##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
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# Full details of the Crystallographic Information File format #
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# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
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data_I
_audit_creation_method SHELXL-2014
_journal_date_recd_electronic 2015-09-07
_journal_date_accepted 2015-09-18
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2015
_journal_volume 71
_journal_issue 10
_journal_page_first 1259
_journal_page_last 1261
_journal_paper_category GM
_journal_paper_doi 10.1107/S2056989015017478
_journal_coeditor_code WM5214
_publ_contact_author_name 'Tomoaki Sugaya'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry,
School of Advanced Science and Engineering,
Waseda University, Okubo, Shinjuku-ku, Tokyo 169-8555, Japan
;
_publ_contact_author_email 'tom-s@aoni.waseda.jp'
_publ_contact_author_fax '+81-3-5286-3241'
_publ_contact_author_phone '+81-3-5286-3241'
_publ_section_title
;\
Crystal structure of
[5-bromo-2-(pyridin-2-yl-\kN)phenyl-\kC^1^](pentane-2,4-\
dionato-\k^2^O,O')platinum(II)
;
_publ_section_title_footnote .
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Fukuda, Keito' .
;
Department of Chemistry and Biochemistry,
School of Advanced Science and Engineering,
Waseda University, Okubo, Shinjuku-ku, Tokyo 169-8555, Japan
;
'Sugaya, Tomoaki' .
;
Department of Chemistry and Biochemistry,
School of Advanced Science and Engineering,
Waseda University, Okubo, Shinjuku-ku, Tokyo 169-8555, Japan
;
'Ishihara, Koji' .
;
Department of Chemistry and Biochemistry,
School of Advanced Science and Engineering,
Waseda University, Okubo, Shinjuku-ku, Tokyo 169-8555, Japan
;
_publ_section_synopsis
;
In the title complex, [Pt(C~11~H~7~BrN)(C~5~H~7~O~2~)], two crystallographically
non-equivalent dimers stacked by \p--\p interactions are arranged
antiparallel to each other.
;
_chemical_name_systematic
;\
[5-Bromo-2-(pyridin-2-yl-\kN)phenyl-\kC^1^](pentane-2,4-\
dionato-\k^2^O,O')platinum(II)
;
_chemical_name_common ?
_chemical_formula_moiety 'C16 H14 Br N O2 Pt'
_chemical_formula_sum 'C16 H14 Br N O2 Pt'
_chemical_formula_iupac '[Pt (C11 H7 Br N) (C5 H7 O2)]'
_chemical_formula_weight 527.28
_chemical_melting_point ?
_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_name_H-M_alt 'C 2/c'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 17.557(2)
_cell_length_b 17.876(2)
_cell_length_c 19.832(2)
_cell_angle_alpha 90
_cell_angle_beta 91.3970(10)
_cell_angle_gamma 90
_cell_volume 6222.4(13)
_cell_formula_units_Z 16
_cell_measurement_reflns_used 9927
_cell_measurement_theta_min 2.28
_cell_measurement_theta_max 27.27
_cell_measurement_temperature 200(2)
_exptl_crystal_description lath
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.180
_exptl_crystal_size_mid 0.060
_exptl_crystal_size_min 0.020
_exptl_crystal_density_diffrn 2.251
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 3936
_exptl_absorpt_coefficient_mu 11.591
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_shelx_estimated_absorpt_T_min 0.229
_shelx_estimated_absorpt_T_max 0.801
_exptl_absorpt_correction_T_min 0.48
_exptl_absorpt_correction_T_max 0.80
_exptl_special_details
;
;
_diffrn_ambient_temperature 200(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type 'Bruker APEXII CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number 35025
_diffrn_reflns_av_R_equivalents 0.0379
_diffrn_reflns_theta_min 1.626
_diffrn_reflns_theta_max 27.481
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 25
_refine_special_details ?
_reflns_number_total 7103
_reflns_number_gt 6001
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0360
_refine_ls_R_factor_gt 0.0273
_refine_ls_wR_factor_gt 0.0658
_refine_ls_wR_factor_ref 0.0697
_refine_ls_goodness_of_fit_ref 1.009
_refine_ls_restrained_S_all 1.009
_refine_ls_number_reflns 7103
_refine_ls_number_parameters 383
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+16.0306P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 3.662
_refine_diff_density_min -1.195
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Br' 'Br' -0.2901 2.4595
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Pt' 'Pt' -1.7033 8.3905
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and MERCURY (Macrae et al.,
2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.63794(4) 0.11449(4) 0.24876(3) 0.06869(19) Uani d 1 . .
Br Br2 0.13287(5) 0.08166(4) 0.25166(3) 0.06997(19) Uani d 1 . .
C C1 0.6968(3) 0.1984(3) 0.6440(3) 0.0478(12) Uani d 1 . .
H H1 0.7459 0.1928 0.6646 0.057 Uiso calc 1 . .
C C2 0.6367(4) 0.2211(3) 0.6835(3) 0.0614(16) Uani d 1 . .
H H2 0.6441 0.2304 0.7304 0.074 Uiso calc 1 . .
C C3 0.5655(4) 0.2296(3) 0.6522(3) 0.0626(17) Uani d 1 . .
H H3 0.5231 0.2449 0.6777 0.075 Uiso calc 1 . .
C C4 0.5565(3) 0.2159(3) 0.5846(3) 0.0484(13) Uani d 1 . .
H H4 0.5080 0.2221 0.5632 0.058 Uiso calc 1 . .
C C5 0.6187(3) 0.1929(2) 0.5470(3) 0.0368(10) Uani d 1 . .
C C6 0.6190(3) 0.1739(2) 0.4758(3) 0.0355(10) Uani d 1 . .
C C7 0.5543(3) 0.1762(3) 0.4328(3) 0.0467(12) Uani d 1 . .
H H7 0.5065 0.1904 0.4502 0.056 Uiso calc 1 . .
C C8 0.5596(3) 0.1583(3) 0.3660(3) 0.0493(14) Uani d 1 . .
H H8 0.5160 0.1593 0.3367 0.059 Uiso calc 1 . .
C C9 0.6299(3) 0.1388(3) 0.3424(3) 0.0455(12) Uani d 1 . .
C C10 0.6949(3) 0.1351(3) 0.3833(2) 0.0392(11) Uani d 1 . .
H H10 0.7421 0.1207 0.3649 0.047 Uiso calc 1 . .
C C11 0.6905(3) 0.1526(2) 0.4509(2) 0.0342(10) Uani d 1 . .
C C12 0.9693(4) 0.1381(4) 0.6572(3) 0.0652(17) Uani d 1 . .
H H12A 0.9552 0.1822 0.6835 0.098 Uiso calc 1 . .
H H12B 1.0234 0.1410 0.6463 0.098 Uiso calc 1 . .
H H12C 0.9602 0.0928 0.6837 0.098 Uiso calc 1 . .
C C13 0.9223(3) 0.1355(3) 0.5936(3) 0.0445(12) Uani d 1 . .
C C14 0.9569(3) 0.1148(3) 0.5327(3) 0.0475(13) Uani d 1 . .
H H14 1.0104 0.1067 0.5349 0.057 Uiso calc 1 . .
C C15 0.9213(3) 0.1051(3) 0.4705(3) 0.0395(11) Uani d 1 . .
C C16 0.9671(3) 0.0762(3) 0.4126(3) 0.0514(14) Uani d 1 . .
H H16A 0.9435 0.0305 0.3947 0.077 Uiso calc 1 . .
H H16B 1.0192 0.0653 0.4286 0.077 Uiso calc 1 . .
H H16C 0.9684 0.1142 0.3770 0.077 Uiso calc 1 . .
C C17 0.1737(3) 0.2277(3) 0.6336(3) 0.0477(13) Uani d 1 . .
H H17 0.1651 0.2790 0.6435 0.057 Uiso calc 1 . .
C C18 0.1893(3) 0.1793(4) 0.6855(3) 0.0591(15) Uani d 1 . .
H H18 0.1913 0.1967 0.7308 0.071 Uiso calc 1 . .
C C19 0.2023(3) 0.1049(4) 0.6714(3) 0.0629(17) Uani d 1 . .
H H19 0.2133 0.0706 0.7069 0.075 Uiso calc 1 . .
C C20 0.1990(3) 0.0805(3) 0.6053(3) 0.0511(13) Uani d 1 . .
H H20 0.2077 0.0293 0.5951 0.061 Uiso calc 1 . .
C C21 0.1831(3) 0.1312(3) 0.5538(3) 0.0411(11) Uani d 1 . .
C C22 0.1765(2) 0.1157(3) 0.4814(3) 0.0377(11) Uani d 1 . .
C C23 0.1874(3) 0.0452(3) 0.4521(3) 0.0452(12) Uani d 1 . .
H H23 0.2023 0.0040 0.4796 0.054 Uiso calc 1 . .
C C24 0.1767(3) 0.0357(3) 0.3844(3) 0.0482(13) Uani d 1 . .
H H24 0.1836 -0.0121 0.3645 0.058 Uiso calc 1 . .
C C25 0.1556(3) 0.0967(3) 0.3451(3) 0.0444(12) Uani d 1 . .
C C26 0.1472(3) 0.1677(3) 0.3722(3) 0.0410(11) Uani d 1 . .
H H26 0.1346 0.2089 0.3438 0.049 Uiso calc 1 . .
C C27 0.1574(3) 0.1782(3) 0.4412(3) 0.0360(10) Uani d 1 . .
C C28 0.1093(4) 0.4917(3) 0.5815(3) 0.0568(15) Uani d 1 . .
H H28A 0.0791 0.4731 0.6189 0.085 Uiso calc 1 . .
H H28B 0.0838 0.5352 0.5611 0.085 Uiso calc 1 . .
H H28C 0.1600 0.5062 0.5985 0.085 Uiso calc 1 . .
C C29 0.1167(3) 0.4308(3) 0.5292(3) 0.0435(12) Uani d 1 . .
C C30 0.1027(3) 0.4486(3) 0.4614(3) 0.0490(13) Uani d 1 . .
H H30 0.0888 0.4990 0.4520 0.059 Uiso calc 1 . .
C C31 0.1067(3) 0.4011(3) 0.4063(3) 0.0433(12) Uani d 1 . .
C C32 0.0874(4) 0.4303(3) 0.3369(3) 0.0617(16) Uani d 1 . .
H H32A 0.1263 0.4141 0.3055 0.093 Uiso calc 1 . .
H H32B 0.0855 0.4851 0.3379 0.093 Uiso calc 1 . .
H H32C 0.0376 0.4108 0.3219 0.093 Uiso calc 1 . .
N N1 0.6882(2) 0.1843(2) 0.5787(2) 0.0349(8) Uani d 1 . .
N N2 0.1701(2) 0.2051(2) 0.5697(2) 0.0368(9) Uani d 1 . .
O O1 0.85200(19) 0.15218(18) 0.59970(18) 0.0418(8) Uani d 1 . .
O O2 0.85083(18) 0.11665(19) 0.45482(17) 0.0402(8) Uani d 1 . .
O O3 0.13515(19) 0.36673(18) 0.55181(18) 0.0410(8) Uani d 1 . .
O O4 0.1237(2) 0.33092(18) 0.40711(17) 0.0400(8) Uani d 1 . .
Pt Pt1 0.77288(2) 0.15171(2) 0.52011(2) 0.03211(6) Uani d 1 . .
Pt Pt2 0.14668(2) 0.27243(2) 0.49142(2) 0.03308(6) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br1 0.0827(5) 0.0827(5) 0.0401(3) -0.0135(4) -0.0115(3) 0.0119(3)
Br2 0.0957(5) 0.0599(4) 0.0547(4) -0.0007(3) 0.0093(3) -0.0143(3)
C1 0.052(3) 0.043(3) 0.047(3) 0.001(2) 0.000(2) -0.003(2)
C2 0.071(4) 0.056(4) 0.057(4) 0.003(3) 0.008(3) -0.005(3)
C3 0.064(4) 0.052(4) 0.073(4) 0.006(3) 0.027(3) -0.001(3)
C4 0.036(3) 0.039(3) 0.070(4) 0.006(2) 0.009(3) 0.006(3)
C5 0.032(2) 0.023(2) 0.056(3) -0.0007(18) 0.001(2) 0.009(2)
C6 0.027(2) 0.026(2) 0.053(3) -0.0041(18) -0.004(2) 0.009(2)
C7 0.031(3) 0.049(3) 0.060(3) 0.000(2) -0.004(2) 0.008(3)
C8 0.038(3) 0.045(3) 0.063(4) -0.007(2) -0.019(3) 0.017(3)
C9 0.050(3) 0.046(3) 0.040(3) -0.008(2) -0.007(2) 0.009(2)
C10 0.037(3) 0.035(2) 0.046(3) -0.004(2) -0.001(2) 0.009(2)
C11 0.033(2) 0.024(2) 0.045(3) -0.0028(18) -0.002(2) 0.0079(19)
C12 0.048(4) 0.079(5) 0.068(4) -0.001(3) -0.020(3) 0.008(3)
C13 0.036(3) 0.043(3) 0.054(3) -0.008(2) -0.011(2) 0.014(2)
C14 0.028(2) 0.046(3) 0.068(4) 0.003(2) -0.006(2) 0.013(3)
C15 0.027(2) 0.040(3) 0.051(3) 0.001(2) 0.001(2) 0.013(2)
C16 0.035(3) 0.052(3) 0.067(4) 0.004(2) 0.006(2) 0.014(3)
C17 0.041(3) 0.051(3) 0.051(3) -0.001(2) 0.000(2) 0.002(2)
C18 0.057(4) 0.071(4) 0.049(3) -0.007(3) -0.009(3) 0.013(3)
C19 0.053(4) 0.074(4) 0.061(4) -0.006(3) -0.011(3) 0.025(3)
C20 0.043(3) 0.045(3) 0.065(4) -0.001(2) -0.006(3) 0.016(3)
C21 0.027(2) 0.036(3) 0.060(3) -0.0026(19) 0.000(2) 0.010(2)
C22 0.022(2) 0.028(2) 0.064(3) -0.0004(17) 0.005(2) 0.009(2)
C23 0.035(3) 0.031(3) 0.070(4) 0.002(2) 0.007(2) 0.005(2)
C24 0.046(3) 0.029(3) 0.069(4) 0.000(2) 0.010(3) -0.005(2)
C25 0.042(3) 0.039(3) 0.053(3) -0.003(2) 0.014(2) -0.006(2)
C26 0.037(3) 0.032(2) 0.054(3) -0.001(2) 0.008(2) 0.003(2)
C27 0.028(2) 0.028(2) 0.052(3) -0.0004(18) 0.005(2) 0.005(2)
C28 0.062(4) 0.042(3) 0.067(4) 0.003(3) 0.004(3) -0.010(3)
C29 0.033(3) 0.031(2) 0.067(3) -0.004(2) 0.008(2) 0.001(2)
C30 0.049(3) 0.032(3) 0.066(4) 0.003(2) 0.007(3) 0.006(2)
C31 0.045(3) 0.027(2) 0.058(3) -0.002(2) 0.008(2) 0.009(2)
C32 0.085(5) 0.037(3) 0.063(4) 0.007(3) 0.004(3) 0.011(3)
N1 0.033(2) 0.0284(19) 0.043(2) 0.0001(16) 0.0005(17) 0.0037(16)
N2 0.0235(19) 0.037(2) 0.050(2) -0.0018(16) 0.0014(16) 0.0063(18)
O1 0.0344(19) 0.043(2) 0.048(2) -0.0013(14) -0.0061(15) 0.0071(15)
O2 0.0295(17) 0.0403(19) 0.051(2) 0.0019(14) 0.0007(14) 0.0059(15)
O3 0.0366(18) 0.0320(17) 0.055(2) -0.0009(14) 0.0031(15) -0.0027(15)
O4 0.045(2) 0.0295(17) 0.0461(19) 0.0016(14) 0.0055(15) 0.0068(14)
Pt1 0.02610(9) 0.02845(10) 0.04157(11) -0.00042(6) -0.00348(7) 0.00636(7)
Pt2 0.02732(10) 0.02679(9) 0.04527(11) -0.00091(6) 0.00418(7) 0.00340(7)
_geom_special_details
;
Distance SDEV
3.4016 (0.0055) C22 - O3_$6 3.4056 (0.0070) C4 - C15_$5 3.6879 (0.0005) Pt1 -
Pt1_$5 3.7230 (0.0005) Pt2 - Pt2_$6
$5 1.5 - x, 0.5 - y, 1 - z $6 0.5 - x, 0.5 -
y, 1 - z
Least-squares planes (x,y,z in crystal coordinates) and
deviations from them (* indicates atom used to define plane)
17.0464 (0.0086) x + 3.5524 (0.0343) y - 3.1157 (0.0389) z
= 1.9362 (0.0174)
* -0.0159 (0.0032) C22 * 0.0106 (0.0035) C23 * 0.0050 (0.0037) C24 * -0.0152
(0.0036) C25 * 0.0096 (0.0034) C26 * 0.0059 (0.0032) C27
Rms deviation of fitted atoms = 0.0112
17.1816 (0.0082) x + 3.3837 (0.0389) y - 2.0681 (0.0436) z
= 2.4419 (0.0278)
Angle to previous plane (with approximate e.s.d.) = 3.118 (0.129)
* -0.0040 (0.0032) N2 * 0.0023 (0.0037) C17 * 0.0000 (0.0041) C18 * -0.0004
(0.0041) C19 * -0.0014 (0.0038) C20 * 0.0036 (0.0033) C21
Rms deviation of fitted atoms = 0.0025
3.5018 (0.0341) x + 17.1159 (0.0108) y - 4.2313 (0.0388) z
= 3.1261 (0.0262)
Angle to previous plane (with approximate e.s.d.) = 66.846 (0.177)
* 0.0047 (0.0032) C6 * -0.0001 (0.0036) C7 * -0.0055 (0.0037) C8 * 0.0064
(0.0036) C9 * -0.0015 (0.0033) C10 * -0.0040 (0.0031) C11
Rms deviation of fitted atoms = 0.0043
3.8621 (0.0359) x + 17.0726 (0.0113) y - 4.0479 (0.0426) z
= 3.4669 (0.0355)
Angle to previous plane (with approximate e.s.d.) = 1.309 (0.166)
* -0.0056 (0.0031) N1 * 0.0048 (0.0038) C1 * -0.0003 (0.0042) C2 * -0.0032
(0.0042) C3 * 0.0024 (0.0037) C4 * 0.0019 (0.0032) C5
Rms deviation of fitted atoms = 0.0035
17.0575 (0.0059) x + 3.8901 (0.0226) y - 2.3217 (0.0295) z
= 2.4371 (0.0163)
Angle to previous plane (with approximate e.s.d.) = 63.889 (0.149)
* 0.0136 (0.0026) O3 * 0.0004 (0.0034) C29 * -0.0121 (0.0038) C30 * -0.0006
(0.0035) C31 * 0.0149 (0.0026) O4 * -0.0162 (0.0018) Pt2
Rms deviation of fitted atoms = 0.0117
17.1494 (0.0057) x + 3.4219 (0.0232) y - 2.3782 (0.0383) z
= 2.2709 (0.0209)
Angle to previous plane (with approximate e.s.d.) = 1.538 (0.086)
* -0.0073 (0.0024) N2 * 0.0020 (0.0029) C21 * 0.0076 (0.0030) C22 * -0.0104
(0.0026) C27 * 0.0081 (0.0018) Pt2
Rms deviation of fitted atoms = 0.0076
3.7521 (0.0218) x + 17.0640 (0.0077) y - 4.2225 (0.0285) z
= 3.2745 (0.0235)
Angle to previous plane (with approximate e.s.d.) = 65.705 (0.111)
* -0.0132 (0.0026) O1 * -0.0080 (0.0035) C13 * 0.0257 (0.0037) C14 * -0.0103
(0.0034) C15 * -0.0121 (0.0026) O2 * 0.0179 (0.0017) Pt1
Rms deviation of fitted atoms = 0.0157
3.7578 (0.0215) x + 17.0576 (0.0090) y - 4.2485 (0.0367) z
= 3.2795 (0.0249)
Angle to previous plane (with approximate e.s.d.) = 0.080 (0.123)
* -0.0089 (0.0023) N1 * 0.0120 (0.0028) C5 * -0.0086 (0.0028) C6 * 0.0027
(0.0024) C11 * 0.0028 (0.0017) Pt1
Rms deviation of fitted atoms = 0.0079
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C9 C10 . 1.385(7) ?
C6 C11 . 1.414(7) ?
C10 C11 . 1.380(7) ?
C12 C13 . 1.492(8) ?
C13 C14 . 1.413(8) ?
C14 C15 . 1.382(7) ?
C15 C16 . 1.508(7) ?
C17 C18 . 1.368(8) ?
C18 C19 . 1.378(9) ?
C1 C2 . 1.390(8) ?
C19 C20 . 1.381(9) ?
C20 C21 . 1.389(7) ?
C21 C22 . 1.463(7) ?
C22 C23 . 1.402(7) ?
C23 C24 . 1.362(8) ?
Br2 C25 . 1.905(5) ?
C24 C25 . 1.386(8) ?
C25 C26 . 1.388(7) ?
C22 C27 . 1.407(6) ?
C26 C27 . 1.388(7) ?
C28 C29 . 1.511(7) ?
C2 C3 . 1.392(9) ?
C29 C30 . 1.397(8) ?
C30 C31 . 1.387(8) ?
C31 C32 . 1.504(8) ?
C3 C4 . 1.367(9) ?
C4 C5 . 1.400(7) ?
C5 C6 . 1.452(7) ?
C6 C7 . 1.404(7) ?
C7 C8 . 1.369(8) ?
Br1 C9 . 1.915(5) ?
C8 C9 . 1.376(8) ?
C1 H1 . 0.9500 ?
C10 H10 . 0.9500 ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C14 H14 . 0.9500 ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
C17 H17 . 0.9500 ?
C18 H18 . 0.9500 ?
C19 H19 . 0.9500 ?
C2 H2 . 0.9500 ?
C20 H20 . 0.9500 ?
C23 H23 . 0.9500 ?
C24 H24 . 0.9500 ?
C26 H26 . 0.9500 ?
C28 H28A . 0.9800 ?
C28 H28B . 0.9800 ?
C28 H28C . 0.9800 ?
C3 H3 . 0.9500 ?
C30 H30 . 0.9500 ?
C32 H32A . 0.9800 ?
C32 H32B . 0.9800 ?
C32 H32C . 0.9800 ?
C4 H4 . 0.9500 ?
C7 H7 . 0.9500 ?
C8 H8 . 0.9500 ?
C1 N1 . 1.325(6) ?
C5 N1 . 1.367(6) ?
C17 N2 . 1.331(7) ?
C21 N2 . 1.378(6) ?
C13 O1 . 1.279(6) ?
C15 O2 . 1.284(5) ?
C29 O3 . 1.270(6) ?
C31 O4 . 1.290(6) ?
C11 Pt1 . 1.970(5) ?
N1 Pt1 . 1.995(4) ?
O1 Pt1 . 2.077(3) y
O2 Pt1 . 2.007(3) y
C27 Pt2 . 1.969(5) ?
N2 Pt2 . 1.999(4) ?
O3 Pt2 . 2.081(3) y
O4 Pt2 . 2.005(3) y
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 122.5(5) ?
N1 C1 H1 . . 118.8 ?
C2 C1 H1 . . 118.8 ?
C1 C2 C3 . . 117.8(6) ?
C1 C2 H2 . . 121.1 ?
C3 C2 H2 . . 121.1 ?
C4 C3 C2 . . 119.9(6) ?
C4 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
C3 C4 C5 . . 120.2(5) ?
C3 C4 H4 . . 119.9 ?
C5 C4 H4 . . 119.9 ?
N1 C5 C4 . . 119.1(5) ?
N1 C5 C6 . . 113.4(4) ?
C4 C5 C6 . . 127.5(5) ?
C7 C6 C11 . . 120.6(5) ?
C7 C6 C5 . . 124.2(5) ?
C11 C6 C5 . . 115.2(4) ?
C8 C7 C6 . . 120.5(5) ?
C8 C7 H7 . . 119.8 ?
C6 C7 H7 . . 119.8 ?
C7 C8 C9 . . 118.2(5) ?
C7 C8 H8 . . 120.9 ?
C9 C8 H8 . . 120.9 ?
C8 C9 C10 . . 123.1(5) ?
C8 C9 Br1 . . 118.4(4) ?
C10 C9 Br1 . . 118.5(4) ?
C11 C10 C9 . . 119.6(5) ?
C11 C10 H10 . . 120.2 ?
C9 C10 H10 . . 120.2 ?
C10 C11 C6 . . 118.1(4) ?
C10 C11 Pt1 . . 128.2(4) ?
C6 C11 Pt1 . . 113.7(4) ?
C13 C12 H12A . . 109.5 ?
C13 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C13 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
O1 C13 C14 . . 125.3(5) ?
O1 C13 C12 . . 115.3(5) ?
C14 C13 C12 . . 119.4(5) ?
C15 C14 C13 . . 126.9(5) ?
C15 C14 H14 . . 116.5 ?
C13 C14 H14 . . 116.5 ?
O2 C15 C14 . . 127.5(5) ?
O2 C15 C16 . . 113.6(5) ?
C14 C15 C16 . . 119.0(4) ?
C15 C16 H16A . . 109.5 ?
C15 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C15 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N2 C17 C18 . . 121.9(6) ?
N2 C17 H17 . . 119.1 ?
C18 C17 H17 . . 119.1 ?
C17 C18 C19 . . 119.3(6) ?
C17 C18 H18 . . 120.3 ?
C19 C18 H18 . . 120.3 ?
C18 C19 C20 . . 119.6(5) ?
C18 C19 H19 . . 120.2 ?
C20 C19 H19 . . 120.2 ?
C19 C20 C21 . . 119.7(6) ?
C19 C20 H20 . . 120.1 ?
C21 C20 H20 . . 120.1 ?
N2 C21 C20 . . 119.2(5) ?
N2 C21 C22 . . 113.4(4) ?
C20 C21 C22 . . 127.4(5) ?
C23 C22 C27 . . 120.8(5) ?
C23 C22 C21 . . 124.6(4) ?
C27 C22 C21 . . 114.6(4) ?
C24 C23 C22 . . 120.3(5) ?
C24 C23 H23 . . 119.9 ?
C22 C23 H23 . . 119.9 ?
C23 C24 C25 . . 119.0(5) ?
C23 C24 H24 . . 120.5 ?
C25 C24 H24 . . 120.5 ?
C24 C25 C26 . . 122.0(5) ?
C24 C25 Br2 . . 118.9(4) ?
C26 C25 Br2 . . 119.0(4) ?
C27 C26 C25 . . 119.5(5) ?
C27 C26 H26 . . 120.2 ?
C25 C26 H26 . . 120.2 ?
C26 C27 C22 . . 118.3(5) ?
C26 C27 Pt2 . . 127.0(4) ?
C22 C27 Pt2 . . 114.7(4) ?
C29 C28 H28A . . 109.5 ?
C29 C28 H28B . . 109.5 ?
H28A C28 H28B . . 109.5 ?
C29 C28 H28C . . 109.5 ?
H28A C28 H28C . . 109.5 ?
H28B C28 H28C . . 109.5 ?
O3 C29 C30 . . 125.6(5) ?
O3 C29 C28 . . 115.7(5) ?
C30 C29 C28 . . 118.7(5) ?
C31 C30 C29 . . 127.4(5) ?
C31 C30 H30 . . 116.3 ?
C29 C30 H30 . . 116.3 ?
O4 C31 C30 . . 127.0(5) ?
O4 C31 C32 . . 113.3(5) ?
C30 C31 C32 . . 119.7(5) ?
C31 C32 H32A . . 109.5 ?
C31 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C31 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
C1 N1 C5 . . 120.5(4) ?
C1 N1 Pt1 . . 123.8(3) ?
C5 N1 Pt1 . . 115.7(3) ?
C17 N2 C21 . . 120.4(4) ?
C17 N2 Pt2 . . 124.1(4) ?
C21 N2 Pt2 . . 115.6(3) ?
C13 O1 Pt1 . . 123.8(3) ?
C15 O2 Pt1 . . 124.2(3) ?
C29 O3 Pt2 . . 123.8(4) ?
C31 O4 Pt2 . . 124.0(3) ?
C11 Pt1 N1 . . 81.89(18) ?
C11 Pt1 O2 . . 93.04(17) ?
N1 Pt1 O2 . . 174.80(15) ?
C11 Pt1 O1 . . 174.72(17) ?
N1 Pt1 O1 . . 92.90(15) ?
O2 Pt1 O1 . . 92.15(14) ?
C27 Pt2 N2 . . 81.73(18) ?
C27 Pt2 O4 . . 92.57(17) ?
N2 Pt2 O4 . . 174.29(15) ?
C27 Pt2 O3 . . 175.20(17) ?
N2 Pt2 O3 . . 93.57(16) ?
O4 Pt2 O3 . . 92.12(13) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 C3 . . . . -0.6(9) ?
C1 C2 C3 C4 . . . . -0.2(9) ?
C2 C3 C4 C5 . . . . 0.4(9) ?
C3 C4 C5 N1 . . . . 0.1(7) ?
C3 C4 C5 C6 . . . . 178.0(5) ?
N1 C5 C6 C7 . . . . 178.2(4) ?
C4 C5 C6 C7 . . . . 0.2(8) ?
N1 C5 C6 C11 . . . . -2.2(6) ?
C4 C5 C6 C11 . . . . 179.8(4) ?
C11 C6 C7 C8 . . . . -0.4(7) ?
C5 C6 C7 C8 . . . . 179.2(5) ?
C6 C7 C8 C9 . . . . -0.6(8) ?
C7 C8 C9 C10 . . . . 1.2(8) ?
C7 C8 C9 Br1 . . . . -179.5(4) ?
C8 C9 C10 C11 . . . . -0.9(8) ?
Br1 C9 C10 C11 . . . . 179.8(3) ?
C9 C10 C11 C6 . . . . -0.1(7) ?
C9 C10 C11 Pt1 . . . . 179.7(4) ?
C7 C6 C11 C10 . . . . 0.7(7) ?
C5 C6 C11 C10 . . . . -178.9(4) ?
C7 C6 C11 Pt1 . . . . -179.1(4) ?
C5 C6 C11 Pt1 . . . . 1.3(5) ?
O1 C13 C14 C15 . . . . -3.6(9) ?
C12 C13 C14 C15 . . . . 175.8(5) ?
C13 C14 C15 O2 . . . . 3.9(9) ?
C13 C14 C15 C16 . . . . -174.6(5) ?
N2 C17 C18 C19 . . . . 0.4(9) ?
C17 C18 C19 C20 . . . . -0.1(9) ?
C18 C19 C20 C21 . . . . 0.3(8) ?
C19 C20 C21 N2 . . . . -0.6(8) ?
C19 C20 C21 C22 . . . . -179.2(5) ?
N2 C21 C22 C23 . . . . 179.7(4) ?
C20 C21 C22 C23 . . . . -1.7(8) ?
N2 C21 C22 C27 . . . . -0.6(6) ?
C20 C21 C22 C27 . . . . 178.0(5) ?
C27 C22 C23 C24 . . . . -2.6(7) ?
C21 C22 C23 C24 . . . . 177.1(5) ?
C22 C23 C24 C25 . . . . 0.6(8) ?
C23 C24 C25 C26 . . . . 1.9(8) ?
C23 C24 C25 Br2 . . . . -175.1(4) ?
C24 C25 C26 C27 . . . . -2.4(8) ?
Br2 C25 C26 C27 . . . . 174.6(4) ?
C25 C26 C27 C22 . . . . 0.3(7) ?
C25 C26 C27 Pt2 . . . . -178.7(4) ?
C23 C22 C27 C26 . . . . 2.1(7) ?
C21 C22 C27 C26 . . . . -177.6(4) ?
C23 C22 C27 Pt2 . . . . -178.8(3) ?
C21 C22 C27 Pt2 . . . . 1.5(5) ?
O3 C29 C30 C31 . . . . -0.6(9) ?
C28 C29 C30 C31 . . . . 179.8(5) ?
C29 C30 C31 O4 . . . . 0.5(9) ?
C29 C30 C31 C32 . . . . 178.3(5) ?
C2 C1 N1 C5 . . . . 1.2(8) ?
C2 C1 N1 Pt1 . . . . 179.9(4) ?
C4 C5 N1 C1 . . . . -0.9(7) ?
C6 C5 N1 C1 . . . . -179.1(4) ?
C4 C5 N1 Pt1 . . . . -179.7(3) ?
C6 C5 N1 Pt1 . . . . 2.1(5) ?
C18 C17 N2 C21 . . . . -0.8(8) ?
C18 C17 N2 Pt2 . . . . 179.5(4) ?
C20 C21 N2 C17 . . . . 0.9(7) ?
C22 C21 N2 C17 . . . . 179.7(4) ?
C20 C21 N2 Pt2 . . . . -179.4(4) ?
C22 C21 N2 Pt2 . . . . -0.6(5) ?
C14 C13 O1 Pt1 . . . . 0.3(7) ?
C12 C13 O1 Pt1 . . . . -179.0(4) ?
C14 C15 O2 Pt1 . . . . -0.7(7) ?
C16 C15 O2 Pt1 . . . . 177.9(3) ?
C30 C29 O3 Pt2 . . . . -1.2(7) ?
C28 C29 O3 Pt2 . . . . 178.4(3) ?
C30 C31 O4 Pt2 . . . . 1.5(7) ?
C32 C31 O4 Pt2 . . . . -176.5(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C1 H1 O1 . 0.95 2.40 2.999(7) 120.6 y
C4 H4 O4 7_556 0.95 2.58 3.281(6) 130.9 y
C17 H17 O3 . 0.95 2.45 3.034(6) 119.8 y
C17 H17 Br1 8_456 0.95 2.87 3.693(6) 145.0 y
_shelx_hkl_file
;
-2 0 0 408.43 14.90
-2 0 0 414.13 14.93
2 0 0 318.11 14.89
2 0 0 332.07 14.89
-4 0 0 474.03 18.17
-4 0 0 458.23 18.15
4 0 0 404.62 18.16
4 0 0 458.88 18.21
6 0 0 99.77 4.44
6 0 0 111.74 4.43
-6 0 0 109.08 4.46
-6 0 0 109.04 4.40
-8 0 0 120.20 5.00
8 0 0 123.60 4.96
8 0 0 113.11 4.98
-8 0 0 122.24 4.91
-10 0 0 165.33 7.22
10 0 0 182.71 7.16
-10 0 0 176.59 7.11
10 0 0 170.88 7.20
12 0 0 20.72 1.02
-12 0 0 20.33 1.09
-12 0 0 20.37 0.95
12 0 0 20.05 1.07
14 0 0 101.66 4.34
-14 0 0 101.32 4.36
14 0 0 100.22 4.27
-16 0 0 20.53 1.19
16 0 0 20.95 1.17
18 0 0 0.12 0.35
-18 0 0 0.08 0.34
20 0 0 0.30 0.42
-20 0 0 0.10 0.40
-22 0 0 14.12 1.12
22 0 0 17.96 1.14
-1 -1 0 0.42 0.06
1 -1 0 0.38 0.04
1 -1 0 0.36 0.04
-1 1 0 0.36 0.06
1 1 0 0.38 0.05
-1 1 0 0.44 0.05
3 -1 0 10.54 0.49
-3 -1 0 9.65 0.51
-3 -1 0 10.58 0.44
3 -1 0 10.52 0.46
-3 1 0 11.08 0.50
3 1 0 10.37 0.49
-3 1 0 9.46 0.50
5 -1 0 162.27 6.14
-5 -1 0 142.09 6.10
5 -1 0 149.92 6.17
-5 -1 0 151.08 6.18
5 1 0 141.71 6.14
-5 1 0 159.03 6.15
-5 1 0 151.53 6.17
5 1 0 147.18 6.17
-7 -1 0 41.45 1.83
7 -1 0 41.83 1.80
7 -1 0 43.22 1.83
-7 -1 0 38.99 1.72
7 1 0 36.34 1.80
7 1 0 40.74 1.78
-7 1 0 42.77 1.83
-7 1 0 44.91 1.78
-9 -1 0 4.63 0.45
9 -1 0 5.42 0.43
9 -1 0 4.96 0.40
-9 -1 0 5.05 0.32
-9 1 0 5.34 0.37
-9 1 0 5.41 0.46
9 1 0 4.81 0.43
9 1 0 4.45 0.38
-11 -1 0 11.69 0.57
11 -1 0 10.46 0.63
-11 -1 0 11.36 0.71
11 -1 0 11.75 0.69
-11 1 0 11.36 0.73
11 1 0 11.11 0.71
11 1 0 10.19 0.64
-11 1 0 10.94 0.60
13 -1 0 15.68 0.83
-13 -1 0 15.62 0.93
13 -1 0 15.37 0.90
13 1 0 15.39 0.85
-13 1 0 14.00 0.91
13 1 0 14.95 0.90
15 -1 0 13.74 0.86
-15 -1 0 14.18 0.90
15 -1 0 14.67 0.80
15 1 0 14.45 0.83
-15 1 0 14.68 0.93
15 1 0 12.18 0.87
17 -1 0 4.37 0.52
-17 -1 0 3.04 0.51
-17 1 0 3.87 0.54
17 1 0 3.61 0.55
19 -1 0 3.03 0.50
-19 -1 0 0.79 0.45
-19 1 0 1.58 0.48
19 1 0 3.67 0.56
-21 -1 0 -0.09 0.43
21 -1 0 0.17 0.39
21 1 0 0.68 0.44
-21 1 0 -0.27 0.41
0 2 0 349.88 14.17
2 -2 0 61.68 2.59
-2 -2 0 60.60 2.61
2 -2 0 63.28 2.59
-2 -2 0 63.71 2.60
-2 2 0 65.47 2.60
2 2 0 63.92 2.58
-2 2 0 65.82 2.63
4 -2 0 26.27 1.14
-4 -2 0 24.03 1.17
4 -2 0 26.80 1.12
4 2 0 28.01 1.17
4 2 0 27.19 1.09
-4 2 0 27.03 1.17
4 2 0 26.50 1.15
-4 2 0 26.89 1.17
6 -2 0 49.56 2.06
6 -2 0 48.66 2.10
-6 -2 0 46.95 2.13
6 2 0 49.54 2.10
-6 2 0 49.69 2.12
-6 2 0 49.95 2.11
6 2 0 51.84 2.13
-8 -2 0 9.13 0.48
8 -2 0 10.85 0.56
8 -2 0 10.81 0.61
-8 -2 0 10.26 0.63
-8 2 0 10.79 0.62
8 2 0 10.47 0.61
-8 2 0 11.08 0.58
8 2 0 10.15 0.58
10 -2 0 95.30 3.69
-10 -2 0 92.47 3.71
-10 -2 0 74.60 3.53
10 -2 0 84.69 3.63
-10 2 0 90.39 3.62
10 2 0 83.69 3.64
10 2 0 79.26 3.67
-10 2 0 91.31 3.69
-12 -2 0 0.67 0.29
12 -2 0 0.30 0.24
12 -2 0 0.27 0.22
-12 2 0 0.29 0.20
-12 2 0 0.24 0.28
12 2 0 0.52 0.28
12 2 0 0.57 0.24
-14 -2 0 44.36 2.12
14 -2 0 44.83 2.08
14 -2 0 45.09 2.01
14 2 0 43.30 2.11
-14 2 0 44.87 2.11
14 2 0 46.69 2.06
16 -2 0 13.22 0.83
-16 -2 0 13.78 0.89
-16 2 0 11.80 0.85
16 2 0 11.87 0.89
16 2 0 12.59 0.80
-18 -2 0 1.22 0.45
18 -2 0 1.03 0.40
-18 2 0 0.53 0.39
18 2 0 1.30 0.44
-20 -2 0 4.40 0.63
20 -2 0 5.12 0.61
-20 2 0 3.58 0.59
20 2 0 4.81 0.67
22 -2 0 2.20 0.54
-22 -2 0 2.29 0.59
-22 2 0 2.55 0.60
22 2 0 1.54 0.54
-1 -3 0 16.29 0.75
-1 -3 0 16.98 0.72
1 -3 0 16.21 0.75
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3 -5 -9 100.51 4.17
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1 5 -9 195.52 8.09
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1 -5 9 11.73 0.67
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3 -5 9 42.01 1.90
3 -5 9 41.64 1.87
3 5 9 42.76 1.88
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1 1 -25 7.35 0.77
-1 1 25 6.57 0.81
-1 -1 -25 1.05 0.43
1 -1 25 1.06 0.50
1 1 25 1.32 0.53
-1 1 -25 0.14 0.37
-3 -1 -25 0.00 0.38
3 1 25 -0.34 0.40
-3 1 -25 -0.23 0.39
4 -2 -25 1.08 0.45
-4 2 25 1.17 0.53
2 -2 -25 -0.60 0.32
-2 -2 25 0.12 0.44
2 2 -25 -0.04 0.41
-2 2 25 -0.24 0.41
0 -2 -25 0.38 0.40
0 -2 25 0.48 0.47
0 2 -25 0.34 0.42
0 2 25 0.57 0.46
-2 -2 -25 0.43 0.40
-2 2 -25 1.16 0.43
2 2 25 0.15 0.44
-4 2 -25 0.18 0.38
-5 3 25 1.14 0.53
3 -3 -25 0.96 0.42
-3 3 25 0.99 0.51
3 3 -25 0.70 0.45
1 -3 -25 -0.06 0.38
-1 -3 25 0.67 0.46
-1 3 25 0.93 0.46
1 3 -25 -0.13 0.37
-1 -3 -25 2.26 0.49
1 3 25 1.02 0.49
-1 3 -25 1.08 0.45
3 3 25 5.37 0.72
-3 3 -25 4.18 0.64
-4 4 25 0.34 0.45
2 -4 -25 0.22 0.41
-2 4 25 0.33 0.45
0 -4 -25 1.44 0.45
0 4 -25 1.22 0.49
0 4 25 0.73 0.49
-2 -4 -25 0.31 0.40
-2 4 -25 -0.07 0.39
2 4 25 0.36 0.48
1 -5 -25 -0.30 0.38
-1 5 25 -0.67 0.39
-1 -5 -25 5.58 0.65
1 5 25 5.63 0.77
-1 5 -25 5.55 0.72
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 59903
_shelx_res_file
;
TITL fuji_sugaya_PtppyBracac_300 in C2/c
CELL 0.71073 17.5569 17.8765 19.8316 90.000 91.397 90.000
ZERR 16.00 0.0021 0.0022 0.0024 0.000 0.001 0.000
LATT 7
SYMM -x, y, -z+1/2
SFAC C H N O Br Pt
UNIT 256 224 16 32 16 16
L.S. 16
ACTA
BOND $H
FMAP 2
PLAN 5
SIZE 0.020 0.060 0.180
HTAB
CONF
rtab sdev Pt2 Pt2_$6
rtab sdev Pt1 Pt1_$5
eqiv $6 -x+1.5, -y+2.5, -z+1
eqiv $5 -x+1.5, -y+1.5, -z+1
EQIV $4 -x+1/2, -y+1/2, -z+1
EQIV $3 -x+1, y, -z+1/2
EQIV $2 x-1/2, -y+1/2, z+1/2
EQIV $1 x-1/2, y+1/2, z
HTAB C32 Br1_$1
HTAB C26 O4
HTAB C17 O3
HTAB C17 Br1_$2
HTAB C16 Br2_$3
HTAB C10 O2
HTAB C4 O4_$4
HTAB C1 O1
HTAB C32 Br1_$1
HTAB C28 Br1_$2
HTAB C26 O4
HTAB C17 O3
HTAB C17 Br1_$2
HTAB C16 Br2_$3
HTAB C10 O2
HTAB C4 O4_$4
HTAB C1 O1
HTAB C32 Br1_$1
HTAB C28 Br1_$2
HTAB C26 O4
HTAB C17 Br1_$2
HTAB C17 O3
HTAB C16 Br2_$3
HTAB C10 O2
HTAB C1 O1
HTAB C4 O4_$4
HTAB C1 O1
HTAB C4 O4_$4
HTAB C10 O2
HTAB C16 Br2_$3
HTAB C17 Br1_$2
HTAB C17 O3
HTAB C26 O4
HTAB C28 Br1_$2
HTAB C32 Br1_$1
HTAB C1 O1
HTAB C4 O4_$4
HTAB C10 O2
HTAB C17 Br1_$2
HTAB C17 O3
HTAB C26 O4
HTAB C28 Br1_$2
HTAB C32 Br1_$1
HTAB C1 O1
HTAB C4 O4_$4
HTAB C10 O2
HTAB C17 Br1_$2
HTAB C17 O3
HTAB C26 O4
HTAB C28 Br1_$2
HTAB C32 Br1_$1
HTAB C1 O1
HTAB C4 O4_$4
HTAB C10 O2
HTAB C16 Br2_$3
HTAB C17 Br1_$2
HTAB C17 O3
HTAB C26 O4
HTAB C28 Br1_$2
HTAB C32 Br1_$1
TEMP -73.000
WGHT 0.036800 16.030602
FVAR 0.02201
BR1 5 0.637939 0.114488 0.248755 11.00000 0.08266 0.08269 =
0.04010 0.01191 -0.01155 -0.01350
BR2 5 0.132873 0.081662 0.251657 11.00000 0.09573 0.05991 =
0.05465 -0.01430 0.00930 -0.00066
C1 1 0.696821 0.198405 0.643992 11.00000 0.05246 0.04331 =
0.04750 -0.00321 -0.00031 0.00120
AFIX 43
H1 2 0.745916 0.192848 0.664588 11.00000 -1.20000
AFIX 0
C2 1 0.636734 0.221069 0.683514 11.00000 0.07089 0.05639 =
0.05730 -0.00462 0.00785 0.00337
AFIX 43
H2 2 0.644064 0.230435 0.730377 11.00000 -1.20000
AFIX 0
C3 1 0.565460 0.229591 0.652168 11.00000 0.06395 0.05226 =
0.07294 -0.00054 0.02739 0.00555
AFIX 43
H3 2 0.523089 0.244880 0.677685 11.00000 -1.20000
AFIX 0
C4 1 0.556521 0.215933 0.584642 11.00000 0.03625 0.03930 =
0.06996 0.00629 0.00887 0.00593
AFIX 43
H4 2 0.507950 0.222089 0.563196 11.00000 -1.20000
AFIX 0
C5 1 0.618736 0.192890 0.546954 11.00000 0.03179 0.02299 =
0.05563 0.00918 0.00094 -0.00073
C6 1 0.618964 0.173905 0.475782 11.00000 0.02692 0.02616 =
0.05304 0.00858 -0.00430 -0.00406
C7 1 0.554286 0.176237 0.432819 11.00000 0.03138 0.04878 =
0.05957 0.00846 -0.00402 -0.00035
AFIX 43
H7 2 0.506459 0.190365 0.450249 11.00000 -1.20000
AFIX 0
C8 1 0.559601 0.158312 0.366003 11.00000 0.03846 0.04542 =
0.06301 0.01662 -0.01862 -0.00708
AFIX 43
H8 2 0.515953 0.159326 0.336747 11.00000 -1.20000
AFIX 0
C9 1 0.629883 0.138788 0.342379 11.00000 0.05017 0.04598 =
0.04011 0.00935 -0.00679 -0.00797
C10 1 0.694851 0.135145 0.383270 11.00000 0.03746 0.03460 =
0.04558 0.00869 -0.00090 -0.00359
AFIX 43
H10 2 0.742114 0.120721 0.364900 11.00000 -1.20000
AFIX 0
C11 1 0.690543 0.152587 0.450851 11.00000 0.03320 0.02375 =
0.04546 0.00794 -0.00182 -0.00281
C12 1 0.969306 0.138116 0.657243 11.00000 0.04778 0.07887 =
0.06777 0.00781 -0.01969 -0.00055
AFIX 137
H12A 2 0.955189 0.182204 0.683517 11.00000 -1.50000
H12B 2 1.023367 0.141041 0.646334 11.00000 -1.50000
H12C 2 0.960225 0.092819 0.683695 11.00000 -1.50000
AFIX 0
C13 1 0.922312 0.135505 0.593565 11.00000 0.03585 0.04334 =
0.05372 0.01374 -0.01051 -0.00779
C14 1 0.956925 0.114816 0.532735 11.00000 0.02778 0.04630 =
0.06793 0.01295 -0.00586 0.00329
AFIX 43
H14 2 1.010404 0.106697 0.534889 11.00000 -1.20000
AFIX 0
C15 1 0.921272 0.105136 0.470452 11.00000 0.02710 0.04019 =
0.05123 0.01250 0.00069 0.00126
C16 1 0.967084 0.076241 0.412643 11.00000 0.03466 0.05233 =
0.06739 0.01395 0.00570 0.00419
AFIX 137
H16A 2 0.943480 0.030476 0.394705 11.00000 -1.50000
H16B 2 1.019152 0.065278 0.428624 11.00000 -1.50000
H16C 2 0.968399 0.114184 0.377024 11.00000 -1.50000
AFIX 0
C17 1 0.173669 0.227729 0.633588 11.00000 0.04117 0.05071 =
0.05114 0.00191 -0.00036 -0.00084
AFIX 43
H17 2 0.165123 0.279005 0.643458 11.00000 -1.20000
AFIX 0
C18 1 0.189330 0.179258 0.685486 11.00000 0.05671 0.07056 =
0.04944 0.01326 -0.00907 -0.00728
AFIX 43
H18 2 0.191273 0.196673 0.730754 11.00000 -1.20000
AFIX 0
C19 1 0.202259 0.104897 0.671402 11.00000 0.05295 0.07433 =
0.06076 0.02545 -0.01071 -0.00629
AFIX 43
H19 2 0.213312 0.070629 0.706923 11.00000 -1.20000
AFIX 0
C20 1 0.199039 0.080537 0.605314 11.00000 0.04275 0.04501 =
0.06514 0.01619 -0.00583 -0.00103
AFIX 43
H20 2 0.207657 0.029345 0.595149 11.00000 -1.20000
AFIX 0
C21 1 0.183143 0.131216 0.553751 11.00000 0.02723 0.03600 =
0.06012 0.00998 -0.00010 -0.00258
C22 1 0.176535 0.115697 0.481414 11.00000 0.02153 0.02773 =
0.06404 0.00936 0.00474 -0.00040
C23 1 0.187425 0.045225 0.452134 11.00000 0.03545 0.03087 =
0.06964 0.00506 0.00699 0.00233
AFIX 43
H23 2 0.202338 0.003979 0.479626 11.00000 -1.20000
AFIX 0
C24 1 0.176707 0.035685 0.384445 11.00000 0.04613 0.02950 =
0.06937 -0.00546 0.01001 -0.00029
AFIX 43
H24 2 0.183581 -0.012075 0.364486 11.00000 -1.20000
AFIX 0
C25 1 0.155625 0.096672 0.345103 11.00000 0.04249 0.03878 =
0.05251 -0.00552 0.01447 -0.00262
C26 1 0.147240 0.167701 0.372250 11.00000 0.03733 0.03189 =
0.05420 0.00276 0.00782 -0.00107
AFIX 43
H26 2 0.134603 0.208856 0.343810 11.00000 -1.20000
AFIX 0
C27 1 0.157449 0.178160 0.441237 11.00000 0.02760 0.02825 =
0.05219 0.00465 0.00462 -0.00038
C28 1 0.109251 0.491702 0.581514 11.00000 0.06207 0.04164 =
0.06690 -0.00979 0.00413 0.00316
AFIX 137
H28A 2 0.079100 0.473137 0.618939 11.00000 -1.50000
H28B 2 0.083819 0.535220 0.561053 11.00000 -1.50000
H28C 2 0.160022 0.506218 0.598473 11.00000 -1.50000
AFIX 0
C29 1 0.116672 0.430845 0.529206 11.00000 0.03274 0.03134 =
0.06659 0.00123 0.00788 -0.00359
C30 1 0.102663 0.448606 0.461438 11.00000 0.04922 0.03172 =
0.06620 0.00630 0.00681 0.00310
AFIX 43
H30 2 0.088806 0.498973 0.452026 11.00000 -1.20000
AFIX 0
C31 1 0.106663 0.401145 0.406335 11.00000 0.04526 0.02658 =
0.05845 0.00914 0.00755 -0.00216
C32 1 0.087356 0.430315 0.336857 11.00000 0.08464 0.03721 =
0.06340 0.01112 0.00365 0.00738
AFIX 137
H32A 2 0.126348 0.414080 0.305497 11.00000 -1.50000
H32B 2 0.085533 0.485093 0.337926 11.00000 -1.50000
H32C 2 0.037609 0.410778 0.321881 11.00000 -1.50000
AFIX 0
N1 3 0.688201 0.184258 0.578664 11.00000 0.03332 0.02841 =
0.04281 0.00373 0.00051 0.00010
N2 3 0.170070 0.205061 0.569652 11.00000 0.02352 0.03677 =
0.05015 0.00633 0.00139 -0.00177
O1 4 0.852002 0.152176 0.599703 11.00000 0.03440 0.04311 =
0.04762 0.00710 -0.00611 -0.00129
O2 4 0.850835 0.116646 0.454819 11.00000 0.02953 0.04032 =
0.05075 0.00594 0.00073 0.00189
O3 4 0.135148 0.366725 0.551814 11.00000 0.03656 0.03197 =
0.05458 -0.00274 0.00307 -0.00092
O4 4 0.123691 0.330924 0.407113 11.00000 0.04450 0.02948 =
0.04610 0.00681 0.00548 0.00160
PT1 6 0.772882 0.151707 0.520115 11.00000 0.02610 0.02845 =
0.04157 0.00636 -0.00348 -0.00042
PT2 6 0.146681 0.272428 0.491418 11.00000 0.02732 0.02679 =
0.04527 0.00340 0.00418 -0.00091
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM fuji_sugaya_PtppyBracac_300 in C2/c
REM R1 = 0.0273 for 6001 Fo > 4sig(Fo) and 0.0360 for all 7103 data
REM 383 parameters refined using 0 restraints
END
WGHT 0.0319 19.5394
REM Instructions for potential hydrogen bonds
HTAB C1 O1
HTAB C4 O4_$4
HTAB C10 O2
HTAB C16 Br2_$3
HTAB C17 Br1_$2
HTAB C17 O3
HTAB C26 O4
HTAB C32 Br1_$1
REM Highest difference peak 3.662, deepest hole -1.195, 1-sigma level 0.125
Q1 1 0.7755 0.1393 0.4778 11.00000 0.05 3.66
Q2 1 0.1406 0.2596 0.4482 11.00000 0.05 2.67
Q3 1 0.7528 0.1179 0.5422 11.00000 0.05 0.83
Q4 1 0.1498 0.0544 0.2831 11.00000 0.05 0.75
Q5 1 0.8048 0.1880 0.4921 11.00000 0.05 0.66
;
_shelx_res_checksum 96257
_shelxl_version_number 2.014