3.0100 . 1_545 no
H10A C8 3.0400 . . no
H10B C8 2.8400 . . no
H10B Br1 2.9700 . 7_566 no
H11A C8 3.1000 . 1_545 no
H11A C9 3.0400 . 1_545 no
H11B H11C 2.4900 . 6_555 no
H11C H11B 2.4900 . 6_545 no
H11C Br1 3.0800 . 7_556 no
H13 C15 2.8000 . . no
H13 H15A 2.5100 . . no
H15A C13 2.8100 . . no
H15A H13 2.5100 . . no
H15A O1 2.7900 . 4_575 no
H15A O2 2.7900 . 4_575 no
H15B N2 2.9200 . 1_565 no
H15B C13 2.9500 . . no
H15B C13 2.9600 . 1_565 no
H16A C13 2.9700 . 1_565 no
H16A C14 2.8800 . 1_565 no
H16A H4A 2.5200 . 3_586 no
H16B C5 3.0700 . 4_585 no
H16C O2 2.6300 . 4_575 no
H16C C7 3.0700 . 4_585 no
_vrf_REFLT03_e029a
;
PROBLEM: Reflection count < 85% complete
RESPONSE: all examined crystals were twinned, therefore
only the unaffected reflections of the major twin component
were used for structure solution and structure refinement.
;
_vrf_PLAT029_e029a
;
PROBLEM: diffrn_measured_fraction_theta_full Low ....... 0.50
RESPONSE: all examined crystals were twinned, therefore
only the unaffected reflections of the major twin component
were used for structure solution and structure refinement.
;
_vrf_PLAT088_e029a
;
PROBLEM: Poor Data / Parameter Ratio ..... 7.78
RESPONSE: all examined crystals were twinned, therefore
only the unaffected reflections of the major twin component
were used for structure solution and structure refinement.
;
#===END
# Attachment '- 7c.cif'
# CIF-file generated for Luo 0422 Luo/Reiser
#==============================================================================
data_e117
_database_code_depnum_ccdc_archive 'CCDC 817028'
#TrackingRef '- 7c.cif'
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
; ?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C16 H13 Br N2 O5 Pt'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural 'C16 H13 Br N2 O5 Pt'
_chemical_formula_sum 'C16 H13 Br N2 O5 Pt'
_chemical_formula_iupac ?
_chemical_formula_weight 588.26
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pt Pt -1.7033 8.3905 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
_cell_length_a 9.6961(10)
_cell_length_b 10.0725(10)
_cell_length_c 10.4364(10)
_cell_angle_alpha 107.818(11)
_cell_angle_beta 111.729(11)
_cell_angle_gamma 99.999(12)
_cell_volume 852.7(2)
_cell_formula_units_Z 2
_cell_measurement_temperature 173
_cell_measurement_reflns_used 8000
_cell_measurement_theta_min 2.85
_cell_measurement_theta_max 26.85
_cell_special_details
;
Cell parameters were determined by indexing 8000 reflections with
I/sigma limit 6.0.
;
_exptl_crystal_description prism
_exptl_crystal_colour 'yellow to orange'
_exptl_crystal_size_max 0.49
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.12
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.291
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 552
_exptl_absorpt_coefficient_mu 10.600
_exptl_crystal_density_meas_temp ?
# Permitted for :
# analytical 'analytical from crystal shape'
# Example: de Meulenaer&Tompa: ABST
# cylinder 'cylindrical'
# gaussian 'Gaussian from crystal shape'
# Example: PLATON/ABSG
# integration 'integration from crystal shape'
# multi-scan 'symmetry-related measurements'
# Example: SADABS, MULABS
# none 'no absorption corr. applied'
# numerical 'numerical from crystal shape'
# psi-scan 'psi-scan corrections'
# Example: PLATON/ABSP
# refdelf 'refined from delta-F'
# Example: SHELXA, DIFABS, DELABS
# sphere 'spherical'
# Example: PLATON/ABSS
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
'numerical from crystal shape (X-SHAPE, X-RED. STOE, 1996)'
_exptl_absorpt_correction_T_min 0.0539
_exptl_absorpt_correction_T_max 0.3258
loop_
_exptl_crystal_face_index_h_
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.1034
0 0 -1 0.1090
1 0 0 0.2176
0 1 0 0.0544
0 -1 0 0.0739
-1 0 0 0.2777
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
Data were collected applying an imaging plate system (STOE) with the
following measurement parameters:
Detector distance [mm] 65
Phi movement mode Oscillation
Phi incr. [degrees] 1.2
Number of exposures 240
Irradiation / exposure [min] 1.00
For a detailed description of the method see: Sheldrick, G.M., Paulus, E.
Vertesy, L. & Hahn, F. (1995) Acta Cryst. B51, 89-98.
;
_diffrn_ambient_temperature 173(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'STOE-IPDS diffractometer'
_diffrn_measurement_method rotation
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
# number of measured reflections (redundant set)
_diffrn_reflns_number 10760
_diffrn_reflns_av_R_equivalents 0.0339
_diffrn_reflns_av_sigmaI/netI 0.0270
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 2.25
_diffrn_reflns_theta_max 26.85
_diffrn_reflns_theta_full 26.85
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measured_fraction_theta_full 0.932
_diffrn_reflns_reduction_process
; ?
;
# number of unique reflections
_reflns_number_total 3422
# number of observed reflections (> n sig(I))
_reflns_number_gt 3092
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'STOE (1998)'
_computing_cell_refinement 'STOE (1998)'
_computing_data_reduction 'STOE (1998)'
_computing_structure_solution 'SIR-97 (Altomare, 1993)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 2003)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
Refinement on F^2 for ALL reflections except those
flagged by the user for potential systematic errors.
Weighted R-factors wR and all goodnesses 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
observed criterion of F^2 > 2sigma(F^2) is used only
for calculating -R-factor-obs etc. and is not
relevant to the choice of reflections for refinement.
R-factors based on F^2 are statistically about twice
as large as those based on F, and R-factors based on
ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
# Permitted for _refine_ls_hydrogen_treatment :
# refall - refined all H parameters
# refxyz - refined H coordinates only
# refU - refined H U only
# noref - no refinement of H parameters
# constr - H parameters constrained
# mixed - some constrained, some independent
# undef - H-atom parameters not defined
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack .
_refine_ls_number_reflns 3422
_refine_ls_number_parameters 226
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0265
_refine_ls_R_factor_gt 0.0233
_refine_ls_wR_factor_ref 0.0572
_refine_ls_wR_factor_gt 0.0563
_refine_ls_goodness_of_fit_ref 1.029
_refine_ls_restrained_S_all 1.029
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.676
_refine_diff_density_min -1.521
_refine_diff_density_rms 0.231
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Pt1 Pt Uani 0.75876(2) 0.44337(2) -0.04191(2) 1.000 0.0297(1) . .
Br1 Br Uani 0.73364(7) 0.17338(5) -0.12068(6) 1.000 0.0472(2) . .
O1 O Uani 0.9026(5) 0.7339(4) -0.2075(4) 1.000 0.0486(11) . .
O2 O Uani 0.8697(5) 0.2548(4) -0.3215(4) 1.000 0.0523(11) . .
O3 O Uani 0.9790(7) 0.3542(6) -0.4382(6) 1.000 0.0783(19) . .
O4 O Uani 0.6134(4) 0.5522(4) 0.2846(4) 1.000 0.0418(10) . .
O5 O Uani 0.5433(5) 0.3789(4) 0.3651(4) 1.000 0.0526(11) . .
N1 N Uani 0.8442(4) 0.5327(4) -0.1654(4) 1.000 0.0345(10) . .
N2 N Uani 0.6759(4) 0.4354(4) 0.1083(4) 1.000 0.0350(10) . .
C1 C Uani 0.7567(5) 0.6435(5) 0.0366(5) 1.000 0.0348(12) . .
C2 C Uani 0.7017(6) 0.6870(5) 0.1473(5) 1.000 0.0385(12) . .
C3 C Uani 0.6928(7) 0.8268(5) 0.1973(6) 1.000 0.0491(16) . .
C4 C Uani 0.7430(7) 0.9272(6) 0.1405(6) 1.000 0.0533(16) . .
C5 C Uani 0.8011(7) 0.8896(5) 0.0374(6) 1.000 0.0475(16) . .
C6 C Uani 0.8047(5) 0.7461(5) -0.0180(5) 1.000 0.0372(12) . .
C7 C Uani 0.8521(5) 0.6725(5) -0.1287(5) 1.000 0.0372(12) . .
C8 C Uani 0.9334(7) 0.6244(6) -0.2988(6) 1.000 0.0491(17) . .
C9 C Uani 0.9003(6) 0.5010(6) -0.2757(5) 1.000 0.0407(14) . .
C10 C Uani 0.9201(6) 0.3641(6) -0.3531(5) 1.000 0.0445(14) . .
C11 C Uani 0.8818(8) 0.1144(6) -0.3940(7) 1.000 0.0590(19) . .
C12 C Uani 0.6626(5) 0.5606(5) 0.1806(5) 1.000 0.0367(12) . .
C13 C Uani 0.5947(6) 0.4094(5) 0.2711(5) 1.000 0.0417(14) . .
C14 C Uani 0.6347(6) 0.3352(5) 0.1661(5) 1.000 0.0385(14) . .
C15 C Uani 0.5253(7) 0.2298(6) 0.3533(6) 1.000 0.0463(16) . .
C16 C Uani 0.4695(8) 0.2115(7) 0.4664(6) 1.000 0.0570(17) . .
H3 H Uiso 0.65370 0.85590 0.26890 1.000 0.0590 calc R
H4 H Uiso 0.73620 1.02350 0.17490 1.000 0.0640 calc R
H5 H Uiso 0.83810 0.96010 0.00450 1.000 0.0570 calc R
H8 H Uiso 0.97220 0.63460 -0.36780 1.000 0.0590 calc R
H11A H Uiso 0.78750 0.05780 -0.49040 1.000 0.0710 calc R
H11B H Uiso 0.89170 0.06030 -0.32910 1.000 0.0710 calc R
H11C H Uiso 0.97440 0.12910 -0.41210 1.000 0.0710 calc R
H14 H Uiso 0.63470 0.23610 0.13750 1.000 0.0460 calc R
H15A H Uiso 0.62680 0.21110 0.37530 1.000 0.0560 calc R
H15B H Uiso 0.44780 0.15890 0.25000 1.000 0.0560 calc R
H16A H Uiso 0.54760 0.28140 0.56830 1.000 0.0680 calc R
H16B H Uiso 0.45570 0.11070 0.46030 1.000 0.0680 calc R
H16C H Uiso 0.36930 0.23060 0.44390 1.000 0.0680 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
Pt1 0.0337(1) 0.0259(1) 0.0303(1) 0.0122(1) 0.0146(1) 0.0097(1)
Br1 0.0717(3) 0.0301(2) 0.0531(3) 0.0188(2) 0.0383(3) 0.0206(2)
O1 0.058(2) 0.0458(19) 0.056(2) 0.0322(17) 0.0312(18) 0.0150(17)
O2 0.068(2) 0.0437(19) 0.056(2) 0.0179(16) 0.042(2) 0.0155(18)
O3 0.125(4) 0.077(3) 0.083(3) 0.043(3) 0.084(3) 0.044(3)
O4 0.0521(19) 0.0366(16) 0.0403(16) 0.0117(13) 0.0284(15) 0.0127(15)
O5 0.073(2) 0.049(2) 0.0513(19) 0.0216(16) 0.0433(19) 0.0183(19)
N1 0.0354(18) 0.0361(18) 0.0333(17) 0.0168(15) 0.0159(15) 0.0090(16)
N2 0.040(2) 0.0307(17) 0.0371(17) 0.0149(15) 0.0202(16) 0.0094(16)
C1 0.037(2) 0.029(2) 0.037(2) 0.0145(17) 0.0149(18) 0.0095(18)
C2 0.039(2) 0.035(2) 0.042(2) 0.0132(19) 0.0199(19) 0.0142(19)
C3 0.062(3) 0.035(2) 0.051(3) 0.012(2) 0.029(3) 0.019(2)
C4 0.065(3) 0.037(2) 0.058(3) 0.019(2) 0.024(3) 0.026(3)
C5 0.053(3) 0.033(2) 0.056(3) 0.023(2) 0.020(2) 0.014(2)
C6 0.038(2) 0.031(2) 0.043(2) 0.0204(18) 0.0147(19) 0.0102(19)
C7 0.038(2) 0.036(2) 0.039(2) 0.0211(18) 0.0153(18) 0.0089(19)
C8 0.053(3) 0.058(3) 0.050(3) 0.033(2) 0.028(2) 0.018(3)
C9 0.039(2) 0.047(3) 0.035(2) 0.0176(19) 0.0166(19) 0.010(2)
C10 0.042(2) 0.053(3) 0.035(2) 0.018(2) 0.0165(19) 0.009(2)
C11 0.068(4) 0.045(3) 0.058(3) 0.010(2) 0.033(3) 0.014(3)
C12 0.040(2) 0.034(2) 0.035(2) 0.0114(17) 0.0188(18) 0.0102(19)
C13 0.051(3) 0.036(2) 0.041(2) 0.0159(19) 0.024(2) 0.013(2)
C14 0.047(3) 0.037(2) 0.035(2) 0.0161(18) 0.0210(19) 0.013(2)
C15 0.057(3) 0.045(3) 0.041(2) 0.021(2) 0.025(2) 0.013(2)
C16 0.063(3) 0.064(3) 0.053(3) 0.030(3) 0.033(3) 0.014(3)
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All su's are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 Br1 2.5267(6) . . yes
Pt1 N1 2.097(4) . . yes
Pt1 N2 2.024(4) . . yes
Pt1 C1 1.937(5) . . yes
O1 C7 1.343(7) . . yes
O1 C8 1.377(8) . . yes
O2 C10 1.309(8) . . yes
O2 C11 1.433(8) . . yes
O3 C10 1.211(9) . . yes
O4 C12 1.356(6) . . yes
O4 C13 1.374(7) . . yes
O5 C13 1.341(7) . . yes
O5 C15 1.443(8) . . yes
N1 C7 1.321(7) . . yes
N1 C9 1.422(7) . . yes
N2 C12 1.312(7) . . yes
N2 C14 1.398(7) . . yes
C1 C2 1.428(7) . . no
C1 C6 1.414(7) . . no
C2 C3 1.374(8) . . no
C2 C12 1.444(8) . . no
C3 C4 1.422(9) . . no
C4 C5 1.376(9) . . no
C5 C6 1.395(8) . . no
C6 C7 1.443(7) . . no
C8 C9 1.345(9) . . no
C9 C10 1.455(8) . . no
C13 C14 1.351(8) . . no
C15 C16 1.514(9) . . no
C3 H3 0.9499 . . no
C4 H4 0.9491 . . no
C5 H5 0.9502 . . no
C8 H8 0.9503 . . no
C11 H11A 0.9798 . . no
C11 H11B 0.9802 . . no
C11 H11C 0.9799 . . no
C14 H14 0.9503 . . no
C15 H15A 0.9901 . . no
C15 H15B 0.9897 . . no
C16 H16A 0.9800 . . no
C16 H16B 0.9797 . . no
C16 H16C 0.9796 . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pt1 N1 110.67(11) . . . yes
Br1 Pt1 N2 90.86(12) . . . yes
Br1 Pt1 C1 169.95(15) . . . yes
N1 Pt1 N2 158.47(16) . . . yes
N1 Pt1 C1 79.17(19) . . . yes
N2 Pt1 C1 79.30(19) . . . yes
C7 O1 C8 104.9(4) . . . yes
C10 O2 C11 118.3(5) . . . yes
C12 O4 C13 104.2(4) . . . yes
C13 O5 C15 113.4(5) . . . yes
Pt1 N1 C7 111.0(3) . . . yes
Pt1 N1 C9 144.0(4) . . . yes
C7 N1 C9 105.1(4) . . . yes
Pt1 N2 C12 113.8(3) . . . yes
Pt1 N2 C14 138.3(3) . . . yes
C12 N2 C14 107.8(4) . . . yes
Pt1 C1 C2 119.9(4) . . . yes
Pt1 C1 C6 120.6(4) . . . yes
C2 C1 C6 119.5(5) . . . no
C1 C2 C3 119.8(5) . . . no
C1 C2 C12 106.7(5) . . . no
C3 C2 C12 133.5(5) . . . no
C2 C3 C4 119.1(6) . . . no
C3 C4 C5 122.3(6) . . . no
C4 C5 C6 118.8(5) . . . no
C1 C6 C5 120.5(5) . . . no
C1 C6 C7 107.6(4) . . . no
C5 C6 C7 132.0(5) . . . no
O1 C7 N1 113.3(4) . . . yes
O1 C7 C6 125.0(5) . . . yes
N1 C7 C6 121.7(5) . . . yes
O1 C8 C9 109.8(5) . . . yes
N1 C9 C8 106.9(5) . . . yes
N1 C9 C10 128.8(5) . . . yes
C8 C9 C10 124.4(5) . . . no
O2 C10 O3 123.8(6) . . . yes
O2 C10 C9 114.0(5) . . . yes
O3 C10 C9 122.2(6) . . . yes
O4 C12 N2 111.9(5) . . . yes
O4 C12 C2 127.8(5) . . . yes
N2 C12 C2 120.3(5) . . . yes
O4 C13 O5 112.9(5) . . . yes
O4 C13 C14 111.0(5) . . . yes
O5 C13 C14 136.1(5) . . . yes
N2 C14 C13 105.2(5) . . . yes
O5 C15 C16 107.8(5) . . . yes
C2 C3 H3 120.41 . . . no
C4 C3 H3 120.49 . . . no
C3 C4 H4 118.87 . . . no
C5 C4 H4 118.86 . . . no
C4 C5 H5 120.60 . . . no
C6 C5 H5 120.60 . . . no
O1 C8 H8 125.04 . . . no
C9 C8 H8 125.15 . . . no
O2 C11 H11A 109.44 . . . no
O2 C11 H11B 109.48 . . . no
O2 C11 H11C 109.49 . . . no
H11A C11 H11B 109.47 . . . no
H11A C11 H11C 109.46 . . . no
H11B C11 H11C 109.50 . . . no
N2 C14 H14 127.37 . . . no
C13 C14 H14 127.44 . . . no
O5 C15 H15A 110.14 . . . no
O5 C15 H15B 110.18 . . . no
C16 C15 H15A 110.14 . . . no
C16 C15 H15B 110.14 . . . no
H15A C15 H15B 108.47 . . . no
C15 C16 H16A 109.45 . . . no
C15 C16 H16B 109.44 . . . no
C15 C16 H16C 109.49 . . . no
H16A C16 H16B 109.43 . . . no
H16A C16 H16C 109.48 . . . no
H16B C16 H16C 109.54 . . . no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 Pt1 N1 C7 177.7(3) . . . . no
N2 Pt1 N1 C7 -0.5(6) . . . . no
C1 Pt1 N1 C7 -0.2(3) . . . . no
Br1 Pt1 N1 C9 -3.3(6) . . . . no
N2 Pt1 N1 C9 178.5(5) . . . . no
C1 Pt1 N1 C9 178.9(6) . . . . no
Br1 Pt1 N2 C12 -178.1(3) . . . . no
N1 Pt1 N2 C12 0.1(6) . . . . no
C1 Pt1 N2 C12 -0.2(4) . . . . no
Br1 Pt1 N2 C14 6.4(5) . . . . no
N1 Pt1 N2 C14 -175.4(4) . . . . no
C1 Pt1 N2 C14 -175.7(5) . . . . no
N1 Pt1 C1 C2 178.9(4) . . . . no
N2 Pt1 C1 C2 -1.2(4) . . . . no
N1 Pt1 C1 C6 0.8(4) . . . . no
N2 Pt1 C1 C6 -179.3(4) . . . . no
C8 O1 C7 N1 -1.8(6) . . . . no
C8 O1 C7 C6 -179.7(5) . . . . no
C7 O1 C8 C9 0.7(6) . . . . no
C11 O2 C10 C9 179.1(5) . . . . no
C11 O2 C10 O3 -1.3(9) . . . . no
C13 O4 C12 C2 -179.4(5) . . . . no
C12 O4 C13 O5 -179.0(4) . . . . no
C12 O4 C13 C14 1.5(6) . . . . no
C13 O4 C12 N2 -0.7(5) . . . . no
C15 O5 C13 C14 0.1(9) . . . . no
C15 O5 C13 O4 -179.2(5) . . . . no
C13 O5 C15 C16 179.2(5) . . . . no
C9 N1 C7 C6 -179.9(4) . . . . no
C7 N1 C9 C10 178.7(5) . . . . no
C7 N1 C9 C8 -1.6(6) . . . . no
Pt1 N1 C9 C8 179.3(4) . . . . no
Pt1 N1 C7 C6 -0.5(6) . . . . no
Pt1 N1 C7 O1 -178.5(3) . . . . no
Pt1 N1 C9 C10 -0.4(9) . . . . no
C9 N1 C7 O1 2.1(6) . . . . no
C14 N2 C12 C2 178.4(5) . . . . no
Pt1 N2 C12 C2 1.5(6) . . . . no
Pt1 N2 C14 C13 177.0(4) . . . . no
Pt1 N2 C12 O4 -177.3(3) . . . . no
C12 N2 C14 C13 1.3(6) . . . . no
C14 N2 C12 O4 -0.4(6) . . . . no
Pt1 C1 C6 C5 179.2(4) . . . . no
Pt1 C1 C2 C3 -176.7(4) . . . . no
C6 C1 C2 C12 -179.8(4) . . . . no
Pt1 C1 C6 C7 -1.2(6) . . . . no
C2 C1 C6 C7 -179.3(4) . . . . no
Pt1 C1 C2 C12 2.2(6) . . . . no
C2 C1 C6 C5 1.1(8) . . . . no
C6 C1 C2 C3 1.4(8) . . . . no
C12 C2 C3 C4 179.7(6) . . . . no
C1 C2 C12 N2 -2.4(7) . . . . no
C1 C2 C3 C4 -1.8(8) . . . . no
C3 C2 C12 O4 -5.1(10) . . . . no
C3 C2 C12 N2 176.3(6) . . . . no
C1 C2 C12 O4 176.3(5) . . . . no
C2 C3 C4 C5 -0.3(9) . . . . no
C3 C4 C5 C6 2.8(9) . . . . no
C4 C5 C6 C7 177.4(6) . . . . no
C4 C5 C6 C1 -3.1(8) . . . . no
C1 C6 C7 N1 1.1(6) . . . . no
C5 C6 C7 O1 -1.7(9) . . . . no
C1 C6 C7 O1 178.8(5) . . . . no
C5 C6 C7 N1 -179.4(6) . . . . no
O1 C8 C9 C10 -179.7(5) . . . . no
O1 C8 C9 N1 0.6(6) . . . . no
C8 C9 C10 O2 -175.2(5) . . . . no
N1 C9 C10 O3 -175.1(6) . . . . no
N1 C9 C10 O2 4.5(8) . . . . no
C8 C9 C10 O3 5.2(9) . . . . no
O5 C13 C14 N2 179.0(6) . . . . no
O4 C13 C14 N2 -1.8(6) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Pt1 O2 3.595(4) . . no
Pt1 C7 4.074(5) . 2_765 no
Pt1 Pt1 4.2963(5) . 2_765 no
Pt1 O2 3.953(4) . 2_765 no
Pt1 O4 3.577(4) . 2_665 no
Pt1 N1 3.571(4) . 2_765 no
Pt1 C2 4.039(6) . 2_665 no
Pt1 C3 4.136(7) . 2_665 no
Pt1 C10 3.736(5) . 2_765 no
Pt1 C8 4.044(6) . 2_765 no
Pt1 C9 3.512(5) . 2_765 no
Pt1 C12 3.784(5) . 2_665 no
Pt1 C13 4.187(6) . 2_665 no
Pt1 H16A 3.4661 . 1_554 no
Br1 O2 3.087(4) . . no
Br1 N2 3.261(4) . . no
Br1 C5 3.749(6) . 1_545 no
Br1 C11 3.584(7) . . no
Br1 C14 3.496(5) . . no
Br1 C7 3.597(5) . 2_765 no
Br1 H11B 3.1521 . . no
Br1 H14 3.1084 . . no
Br1 H5 2.9734 . 1_545 no
Br1 H15B 3.0905 . 2_655 no
O2 Pt1 3.595(4) . . no
O2 Br1 3.087(4) . . no
O2 N1 2.881(6) . . no
O2 Pt1 3.953(4) . 2_765 no
O3 C12 3.267(8) . 2_765 no
O3 C8 3.214(9) . 2_764 no
O4 C16 3.390(8) . 2_666 no
O4 Pt1 3.577(4) . 2_665 no
O3 H11C 2.3598 . . no
O3 H8 2.2730 . 2_764 no
O3 H8 2.7114 . . no
N1 O2 2.881(6) . . no
N1 C1 2.574(6) . . no
N1 C6 2.415(7) . . no
N1 Pt1 3.571(4) . 2_765 no
N2 Br1 3.261(4) . . no
N2 C1 2.528(7) . . no
N2 C2 2.393(7) . . no
N2 C2 3.351(7) . 2_665 no
C1 N1 2.574(6) . . no
C1 N2 2.528(7) . . no
C1 C7 2.305(7) . . no
C1 C12 2.304(7) . . no
C1 C13 3.525(7) . 2_665 no
C2 Pt1 4.039(6) . 2_665 no
C2 N2 3.351(7) . 2_665 no
C2 C14 3.576(7) . 2_665 no
C3 C14 3.553(7) . 2_665 no
C3 Pt1 4.136(7) . 2_665 no
C5 Br1 3.749(6) . 1_565 no
C6 C13 3.495(7) . 2_665 no
C7 Pt1 4.074(5) . 2_765 no
C7 Br1 3.597(5) . 2_765 no
C8 O3 3.214(9) . 2_764 no
C8 Pt1 4.044(6) . 2_765 no
C9 Pt1 3.512(5) . 2_765 no
C10 C12 3.591(8) . 2_765 no
C10 Pt1 3.736(5) . 2_765 no
C10 C15 3.585(8) . 1_554 no
C11 Br1 3.584(7) . . no
C12 C12 3.562(7) . 2_665 no
C12 O3 3.267(8) . 2_765 no
C12 Pt1 3.784(5) . 2_665 no
C12 C10 3.591(8) . 2_765 no
C13 C1 3.525(7) . 2_665 no
C13 Pt1 4.187(6) . 2_665 no
C13 C6 3.495(7) . 2_665 no
C14 C3 3.553(7) . 2_665 no
C14 C2 3.576(7) . 2_665 no
C15 C10 3.585(8) . 1_556 no
C16 O4 3.390(8) . 2_666 no
C2 H11C 3.0581 . 2_765 no
C3 H11C 3.0285 . 2_765 no
C3 H11A 3.0465 . 1_566 no
C5 H15B 2.8972 . 2_665 no
C10 H15A 2.8867 . 1_554 no
C14 H15B 2.8659 . . no
C14 H15A 2.8453 . . no
C15 H14 2.8345 . . no
H3 H11A 2.3819 . 1_566 no
H4 H14 2.5818 . 1_565 no
H5 Br1 2.9734 . 1_565 no
H8 O3 2.7114 . . no
H8 O3 2.2730 . 2_764 no
H11A C3 3.0465 . 1_544 no
H11A H3 2.3819 . 1_544 no
H11B Br1 3.1521 . . no
H11C O3 2.3598 . . no
H11C C2 3.0582 . 2_765 no
H11C C3 3.0285 . 2_765 no
H14 Br1 3.1084 . . no
H14 C15 2.8345 . . no
H14 H4 2.5818 . 1_545 no
H14 H15A 2.5971 . . no
H15A C10 2.8867 . 1_556 no
H15A C14 2.8453 . . no
H15A H14 2.5971 . . no
H15B C14 2.8659 . . no
H15B Br1 3.0905 . 2_655 no
H15B C5 2.8972 . 2_665 no
H16A Pt1 3.4661 . 1_556 no
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
_geom_hbond_publ_flag
C8 H8 O3 0.9500 2.2700 3.214(9) 170.00 2_764 yes
_vrf_PLAT029_e117
;
PROBLEM: diffrn_measured_fraction_theta_full Low ....... 0.93
RESPONSE:There is a missing cusp of data due to data collection by rotation
around the spindle axis only.
;
#===END