# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007
data_global
#==============================================================================
#===============================================================================
# 1. submission details
_publ_contact_author_name 'Manfred Scheer'
_publ_contact_author_address # address of author for correspondence
;
Institute of Inorganic Chemistry
University of Regensburg
Regensburg
93040
GERMANY
;
_publ_contact_author_email MANFRED.SCHEER@CHEMIE.UNI-REGENSBURG.DE
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_requested_journal 'Chemical Communications'
_journal_coden_Cambridge 182
# publication choise fi, ci or ei for inorganic
# fm, cm or em for metal-organic
# fo, co or eo for organic
_publ_requested_category ?
_publ_requested_coeditor_name ?
_publ_contact_letter # include date of submission
;
date of submission ?
please consider this cif submission for publication as a
regular structural paper in acta crystallographica c.
;
#===============================================================================
# 2. processing summary (journal office only)
_journal_coden_astm ?
_journal_name_full ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
#===============================================================================
# 3. title and author list
_publ_section_title
;
Cu(I) mediated oligomerisation of a phosphaalkyne
;
_publ_section_title_footnote
;
;
# the loop structure below should contain the names and adresses of all
# authors, in the required order of publication. repeat as necessary.
loop_
_publ_author_name
'Manfred Scheer'
J.Nixon
'Ulf Vogel'
#===============================================================================
# 4. text
_publ_section_synopsis
;
?
;
_publ_section_abstract
;
?
;
# insert blank lines between paragraphs
_publ_section_comment
;
;
_publ_section_exptl_prep
;
?
;
_publ_section_exptl_refinement
;
the data were collected at 103k using an oxford diffraction cryojet
cooler. the structure was solved by direct methods (sir-97)
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., burla, m.c., camalli, m., cascarano, g.l., giacovazzo, c.
guagliardi, a., moliterni, a.g.g., polidori, g. & spagna, r.
(1999) j. appl. cryst. 32, 115-119.
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. (2003). j. appl. cryst. 36, 7-13.
wilson, a.j.c. (1992) ed. international tables for crystallography,
volume c, kluwer academic publishers, dordrecht, the netherlands.
;
_publ_section_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.
;
#===============================================================================
data_476
_database_code_depnum_ccdc_archive 'CCDC 656701'
# 0. audit details
_audit_creation_date 'apr 13 10:10:07 2007'
_audit_creation_method 'platon
option'
_audit_update_record
;
;
#===============================================================================
# 5. chemical data
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C22 H40 Cu3 I3 N P5'
# 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 'C22 H40 Cu3 I3 N P5'
_chemical_formula_iupac ?
_chemical_formula_weight 1044.75
_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
p p 0.2955 0.4335 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
n n 0.0311 0.0180 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
i i -0.3257 6.8362 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
cu cu -1.9646 0.5888 '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 0.0181 0.0091 '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_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
_cell_length_a 11.693(2)
_cell_length_b 12.8918(16)
_cell_length_c 13.172(3)
_cell_angle_alpha 89.985(13)
_cell_angle_beta 64.793(18)
_cell_angle_gamma 77.478(12)
_cell_volume 1744.2(6)
_cell_formula_units_z 2
_cell_measurement_temperature 103(1)
_cell_measurement_reflns_used 3361
_cell_measurement_theta_min 3.5255
_cell_measurement_theta_max 51.2205
_cell_special_details
;
;
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.085
_exptl_crystal_size_mid 0.053
_exptl_crystal_size_min 0.024
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.989
_exptl_crystal_density_method 'not measured'
_exptl_crystal_f_000 1000
_exptl_absorpt_coefficient_mu 25.236
_exptl_crystal_density_meas_temp ?
# permitted for _exptl_absorpt_correction_type :
# 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 multi-scan
_exptl_absorpt_process_details
;
crysalis red, oxford diffraction ltd.,
version 1.171.30.3 (release 12-05-2006 crysalis171 .net)
(compiled may 12 2006,14:43:55)
empirical absorption correction using spherical harmonics,
implemented in scale3 abspack scaling algorithm.
;
_exptl_absorpt_correction_t_min 0.449
_exptl_absorpt_correction_t_max 1.450
#===============================================================================
# 7. experimental data
_exptl_special_details
;
;
_diffrn_ambient_temperature 103(1)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_probe X-ray
_diffrn_radiation_type cuk\a
_diffrn_radiation_source 'enhance (cu) x-ray source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'oxford diffraction gemini ultra'
_diffrn_measurement_method omega-scan
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -78.00 -23.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 0.1529 -75.0000 120.0000 0.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
2 omega -37.00 18.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 0.1529 87.0000 44.0000 0.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
3 omega 23.00 78.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 0.1529 75.0000 120.0000 0.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
4 omega -23.00 28.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 0.1529 -45.0000 120.0000 0.0000 0.0000 51
#__ type_ start__ end____ width___ exp.time_
5 omega 24.00 75.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 0.1529 45.0000 240.0000 0.0000 0.0000 51
#__ type_ start__ end____ width___ exp.time_
6 omega -113.00 -63.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 117.0000 178.0000 0.0000 0.0000 50
#__ type_ start__ end____ width___ exp.time_
7 omega -106.00 -54.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 105.0000 92.0000 0.0000 0.0000 52
#__ type_ start__ end____ width___ exp.time_
8 phi 60.00 120.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -60.8272 0.0000 - 0.0000 0.0000 60
#__ type_ start__ end____ width___ exp.time_
9 omega -139.00 -84.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -75.0000 240.0000 0.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
10 omega -82.00 -29.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -66.0000 345.0000 0.0000 0.0000 53
#__ type_ start__ end____ width___ exp.time_
11 omega -54.00 -2.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 105.0000 92.0000 0.0000 0.0000 52
#__ type_ start__ end____ width___ exp.time_
12 omega -135.00 -83.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -60.0000 289.0000 0.0000 0.0000 52
#__ type_ start__ end____ width___ exp.time_
13 omega -137.00 -83.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -69.0000 259.0000 0.0000 0.0000 54
#__ type_ start__ end____ width___ exp.time_
14 omega -83.00 -28.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -72.0000 149.0000 0.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
15 omega -83.00 -29.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -69.0000 259.0000 0.0000 0.0000 54
#__ type_ start__ end____ width___ exp.time_
16 omega -131.00 -83.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -66.0000 345.0000 0.0000 0.0000 48
#__ type_ start__ end____ width___ exp.time_
17 omega -140.00 -84.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -78.0000 45.0000 0.0000 0.0000 56
#__ type_ start__ end____ width___ exp.time_
18 omega 29.00 84.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 75.0000 23.0000 0.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
19 omega 31.00 84.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 66.0000 209.0000 0.0000 0.0000 53
#__ type_ start__ end____ width___ exp.time_
20 omega 31.00 84.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 75.0000 240.0000 0.0000 0.0000 53
#__ type_ start__ end____ width___ exp.time_
21 omega 98.00 126.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 45.0000 120.0000 0.0000 0.0000 28
#__ type_ start__ end____ width___ exp.time_
22 omega 46.00 93.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 -75.0000 240.0000 0.0000 0.0000 47
#__ type_ start__ end____ width___ exp.time_
23 omega 47.00 77.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 45.0000 0.0000 0.0000 0.0000 30
#__ type_ start__ end____ width___ exp.time_
24 omega 35.00 85.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 45.0000 120.0000 0.0000 0.0000 50
;
_diffrn_detector_area_resol_mean 10.5431
_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 11103
_diffrn_reflns_av_r_equivalents 0.0487
_diffrn_reflns_av_sigmai/neti 0.1286
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 3.53
_diffrn_reflns_theta_max 51.27
_diffrn_reflns_theta_full 51.27
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_reduction_process
;
;
# number of unique reflections
_reflns_number_total 3742
# number of observed reflections (> n sig(i))
_reflns_number_gt 2138
_reflns_threshold_expression i>2\s(i)
_computing_data_collection
;
crysalis ccd, oxford diffraction ltd.,
version 1.171.30.3 (release 12-05-2006 crysalis171 .net)
;
_computing_cell_refinement
;
crysalis red, oxford diffraction ltd.,
version 1.171.30.3 (release 12-05-2006 crysalis171 .net)
;
_computing_data_reduction
;
crysalis red, oxford diffraction ltd.,
version 1.171.30.3 (release 12-05-2006 crysalis171 .net)
;
_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^)+(0.0297p)^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 3742
_refine_ls_number_parameters 308
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_r_factor_all 0.0749
_refine_ls_r_factor_gt 0.0368
_refine_ls_wr_factor_ref 0.0655
_refine_ls_wr_factor_gt 0.0628
_refine_ls_goodness_of_fit_ref 0.811
_refine_ls_restrained_s_all 0.811
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.886
_refine_diff_density_min -0.452
_refine_diff_density_rms 0.119
#===============================================================================
# 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
i1 i uani 0.52286(6) 0.60044(5) 0.10849(6) 1.000 0.0400(3) . .
i2 i uani 0.40529(6) 0.40074(5) 0.59822(6) 1.000 0.0371(3) . .
i3 i uani 0.20318(6) 0.63250(6) 0.43801(6) 1.000 0.0424(3) . .
cu1 cu uani 0.44372(13) 0.53088(11) 0.31152(12) 1.000 0.0396(6) . .
cu2 cu uani 0.64393(14) 0.41109(12) -0.02385(12) 1.000 0.0454(7) . .
cu3 cu uani 0.34219(13) 0.60111(11) 0.54559(12) 1.000 0.0432(6) . .
p1 p uani 0.5195(3) 0.3517(2) 0.2747(2) 1.000 0.0351(11) . .
p2 p uani 0.6673(3) 0.2970(2) 0.0971(2) 1.000 0.0392(11) . .
p3 p uani 0.6890(3) 0.2882(2) 0.3075(2) 1.000 0.0385(11) . .
p4 p uani 0.8291(3) 0.1257(2) 0.1341(2) 1.000 0.0491(12) . .
p5 p uani 0.5776(3) 0.1127(2) 0.2413(3) 1.000 0.0503(12) . .
n1 n uani 0.8031(9) 0.4332(8) -0.1504(8) 1.000 0.051(4) . .
c1 c uani 0.8932(13) 0.4458(9) -0.2189(10) 1.000 0.042(6) . .
c1l c uani 1.0156(9) 0.4503(8) -0.3189(9) 1.000 0.065(5) . .
c2 c uani 0.7983(9) 0.2749(8) 0.1490(7) 1.000 0.036(4) . .
c3 c uani 0.7012(9) 0.1394(8) 0.2885(8) 1.000 0.037(4) . .
c4 c uani 0.6824(9) 0.1509(7) 0.0932(9) 1.000 0.036(4) . .
c5 c uani 0.4483(9) 0.2338(7) 0.3093(8) 1.000 0.043(4) . .
c11 c uani 0.9131(10) 0.3269(9) 0.1029(9) 1.000 0.037(5) . .
c31 c uani 0.7322(11) 0.0673(9) 0.3692(10) 1.000 0.045(5) . .
c41 c uani 0.7023(11) 0.0828(9) -0.0079(10) 1.000 0.049(5) . .
c51 c uani 0.3124(10) 0.2470(10) 0.3093(10) 1.000 0.048(5) . .
c111 c uani 0.8689(9) 0.4467(8) 0.1164(7) 1.000 0.043(5) . .
c112 c uani 0.9961(9) 0.2832(8) -0.0225(8) 1.000 0.055(5) . .
c113 c uani 0.9992(10) 0.2902(8) 0.1656(8) 1.000 0.058(5) . .
c311 c uani 0.6192(10) 0.0959(7) 0.4869(9) 1.000 0.058(5) . .
c312 c uani 0.8569(10) 0.0872(8) 0.3736(9) 1.000 0.061(5) . .
c313 c uani 0.7583(10) -0.0517(8) 0.3300(8) 1.000 0.062(5) . .
c411 c uani 0.7343(10) -0.0376(8) 0.0046(9) 1.000 0.062(6) . .
c412 c uani 0.8132(10) 0.1098(8) -0.1129(8) 1.000 0.064(5) . .
c413 c uani 0.5791(10) 0.1099(7) -0.0264(8) 1.000 0.050(5) . .
c511 c uani 0.2809(9) 0.1381(8) 0.3061(8) 1.000 0.057(5) . .
c512 c uani 0.3124(10) 0.3007(8) 0.2054(8) 1.000 0.047(5) . .
c513 c uani 0.2068(9) 0.3154(8) 0.4153(8) 1.000 0.052(5) . .
h1l1 h uiso 1.08320 0.38570 -0.32900 1.000 0.0980 calc r
h1l2 h uiso 1.04430 0.51340 -0.30710 1.000 0.0980 calc r
h1l3 h uiso 0.99980 0.45480 -0.38630 1.000 0.0980 calc r
h5a h uiso 0.42780 0.23050 0.39100 1.000 0.0510 calc r
h11a h uiso 0.81640 0.46850 0.07520 1.000 0.0640 calc r
h11b h uiso 0.94500 0.47750 0.08630 1.000 0.0640 calc r
h11c h uiso 0.81640 0.47210 0.19660 1.000 0.0640 calc r
h11d h uiso 0.94580 0.30690 -0.06530 1.000 0.0820 calc r
h11e h uiso 1.01990 0.20500 -0.02920 1.000 0.0820 calc r
h11f h uiso 1.07530 0.31010 -0.05270 1.000 0.0820 calc r
h11g h uiso 1.07330 0.32350 0.13720 1.000 0.0870 calc r
h11h h uiso 1.03120 0.21230 0.15250 1.000 0.0870 calc r
h11i h uiso 0.94740 0.31160 0.24670 1.000 0.0870 calc r
h31a h uiso 0.60550 0.17110 0.51190 1.000 0.0870 calc r
h31b h uiso 0.63940 0.05050 0.53960 1.000 0.0870 calc r
h31c h uiso 0.54000 0.08460 0.48470 1.000 0.0870 calc r
h31d h uiso 0.93050 0.06780 0.29870 1.000 0.0920 calc r
h31e h uiso 0.87630 0.04340 0.42780 1.000 0.0920 calc r
h31f h uiso 0.84250 0.16280 0.39730 1.000 0.0920 calc r
h31g h uiso 0.83220 -0.06950 0.25510 1.000 0.0920 calc r
h31h h uiso 0.68080 -0.06550 0.32640 1.000 0.0920 calc r
h31i h uiso 0.77830 -0.09590 0.38360 1.000 0.0920 calc r
h41a h uiso 0.66210 -0.05420 0.07020 1.000 0.0940 calc r
h41b h uiso 0.81400 -0.05640 0.01520 1.000 0.0940 calc r
h41c h uiso 0.74700 -0.07860 -0.06350 1.000 0.0940 calc r
h41d h uiso 0.79160 0.18630 -0.12040 1.000 0.0950 calc r
h41e h uiso 0.82400 0.06880 -0.18040 1.000 0.0950 calc r
h41f h uiso 0.89440 0.09140 -0.10470 1.000 0.0950 calc r
h41g h uiso 0.55830 0.18610 -0.03580 1.000 0.0750 calc r
h41h h uiso 0.50650 0.09370 0.03900 1.000 0.0750 calc r
h41i h uiso 0.59340 0.06750 -0.09430 1.000 0.0750 calc r
h51a h uiso 0.28130 0.10270 0.37180 1.000 0.0850 calc r
h51b h uiso 0.34650 0.09370 0.23690 1.000 0.0850 calc r
h51c h uiso 0.19470 0.14820 0.30740 1.000 0.0850 calc r
h51d h uiso 0.33250 0.37050 0.20650 1.000 0.0710 calc r
h51e h uiso 0.22630 0.31030 0.20660 1.000 0.0710 calc r
h51f h uiso 0.37820 0.25560 0.13680 1.000 0.0710 calc r
h51g h uiso 0.20650 0.28150 0.48200 1.000 0.0770 calc r
h51h h uiso 0.12190 0.32260 0.41480 1.000 0.0770 calc r
h51i h uiso 0.22390 0.38630 0.41750 1.000 0.0770 calc r
loop_
_atom_site_aniso_label
_atom_site_aniso_u_11
_atom_site_aniso_u_22
_atom_site_aniso_u_33
_atom_site_aniso_u_23
_atom_site_aniso_u_13
_atom_site_aniso_u_12
i1 0.0371(5) 0.0478(5) 0.0365(5) 0.0074(4) -0.0176(4) -0.0095(4)
i2 0.0266(5) 0.0492(5) 0.0363(5) 0.0033(4) -0.0135(4) -0.0109(4)
i3 0.0281(5) 0.0580(6) 0.0394(5) -0.0015(4) -0.0163(4) -0.0038(4)
cu1 0.0316(10) 0.0479(11) 0.0385(11) 0.0035(9) -0.0157(9) -0.0069(9)
cu2 0.0370(11) 0.0596(12) 0.0384(11) 0.0040(9) -0.0161(9) -0.0102(9)
cu3 0.0342(10) 0.0561(12) 0.0421(11) 0.0037(9) -0.0199(9) -0.0094(9)
p1 0.0277(19) 0.043(2) 0.035(2) 0.0034(17) -0.0147(16) -0.0070(16)
p2 0.0321(19) 0.042(2) 0.043(2) -0.0006(17) -0.0179(17) -0.0049(17)
p3 0.0280(19) 0.051(2) 0.035(2) 0.0039(17) -0.0141(17) -0.0056(17)
p4 0.042(2) 0.051(2) 0.051(2) 0.0006(19) -0.022(2) -0.0009(18)
p5 0.046(2) 0.048(2) 0.058(2) 0.0009(19) -0.025(2) -0.0083(18)
n1 0.035(7) 0.070(8) 0.049(8) -0.002(7) -0.012(6) -0.028(7)
c1 0.061(11) 0.040(8) 0.045(10) -0.001(8) -0.040(9) -0.014(9)
c1l 0.035(8) 0.084(10) 0.059(9) 0.003(8) 0.000(8) -0.026(8)
c2 0.031(7) 0.062(9) 0.017(7) 0.005(6) -0.012(6) -0.013(7)
c3 0.040(7) 0.042(8) 0.024(7) 0.006(6) -0.016(6) 0.004(6)
c4 0.017(7) 0.020(7) 0.058(8) -0.021(6) -0.008(6) 0.003(5)
c5 0.039(8) 0.048(8) 0.035(7) 0.000(6) -0.008(6) -0.017(7)
c11 0.030(8) 0.036(9) 0.039(9) -0.007(7) -0.011(7) -0.003(7)
c31 0.040(8) 0.046(9) 0.051(9) 0.004(8) -0.024(8) -0.004(7)
c41 0.045(9) 0.041(9) 0.058(10) -0.004(8) -0.021(8) -0.005(7)
c51 0.023(8) 0.052(9) 0.057(10) 0.000(8) -0.002(7) -0.016(7)
c111 0.036(7) 0.072(10) 0.024(7) 0.006(7) -0.015(6) -0.018(7)
c112 0.036(8) 0.068(9) 0.051(9) -0.006(7) -0.008(7) -0.016(7)
c113 0.044(8) 0.088(10) 0.049(8) -0.009(8) -0.023(7) -0.024(7)
c311 0.064(9) 0.040(8) 0.063(9) 0.020(7) -0.024(8) -0.004(7)
c312 0.062(9) 0.054(9) 0.085(10) 0.024(7) -0.057(8) 0.005(7)
c313 0.070(9) 0.041(9) 0.063(9) -0.012(7) -0.035(8) 0.021(7)
c411 0.078(10) 0.037(9) 0.090(10) -0.009(7) -0.061(9) 0.003(7)
c412 0.054(9) 0.088(10) 0.045(9) -0.009(8) -0.019(8) -0.014(8)
c413 0.054(9) 0.044(8) 0.061(9) -0.006(7) -0.038(7) -0.004(7)
c511 0.048(8) 0.076(10) 0.059(9) 0.022(8) -0.030(7) -0.026(8)
c512 0.060(9) 0.055(8) 0.043(8) 0.007(7) -0.035(7) -0.019(7)
c513 0.044(8) 0.067(9) 0.049(9) 0.015(7) -0.023(8) -0.018(7)
#===============================================================================
# 10. molecular geometry
_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
i1 cu1 2.6577(17) . . yes
i1 cu2 2.7209(17) . . yes
i1 cu2 2.655(2) . 2_665 yes
i2 cu3 2.7029(17) . . yes
i2 cu1 2.7877(19) . 2_666 yes
i2 cu3 2.7409(19) . 2_666 yes
i3 cu1 2.6105(18) . . yes
i3 cu3 2.5476(19) . . yes
cu1 p1 2.259(3) . . yes
cu2 p2 2.230(3) . . yes
cu2 n1 1.978(11) . . yes
cu3 p3 2.256(3) . 2_666 yes
p1 p2 2.233(4) . . yes
p1 p3 2.193(5) . . yes
p1 c5 1.854(10) . . yes
p2 c2 1.897(12) . . yes
p2 c4 1.852(9) . . yes
p3 c2 1.912(9) . . yes
p3 c3 1.901(10) . . yes
p4 c2 1.873(10) . . yes
p4 c3 1.923(10) . . yes
p4 c4 1.971(12) . . yes
p5 c3 1.891(12) . . yes
p5 c4 1.943(11) . . yes
p5 c5 1.830(10) . . yes
n1 c1 1.102(17) . . yes
c1 c1l 1.489(18) . . no
c2 c11 1.522(16) . . no
c3 c31 1.519(16) . . no
c4 c41 1.499(16) . . no
c5 c51 1.561(18) . . no
c11 c111 1.503(15) . . no
c11 c112 1.545(14) . . no
c11 c113 1.556(17) . . no
c31 c311 1.526(16) . . no
c31 c312 1.559(19) . . no
c31 c313 1.542(15) . . no
c41 c411 1.542(15) . . no
c41 c412 1.544(16) . . no
c41 c413 1.529(19) . . no
c51 c511 1.532(17) . . no
c51 c512 1.534(16) . . no
c51 c513 1.520(16) . . no
c1l h1l1 0.9800 . . no
c1l h1l2 0.9800 . . no
c1l h1l3 0.9800 . . no
c5 h5a 1.0000 . . no
c111 h11a 0.9800 . . no
c111 h11b 0.9800 . . no
c111 h11c 0.9800 . . no
c112 h11d 0.9800 . . no
c112 h11e 0.9800 . . no
c112 h11f 0.9800 . . no
c113 h11g 0.9800 . . no
c113 h11h 0.9800 . . no
c113 h11i 0.9800 . . no
c311 h31a 0.9800 . . no
c311 h31b 0.9800 . . no
c311 h31c 0.9800 . . no
c312 h31d 0.9800 . . no
c312 h31e 0.9800 . . no
c312 h31f 0.9800 . . no
c313 h31g 0.9800 . . no
c313 h31h 0.9800 . . no
c313 h31i 0.9800 . . no
c411 h41a 0.9800 . . no
c411 h41b 0.9800 . . no
c411 h41c 0.9800 . . no
c412 h41d 0.9800 . . no
c412 h41e 0.9800 . . no
c412 h41f 0.9800 . . no
c413 h41g 0.9800 . . no
c413 h41h 0.9800 . . no
c413 h41i 0.9800 . . no
c511 h51a 0.9800 . . no
c511 h51b 0.9800 . . no
c511 h51c 0.9800 . . no
c512 h51d 0.9800 . . no
c512 h51e 0.9800 . . no
c512 h51f 0.9800 . . no
c513 h51g 0.9800 . . no
c513 h51h 0.9800 . . no
c513 h51i 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
cu1 i1 cu2 100.12(5) . . . yes
cu1 i1 cu2 110.03(6) . . 2_665 yes
cu2 i1 cu2 79.56(6) . . 2_665 yes
cu1 i2 cu3 89.21(5) 2_666 . . yes
cu3 i2 cu3 86.50(5) . . 2_666 yes
cu1 i2 cu3 62.18(5) 2_666 . 2_666 yes
cu1 i3 cu3 67.21(5) . . . yes
i1 cu1 i3 109.43(6) . . . yes
i1 cu1 p1 103.92(8) . . . yes
i1 cu1 i2 103.88(6) . . 2_666 yes
i3 cu1 p1 125.90(11) . . . yes
i2 cu1 i3 106.25(6) 2_666 . . yes
i2 cu1 p1 105.48(11) 2_666 . . yes
i1 cu2 p2 102.97(9) . . . yes
i1 cu2 n1 106.9(3) . . . yes
i1 cu2 i1 100.44(6) . . 2_665 yes
p2 cu2 n1 118.1(3) . . . yes
i1 cu2 p2 119.67(12) 2_665 . . yes
i1 cu2 n1 106.5(3) 2_665 . . yes
i2 cu3 i3 117.47(6) . . . yes
i2 cu3 i2 93.50(5) . . 2_666 yes
i2 cu3 p3 106.01(9) . . 2_666 yes
i2 cu3 i3 109.48(6) 2_666 . . yes
i3 cu3 p3 124.16(11) . . 2_666 yes
i2 cu3 p3 100.57(11) 2_666 . 2_666 yes
cu1 p1 p2 114.05(13) . . . yes
cu1 p1 p3 114.33(16) . . . yes
cu1 p1 c5 136.2(4) . . . yes
p2 p1 p3 81.48(16) . . . yes
p2 p1 c5 99.9(3) . . . yes
p3 p1 c5 96.8(4) . . . yes
cu2 p2 p1 112.55(15) . . . yes
cu2 p2 c2 126.9(3) . . . yes
cu2 p2 c4 130.5(4) . . . yes
p1 p2 c2 88.5(3) . . . yes
p1 p2 c4 101.3(4) . . . yes
c2 p2 c4 87.5(5) . . . yes
p1 p3 c2 89.2(4) . . . yes
p1 p3 c3 99.8(4) . . . yes
cu3 p3 p1 103.91(14) 2_666 . . yes
c2 p3 c3 86.3(4) . . . yes
cu3 p3 c2 133.4(4) 2_666 . . yes
cu3 p3 c3 133.0(3) 2_666 . . yes
c2 p4 c3 86.8(4) . . . yes
c2 p4 c4 84.8(4) . . . yes
c3 p4 c4 86.8(5) . . . yes
c3 p5 c4 88.5(5) . . . yes
c3 p5 c5 99.4(5) . . . yes
c4 p5 c5 103.9(4) . . . yes
cu2 n1 c1 178.1(12) . . . yes
n1 c1 c1l 172.8(13) . . . yes
p2 c2 p3 98.7(5) . . . yes
p2 c2 p4 94.5(5) . . . yes
p2 c2 c11 123.3(7) . . . yes
p3 c2 p4 93.6(4) . . . yes
p3 c2 c11 120.6(7) . . . yes
p4 c2 c11 119.4(8) . . . yes
p3 c3 p4 92.4(5) . . . yes
p3 c3 p5 111.5(6) . . . yes
p3 c3 c31 119.3(8) . . . yes
p4 c3 p5 90.6(5) . . . yes
p4 c3 c31 118.8(8) . . . yes
p5 c3 c31 118.1(8) . . . yes
p2 c4 p4 92.8(5) . . . yes
p2 c4 p5 110.6(5) . . . yes
p2 c4 c41 123.5(8) . . . yes
p4 c4 p5 87.7(5) . . . yes
p4 c4 c41 116.0(8) . . . yes
p5 c4 c41 117.7(8) . . . yes
p1 c5 p5 108.9(6) . . . yes
p1 c5 c51 115.6(7) . . . yes
p5 c5 c51 120.9(8) . . . yes
c2 c11 c111 111.6(10) . . . no
c2 c11 c112 107.6(9) . . . no
c2 c11 c113 108.6(9) . . . no
c111 c11 c112 111.2(8) . . . no
c111 c11 c113 110.5(9) . . . no
c112 c11 c113 107.2(9) . . . no
c3 c31 c311 109.2(10) . . . no
c3 c31 c312 108.4(9) . . . no
c3 c31 c313 111.7(9) . . . no
c311 c31 c312 108.9(10) . . . no
c311 c31 c313 110.2(9) . . . no
c312 c31 c313 108.4(10) . . . no
c4 c41 c411 112.5(9) . . . no
c4 c41 c412 108.6(10) . . . no
c4 c41 c413 109.6(9) . . . no
c411 c41 c412 110.2(9) . . . no
c411 c41 c413 108.5(10) . . . no
c412 c41 c413 107.4(9) . . . no
c5 c51 c511 110.7(9) . . . no
c5 c51 c512 109.7(10) . . . no
c5 c51 c513 110.2(9) . . . no
c511 c51 c512 108.7(9) . . . no
c511 c51 c513 108.4(9) . . . no
c512 c51 c513 109.2(10) . . . no
c1 c1l h1l1 109.00 . . . no
c1 c1l h1l2 109.00 . . . no
c1 c1l h1l3 109.00 . . . no
h1l1 c1l h1l2 109.00 . . . no
h1l1 c1l h1l3 110.00 . . . no
h1l2 c1l h1l3 109.00 . . . no
p1 c5 h5a 103.00 . . . no
p5 c5 h5a 103.00 . . . no
c51 c5 h5a 103.00 . . . no
c11 c111 h11a 109.00 . . . no
c11 c111 h11b 109.00 . . . no
c11 c111 h11c 109.00 . . . no
h11a c111 h11b 110.00 . . . no
h11a c111 h11c 109.00 . . . no
h11b c111 h11c 110.00 . . . no
c11 c112 h11d 109.00 . . . no
c11 c112 h11e 110.00 . . . no
c11 c112 h11f 109.00 . . . no
h11d c112 h11e 109.00 . . . no
h11d c112 h11f 109.00 . . . no
h11e c112 h11f 109.00 . . . no
c11 c113 h11g 110.00 . . . no
c11 c113 h11h 110.00 . . . no
c11 c113 h11i 110.00 . . . no
h11g c113 h11h 109.00 . . . no
h11g c113 h11i 109.00 . . . no
h11h c113 h11i 109.00 . . . no
c31 c311 h31a 109.00 . . . no
c31 c311 h31b 110.00 . . . no
c31 c311 h31c 109.00 . . . no
h31a c311 h31b 110.00 . . . no
h31a c311 h31c 109.00 . . . no
h31b c311 h31c 109.00 . . . no
c31 c312 h31d 110.00 . . . no
c31 c312 h31e 110.00 . . . no
c31 c312 h31f 110.00 . . . no
h31d c312 h31e 109.00 . . . no
h31d c312 h31f 110.00 . . . no
h31e c312 h31f 109.00 . . . no
c31 c313 h31g 110.00 . . . no
c31 c313 h31h 109.00 . . . no
c31 c313 h31i 110.00 . . . no
h31g c313 h31h 109.00 . . . no
h31g c313 h31i 109.00 . . . no
h31h c313 h31i 109.00 . . . no
c41 c411 h41a 109.00 . . . no
c41 c411 h41b 109.00 . . . no
c41 c411 h41c 109.00 . . . no
h41a c411 h41b 109.00 . . . no
h41a c411 h41c 109.00 . . . no
h41b c411 h41c 110.00 . . . no
c41 c412 h41d 109.00 . . . no
c41 c412 h41e 109.00 . . . no
c41 c412 h41f 110.00 . . . no
h41d c412 h41e 109.00 . . . no
h41d c412 h41f 109.00 . . . no
h41e c412 h41f 109.00 . . . no
c41 c413 h41g 109.00 . . . no
c41 c413 h41h 110.00 . . . no
c41 c413 h41i 110.00 . . . no
h41g c413 h41h 109.00 . . . no
h41g c413 h41i 109.00 . . . no
h41h c413 h41i 110.00 . . . no
c51 c511 h51a 110.00 . . . no
c51 c511 h51b 110.00 . . . no
c51 c511 h51c 109.00 . . . no
h51a c511 h51b 109.00 . . . no
h51a c511 h51c 110.00 . . . no
h51b c511 h51c 109.00 . . . no
c51 c512 h51d 109.00 . . . no
c51 c512 h51e 109.00 . . . no
c51 c512 h51f 109.00 . . . no
h51d c512 h51e 109.00 . . . no
h51d c512 h51f 110.00 . . . no
h51e c512 h51f 109.00 . . . no
c51 c513 h51g 110.00 . . . no
c51 c513 h51h 109.00 . . . no
c51 c513 h51i 109.00 . . . no
h51g c513 h51h 109.00 . . . no
h51g c513 h51i 109.00 . . . no
h51h c513 h51i 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
cu2 i1 cu1 i3 -135.30(6) . . . . no
cu2 i1 cu1 i3 -52.82(7) 2_665 . . . no
cu2 i1 cu1 p1 1.42(12) . . . . no
cu2 i1 cu1 p1 83.90(12) 2_665 . . . no
cu2 i1 cu1 i2 111.56(6) . . . 2_666 no
cu2 i1 cu1 i2 -165.95(5) 2_665 . . 2_666 no
cu2 i1 cu2 n1 -111.3(3) 2_665 2_665 . . no
cu2 i1 cu2 i1 0.00(6) 2_665 . . 2_665 no
cu1 i1 cu2 i1 97.06(6) 2_665 2_665 . . no
cu2 i1 cu2 i1 0.00(6) 2_665 2_665 . . no
cu1 i1 cu2 p2 -151.37(10) 2_665 2_665 . . no
cu2 i1 cu2 p2 111.57(11) 2_665 2_665 . . no
cu1 i1 cu2 n1 -14.2(3) 2_665 2_665 . . no
cu2 i1 cu2 n1 111.0(3) 2_665 . . . no
cu1 i1 cu2 i1 108.72(6) . . . 2_665 no
cu2 i1 cu2 p2 -123.98(12) 2_665 . . . no
cu1 i1 cu2 n1 -140.3(3) . . . . no
cu1 i1 cu2 p2 -15.27(12) . . . . no
cu3 i2 cu3 i3 114.10(7) 2_666 . . . no
cu1 i2 cu3 i2 62.18(5) 2_666 . . 2_666 no
cu3 i2 cu1 i3 114.92(6) 2_666 2_666 . . no
cu3 i2 cu1 p1 -107.13(9) . 2_666 . . no
cu1 i2 cu3 i3 176.28(7) 2_666 . . . no
cu3 i2 cu1 p1 -20.67(9) 2_666 2_666 . . no
cu3 i2 cu3 i2 0.00(6) 2_666 . . 2_666 no
cu3 i2 cu1 i1 143.87(7) . 2_666 . . no
cu3 i2 cu1 i1 -129.67(6) 2_666 2_666 . . no
cu3 i2 cu1 i3 28.47(5) . 2_666 . . no
cu3 i2 cu3 p3 -102.05(11) 2_666 . . 2_666 no
cu1 i2 cu3 p3 -162.03(10) . 2_666 . 2_666 no
cu3 i2 cu3 i2 0.00(5) 2_666 2_666 . . no
cu1 i2 cu3 p3 -39.87(11) 2_666 . . 2_666 no
cu1 i2 cu3 i2 90.96(6) . 2_666 . . no
cu3 i2 cu3 i3 -120.78(6) 2_666 2_666 . . no
cu1 i2 cu3 i3 -29.83(5) . 2_666 . . no
cu1 i3 cu3 i2 30.63(5) . . . 2_666 no
cu1 i3 cu3 p3 149.00(13) . . . 2_666 no
cu3 i3 cu1 p1 94.17(12) . . . . no
cu3 i3 cu1 i2 -29.47(5) . . . 2_666 no
cu3 i3 cu1 i1 -141.06(7) . . . . no
cu1 i3 cu3 i2 -74.25(7) . . . . no
i2 cu1 p1 p2 -95.23(18) 2_666 . . . no
i2 cu1 p1 p3 -3.87(15) 2_666 . . . no
i3 cu1 p1 c5 3.4(5) . . . . no
i3 cu1 p1 p3 -127.85(14) . . . . no
i1 cu1 p1 p2 13.8(2) . . . . no
i1 cu1 p1 p3 105.10(13) . . . . no
i2 cu1 p1 c5 127.4(5) 2_666 . . . no
i3 cu1 p1 p2 140.80(16) . . . . no
i1 cu1 p1 c5 -123.7(5) . . . . no
i1 cu2 p2 c2 -80.8(4) . . . . no
i1 cu2 p2 p1 25.2(2) . . . . no
i1 cu2 p2 c2 169.1(4) 2_665 . . . no
i1 cu2 p2 c4 44.3(5) 2_665 . . . no
i1 cu2 p2 c4 154.5(5) . . . . no
n1 cu2 p2 p1 142.6(4) . . . . no
n1 cu2 p2 c2 36.7(5) . . . . no
n1 cu2 p2 c4 -88.1(6) . . . . no
i1 cu2 p2 p1 -84.96(18) 2_665 . . . no
i2 cu3 p3 p1 47.33(14) . . 2_666 2_666 no
i2 cu3 p3 c2 -55.1(5) . . 2_666 2_666 no
i2 cu3 p3 c3 165.4(5) . . 2_666 2_666 no
i3 cu3 p3 p1 -171.90(11) . . 2_666 2_666 no
i3 cu3 p3 c2 85.7(5) . . 2_666 2_666 no
i3 cu3 p3 c3 -53.9(6) . . 2_666 2_666 no
cu1 p1 p2 cu2 -27.2(3) . . . . no
cu1 p1 p2 c2 102.6(4) . . . . no
cu1 p1 p2 c4 -170.3(4) . . . . no
p3 p1 p2 cu2 -140.09(17) . . . . no
p3 p1 p2 c2 -10.4(3) . . . . no
p3 p1 p2 c4 76.8(4) . . . . no
c5 p1 p2 cu2 124.4(4) . . . . no
c5 p1 p2 c2 -105.9(5) . . . . no
c5 p1 p2 c4 -18.7(5) . . . . no
cu1 p1 p3 c2 -102.4(3) . . . . no
cu1 p1 p3 c3 171.6(3) . . . . no
cu1 p1 p3 cu3 32.50(17) . . . 2_666 no
p2 p1 p3 c2 10.3(3) . . . . no
p2 p1 p3 c3 -75.8(3) . . . . no
p2 p1 p3 cu3 145.11(14) . . . 2_666 no
c5 p1 p3 c2 109.3(4) . . . . no
c5 p1 p3 c3 23.2(4) . . . . no
c5 p1 p3 cu3 -115.9(3) . . . 2_666 no
cu1 p1 c5 p5 177.8(2) . . . . no
cu1 p1 c5 c51 37.7(10) . . . . no
p2 p1 c5 p5 36.6(5) . . . . no
p2 p1 c5 c51 -103.4(7) . . . . no
p3 p1 c5 p5 -45.9(5) . . . . no
p3 p1 c5 c51 174.1(7) . . . . no
cu2 p2 c2 p3 129.3(3) . . . . no
cu2 p2 c2 p4 -136.4(3) . . . . no
cu2 p2 c2 c11 -6.5(10) . . . . no
p1 p2 c2 p3 11.9(4) . . . . no
p1 p2 c2 p4 106.3(3) . . . . no
p1 p2 c2 c11 -123.8(8) . . . . no
c4 p2 c2 p3 -89.5(5) . . . . no
c4 p2 c2 p4 4.9(4) . . . . no
c4 p2 c2 c11 134.8(9) . . . . no
cu2 p2 c4 p4 134.2(3) . . . . no
cu2 p2 c4 p5 -137.3(4) . . . . no
cu2 p2 c4 c41 10.3(13) . . . . no
p1 p2 c4 p4 -92.6(4) . . . . no
p1 p2 c4 p5 -4.1(6) . . . . no
p1 p2 c4 c41 143.5(10) . . . . no
c2 p2 c4 p4 -4.7(4) . . . . no
c2 p2 c4 p5 83.9(6) . . . . no
c2 p2 c4 c41 -128.6(10) . . . . no
p1 p3 c2 p2 -12.1(4) . . . . no
p1 p3 c2 p4 -107.3(4) . . . . no
p1 p3 c2 c11 125.2(8) . . . . no
c3 p3 c2 p2 87.8(5) . . . . no
c3 p3 c2 p4 -7.4(5) . . . . no
c3 p3 c2 c11 -134.9(9) . . . . no
cu3 p3 c2 p2 -120.7(4) 2_666 . . . no
cu3 p3 c2 p4 144.2(3) 2_666 . . . no
cu3 p3 c2 c11 16.6(11) 2_666 . . . no
p1 p3 c3 p4 95.8(4) . . . . no
p1 p3 c3 p5 4.2(5) . . . . no
p1 p3 c3 c31 -139.0(9) . . . . no
c2 p3 c3 p4 7.2(5) . . . . no
c2 p3 c3 p5 -84.4(6) . . . . no
c2 p3 c3 c31 132.4(10) . . . . no
cu3 p3 c3 p4 -144.6(3) 2_666 . . . no
cu3 p3 c3 p5 123.8(4) 2_666 . . . no
cu3 p3 c3 c31 -19.4(12) 2_666 . . . no
c3 p4 c2 p2 -91.7(5) . . . . no
c3 p4 c2 p3 7.3(5) . . . . no
c3 p4 c2 c11 135.7(8) . . . . no
c4 p4 c2 p2 -4.7(4) . . . . no
c4 p4 c2 p3 94.4(5) . . . . no
c4 p4 c2 c11 -137.3(8) . . . . no
c2 p4 c3 p3 -7.3(5) . . . . no
c2 p4 c3 p5 104.2(5) . . . . no
c2 p4 c3 c31 -133.0(9) . . . . no
c4 p4 c3 p3 -92.3(5) . . . . no
c4 p4 c3 p5 19.2(4) . . . . no
c4 p4 c3 c31 142.1(9) . . . . no
c2 p4 c4 p2 4.8(4) . . . . no
c2 p4 c4 p5 -105.8(4) . . . . no
c2 p4 c4 c41 134.4(8) . . . . no
c3 p4 c4 p2 91.8(5) . . . . no
c3 p4 c4 p5 -18.7(4) . . . . no
c3 p4 c4 c41 -138.6(8) . . . . no
c4 p5 c3 p3 73.3(5) . . . . no
c4 p5 c3 p4 -19.5(4) . . . . no
c4 p5 c3 c31 -143.0(8) . . . . no
c5 p5 c3 p3 -30.6(6) . . . . no
c5 p5 c3 p4 -123.4(4) . . . . no
c5 p5 c3 c31 113.2(8) . . . . no
c3 p5 c4 p2 -73.1(6) . . . . no
c3 p5 c4 p4 19.0(4) . . . . no
c3 p5 c4 c41 137.4(9) . . . . no
c5 p5 c4 p2 26.2(7) . . . . no
c5 p5 c4 p4 118.3(5) . . . . no
c5 p5 c4 c41 -123.4(9) . . . . no
c3 p5 c5 p1 49.9(6) . . . . no
c3 p5 c5 c51 -172.6(8) . . . . no
c4 p5 c5 p1 -40.9(7) . . . . no
c4 p5 c5 c51 96.7(9) . . . . no
p2 c2 c11 c111 57.9(11) . . . . no
p2 c2 c11 c112 -64.4(11) . . . . no
p2 c2 c11 c113 180.0(7) . . . . no
p3 c2 c11 c111 -68.8(11) . . . . no
p3 c2 c11 c112 168.9(7) . . . . no
p3 c2 c11 c113 53.3(11) . . . . no
p4 c2 c11 c111 176.5(7) . . . . no
p4 c2 c11 c112 54.2(11) . . . . no
p4 c2 c11 c113 -61.4(10) . . . . no
p3 c3 c31 c311 66.4(12) . . . . no
p3 c3 c31 c312 -52.1(11) . . . . no
p3 c3 c31 c313 -171.4(8) . . . . no
p4 c3 c31 c311 177.7(8) . . . . no
p4 c3 c31 c312 59.3(11) . . . . no
p4 c3 c31 c313 -60.1(13) . . . . no
p5 c3 c31 c311 -74.5(11) . . . . no
p5 c3 c31 c312 167.1(7) . . . . no
p5 c3 c31 c313 47.7(12) . . . . no
p2 c4 c41 c411 170.5(9) . . . . no
p2 c4 c41 c412 48.3(14) . . . . no
p2 c4 c41 c413 -68.7(12) . . . . no
p4 c4 c41 c411 57.7(12) . . . . no
p4 c4 c41 c412 -64.5(10) . . . . no
p4 c4 c41 c413 178.5(7) . . . . no
p5 c4 c41 c411 -44.2(14) . . . . no
p5 c4 c41 c412 -166.3(8) . . . . no
p5 c4 c41 c413 76.7(10) . . . . no
p1 c5 c51 c511 164.3(7) . . . . no
p1 c5 c51 c512 44.3(11) . . . . no
p1 c5 c51 c513 -75.9(10) . . . . no
p5 c5 c51 c511 29.4(12) . . . . no
p5 c5 c51 c512 -90.6(10) . . . . no
p5 c5 c51 c513 149.2(8) . . . . 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
i1 p1 3.880(3) . . no
i1 p2 3.886(3) . . no
i1 i1 4.1312(14) . 2_665 no
i2 i2 3.9653(13) . 2_666 no
i2 p3 3.856(3) . . no
i2 cu1 4.0195(18) . . no
i2 p1 3.890(3) . . no
i2 p3 3.970(3) . 2_666 no
i3 c1l 3.840(12) . 2_665 no
i3 c1 3.726(14) . 2_665 no
i1 h11a 3.3200 . . no
i1 h41g 3.0100 . 2_665 no
i2 h31a 3.2000 . . no
i2 h11c 2.9800 . 2_666 no
i3 h51i 3.1300 . . no
i3 h1l3 3.1500 . 2_665 no
i3 h31f 3.2200 . 2_666 no
i3 h51h 3.3600 . 2_566 no
cu1 i2 4.0195(18) . . no
cu1 c512 4.114(11) . . no
cu1 c513 4.168(11) . . no
cu2 c112 4.098(12) . . no
cu2 c412 3.882(10) . . no
cu2 c111 3.900(11) . . no
cu2 c413 4.117(10) . . no
cu3 c312 4.066(10) . 2_666 no
cu3 c311 4.030(9) . 2_666 no
cu3 c113 4.125(11) . 2_666 no
cu3 c111 4.194(9) . 2_666 no
cu1 h51i 3.3200 . . no
cu1 h51d 3.2500 . . no
cu2 h51d 3.6800 . 2_665 no
cu2 h11d 3.3000 . . no
cu2 h41g 3.2900 . . no
cu2 h11a 3.0300 . . no
cu2 h41d 2.9900 . . no
cu3 h1l2 3.6200 . 1_456 no
cu3 h11c 3.3500 . 2_666 no
cu3 h11i 3.2700 . 2_666 no
cu3 h31a 3.1600 . 2_666 no
cu3 h31f 3.2000 . 2_666 no
p1 i1 3.880(3) . . no
p1 cu2 3.712(3) . . no
p1 cu3 4.264(3) . . no
p1 cu3 3.504(4) . 2_666 no
p2 i1 3.886(3) . . no
p2 cu1 3.768(3) . . no
p3 i2 3.856(3) . . no
p1 h51i 3.0800 . . no
p1 h51d 2.6600 . . no
p2 h11a 3.0400 . . no
p2 h41d 2.8100 . . no
p2 h41g 3.0700 . . no
p2 h11d 3.0700 . . no
p3 h11c 3.1100 . . no
p3 h11i 2.8600 . . no
p3 h31a 2.9800 . . no
p3 h31f 2.7900 . . no
p4 h11e 2.7500 . . no
p4 h11h 2.9200 . . no
p4 h31d 2.9100 . . no
p4 h31g 2.9800 . . no
p4 h41b 2.9000 . . no
p4 h41f 2.9100 . . no
p5 h31c 3.0800 . . no
p5 h31h 2.8200 . . no
p5 h41a 2.8100 . . no
p5 h41h 3.1300 . . no
p5 h51a 3.1800 . . no
p5 h51b 2.7900 . . no
n1 h11d 2.6700 . . no
c1 i3 3.726(14) . 2_665 no
c1 c512 3.567(17) . 2_665 no
c1l i3 3.840(12) . 2_665 no
c1l c513 3.454(14) . 1_654 no
c1 h11d 2.8700 . . no
c1 h51d 3.0900 . 2_665 no
c1l h51g 3.0800 . 1_654 no
c111 cu2 3.900(11) . . no
c111 cu3 4.194(9) . 2_666 no
c112 cu2 4.098(12) . . no
c113 cu3 4.125(11) . 2_666 no
c111 h11b 2.9600 . 2_765 no
c113 h51e 2.9900 . 1_655 no
c113 h1l2 2.9600 . 2_765 no
c311 cu3 4.030(9) . 2_666 no
c312 cu3 4.066(10) . 2_666 no
c412 cu2 3.882(10) . . no
c413 cu2 4.117(10) . . no
c411 h11h 3.0600 . 2_755 no
c512 c1 3.567(17) . 2_665 no
c512 cu1 4.114(11) . . no
c413 h41h 3.0300 . 2_655 no
c413 h51f 2.7300 . . no
c513 cu1 4.168(11) . . no
c513 c1l 3.454(14) . 1_456 no
c513 h1l1 3.0900 . 1_456 no
c513 h1l3 2.9400 . 1_456 no
h1l1 c513 3.0900 . 1_654 no
h1l1 h51g 2.4900 . 1_654 no
h1l2 cu3 3.6200 . 1_654 no
h1l2 c113 2.9600 . 2_765 no
h1l2 h11i 2.4300 . 2_765 no
h1l3 c513 2.9400 . 1_654 no
h1l3 i3 3.1500 . 2_665 no
h5a h51g 2.2800 . . no
h11a i1 3.3200 . . no
h11a cu2 3.0300 . . no
h11a p2 3.0400 . . no
h11a h11d 2.5100 . . no
h11b h11f 2.5600 . . no
h11b h11g 2.4900 . . no
h11b c111 2.9600 . 2_765 no
h11b h11b 2.2300 . 2_765 no
h11c p3 3.1100 . . no
h11c h11i 2.5600 . . no
h11c i2 2.9800 . 2_666 no
h11c cu3 3.3500 . 2_666 no
h11d cu2 3.3000 . . no
h11d p2 3.0700 . . no
h11d n1 2.6700 . . no
h11d c1 2.8700 . . no
h11d h11a 2.5100 . . no
h11e p4 2.7500 . . no
h11e h11h 2.4600 . . no
h11e h41b 2.4800 . 2_755 no
h11f h11b 2.5600 . . no
h11f h11g 2.5000 . . no
h11g h11b 2.4900 . . no
h11g h11f 2.5000 . . no
h11g h51e 2.3100 . 1_655 no
h11h p4 2.9200 . . no
h11h h11e 2.4600 . . no
h11h c411 3.0600 . 2_755 no
h11h h41c 2.5600 . 2_755 no
h11i p3 2.8600 . . no
h11i h11c 2.5600 . . no
h11i cu3 3.2700 . 2_666 no
h11i h1l2 2.4300 . 2_765 no
h31a i2 3.2000 . . no
h31a p3 2.9800 . . no
h31a h31f 2.5100 . . no
h31a cu3 3.1600 . 2_666 no
h31b h31e 2.5000 . . no
h31b h31i 2.5000 . . no
h31b h51a 2.5000 . 2_656 no
h31c p5 3.0800 . . no
h31c h31h 2.5500 . . no
h31c h31c 2.5200 . 2_656 no
h31d p4 2.9100 . . no
h31d h31g 2.5000 . . no
h31e h31b 2.5000 . . no
h31e h31i 2.5200 . . no
h31f p3 2.7900 . . no
h31f h31a 2.5100 . . no
h31f i3 3.2200 . 2_666 no
h31f cu3 3.2000 . 2_666 no
h31g p4 2.9800 . . no
h31g h31d 2.5000 . . no
h31h p5 2.8200 . . no
h31h h31c 2.5500 . . no
h31i h31b 2.5000 . . no
h31i h31e 2.5200 . . no
h41a p5 2.8100 . . no
h41a h41h 2.5000 . . no
h41b p4 2.9000 . . no
h41b h41f 2.5500 . . no
h41b h11e 2.4800 . 2_755 no
h41c h41e 2.5200 . . no
h41c h41i 2.4700 . . no
h41c h11h 2.5600 . 2_755 no
h41d cu2 2.9900 . . no
h41d p2 2.8100 . . no
h41d h41g 2.4700 . . no
h41e h41c 2.5200 . . no
h41e h41i 2.4400 . . no
h41f p4 2.9100 . . no
h41f h41b 2.5500 . . no
h41g cu2 3.2900 . . no
h41g p2 3.0700 . . no
h41g h41d 2.4700 . . no
h41g h51f 2.3500 . . no
h41g i1 3.0100 . 2_665 no
h41h p5 3.1300 . . no
h41h h41a 2.5000 . . no
h41h h51b 2.4800 . . no
h41h h51f 2.2900 . . no
h41h c413 3.0300 . 2_655 no
h41h h41i 2.5600 . 2_655 no
h41i h41c 2.4700 . . no
h41i h41e 2.4400 . . no
h41i h41h 2.5600 . 2_655 no
h41i h51b 2.5700 . 2_655 no
h51a p5 3.1800 . . no
h51a h51g 2.5000 . . no
h51a h31b 2.5000 . 2_656 no
h51b p5 2.7900 . . no
h51b h41h 2.4800 . . no
h51b h51f 2.4800 . . no
h51b h41i 2.5700 . 2_655 no
h51c h51e 2.4900 . . no
h51c h51h 2.4300 . . no
h51d cu1 3.2500 . . no
h51d p1 2.6600 . . no
h51d h51i 2.5000 . . no
h51d cu2 3.6800 . 2_665 no
h51d c1 3.0900 . 2_665 no
h51e c113 2.9900 . 1_455 no
h51e h11g 2.3100 . 1_455 no
h51e h51c 2.4900 . . no
h51e h51h 2.4700 . . no
h51f c413 2.7300 . . no
h51f h41g 2.3500 . . no
h51f h41h 2.2900 . . no
h51f h51b 2.4800 . . no
h51g c1l 3.0800 . 1_456 no
h51g h1l1 2.4900 . 1_456 no
h51g h5a 2.2800 . . no
h51g h51a 2.5000 . . no
h51h h51c 2.4300 . . no
h51h h51e 2.4700 . . no
h51h i3 3.3600 . 2_566 no
h51i i3 3.1300 . . no
h51i cu1 3.3200 . . no
h51i p1 3.0800 . . no
h51i h51d 2.5000 . . 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
#
#d h a d - h h...a d...a d - h...a symm(a)
#
c111 h11c i2 0.9800 2.9800 3.909(9) 158.00 2_666 yes
c112 h11e p4 0.9800 2.7500 3.237(11) 111.00 . yes
c313 h31h p5 0.9800 2.8200 3.237(12) 107.00 . yes
c411 h41a p5 0.9800 2.8100 3.230(11) 107.00 . yes
c413 h41g i1 0.9800 3.0100 3.962(9) 166.00 2_665 yes
c511 h51b p5 0.9800 2.7900 3.140(12) 102.00 . yes
# loop mechanism for extra tables(s)
#loop_
#_publ_manuscript_incl_extra_item
#'_geom_extra_tablea_col_1'
#'_geom_extra_tablea_col_2'
#'_geom_extra_tablea_col_3'
#'_geom_extra_table_head_a'
#'_geom_table_footnote_a'
#'_geom_extra_tableb_col_1'
#'_geom_extra_tableb_col_2'
#'_geom_extra_tableb_col_3'
#'_geom_extra_table_head_b'
#'_geom_table_footnote_b'
#
#loop_
#_geom_extra_tablea_col_1
#_geom_extra_tablea_col_2
#_geom_extra_tablea_col_3
# ? ? ?
#
#loop_
#_geom_extra_tableb_col_1
#_geom_extra_tableb_col_2
#_geom_extra_tableb_col_3
# ? ? ?
#
#_geom_table_footnote_a
#;
# ?
#;
#
#_geom_table_footnote_b
#;
# ?
#;
#
#_geom_table_footnote_a
#;
# ?
#;
#
#_geom_table_footnote_b
#;
# ?
#;
#===end
# Attachment 'compound3.cif'
# CIF-file generated for u512_neu R = 0.04
#==============================================================================
#===============================================================================
data_u512_neu
_database_code_depnum_ccdc_archive 'CCDC 656702'
# 0. AUDIT DETAILS
_audit_creation_date 'Apr 13 16:08:54 2007'
_audit_creation_method 'PLATON option'
_audit_update_record
;
;
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C44 H78 Cu4 I4 N2 P8'
# 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 'C22 H39 Cu2 I2 N P4'
_chemical_formula_iupac ?
_chemical_formula_weight 1644.64
_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
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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 0.0181 0.0091 '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_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,1/2-z
3 -x,-y,-z
4 x,1/2-y,1/2+z
_cell_length_a 15.505(3)
_cell_length_b 11.6415(18)
_cell_length_c 18.001(3)
_cell_angle_alpha 90
_cell_angle_beta 111.426(18)
_cell_angle_gamma 90
_cell_volume 3024.7(10)
_cell_formula_units_Z 2
_cell_measurement_temperature 104(1)
_cell_measurement_reflns_used 6773
_cell_measurement_theta_min 2.6216
_cell_measurement_theta_max 51.2281
_cell_special_details
;
;
_exptl_crystal_description plate
_exptl_crystal_colour red
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.04
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.806
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 1608
_exptl_absorpt_coefficient_mu 19.841
_exptl_crystal_density_meas_temp ?
# Permitted for _exptl_absorpt_correction_type :
# 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 multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
(compiled May 12 2006,14:43:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min 0.49020
_exptl_absorpt_correction_T_max 1.39953
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
;
_diffrn_ambient_temperature 104(1)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method omega-scan
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -28.00 23.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 0.1529 45.0000 120.0000 0.0000 0.0000 51
#__ type_ start__ end____ width___ exp.time_
2 omega -28.00 23.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 0.1529 45.0000 0.0000 0.0000 0.0000 51
#__ type_ start__ end____ width___ exp.time_
3 omega 23.00 78.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 0.1529 75.0000 120.0000 0.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
4 omega 25.00 77.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 0.1529 35.0000 -149.0000 0.0000 0.0000 52
#__ type_ start__ end____ width___ exp.time_
5 omega -83.00 -28.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -72.0000 257.0000 0.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
6 omega -89.00 -38.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 45.0000 240.0000 0.0000 0.0000 51
#__ type_ start__ end____ width___ exp.time_
7 omega -108.00 -56.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 108.0000 217.0000 0.0000 0.0000 52
#__ type_ start__ end____ width___ exp.time_
8 omega -139.00 -84.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -75.0000 240.0000 0.0000 0.0000 55
#__ type_ start__ end____ width___ exp.time_
9 omega -83.00 -30.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -65.0000 60.0000 0.0000 0.0000 53
#__ type_ start__ end____ width___ exp.time_
10 omega -70.00 -29.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -60.8272 -69.0000 159.0000 0.0000 0.0000 41
#__ type_ start__ end____ width___ exp.time_
11 omega 86.00 137.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 45.0000 0.0000 0.0000 0.0000 51
#__ type_ start__ end____ width___ exp.time_
12 omega 39.00 90.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 -45.0000 240.0000 0.0000 0.0000 51
#__ type_ start__ end____ width___ exp.time_
13 omega 35.00 63.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 35.0000 30.0000 0.0000 0.0000 28
#__ type_ start__ end____ width___ exp.time_
14 omega 41.00 84.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 67.0000 183.0000 0.0000 0.0000 43
#__ type_ start__ end____ width___ exp.time_
15 omega -12.00 38.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 -35.0000 149.0000 0.0000 0.0000 50
#__ type_ start__ end____ width___ exp.time_
16 omega 86.00 137.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 45.0000 240.0000 0.0000 0.0000 51
#__ type_ start__ end____ width___ exp.time_
17 omega 43.00 90.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 -35.0000 149.0000 0.0000 0.0000 47
#__ type_ start__ end____ width___ exp.time_
18 omega 85.00 136.00 1.0000 34.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 62.4840 55.0000 110.0000 0.0000 0.0000 51
;
_diffrn_detector_area_resol_mean 10.5431
_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 13212
_diffrn_reflns_av_R_equivalents 0.0466
_diffrn_reflns_av_sigmaI/netI 0.0449
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 3.06
_diffrn_reflns_theta_max 51.53
_diffrn_reflns_theta_full 51.53
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_reduction_process
;
;
# number of unique reflections
_reflns_number_total 3267
# number of observed reflections (> n sig(I))
_reflns_number_gt 2433
_reflns_threshold_expression I>2\s(I)
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_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^)+(0.0713P)^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 3267
_refine_ls_number_parameters 293
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0536
_refine_ls_R_factor_gt 0.0391
_refine_ls_wR_factor_ref 0.1000
_refine_ls_wR_factor_gt 0.0963
_refine_ls_goodness_of_fit_ref 0.937
_refine_ls_restrained_S_all 0.937
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.941
_refine_diff_density_min -0.657
_refine_diff_density_rms 0.120
#===============================================================================
# 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
I1 I Uani 0.88461(4) 0.71574(5) 0.03083(4) 1.000 0.0478(2) . .
I2 I Uani 0.96547(3) 1.06967(5) 0.08734(3) 1.000 0.0430(2) . .
Cu1 Cu Uani 1.00529(8) 0.84611(11) 0.13498(8) 1.000 0.0494(5) . .
Cu2 Cu Uani 0.89483(8) 0.91280(10) -0.03188(8) 1.000 0.0483(5) . .
P1 P Uani 1.15336(15) 0.84045(19) 0.14572(15) 1.000 0.0462(9) . .
P2 P Uani 0.77742(14) 1.00649(19) -0.12515(14) 1.000 0.0424(8) . .
P3 P Uani 0.59568(17) 0.9568(2) -0.19219(17) 1.000 0.0613(10) . .
P4 P Uani 1.35965(15) 0.8160(2) 0.19037(15) 1.000 0.0482(9) . .
N1 N Uani 0.9976(5) 0.8496(6) 0.2444(5) 1.000 0.048(3) . .
C1 C Uani 1.2464(5) 0.7527(7) 0.1827(5) 1.000 0.042(3) . .
C2 C Uani 0.6728(5) 1.0685(7) -0.1154(5) 1.000 0.047(3) . .
C3 C Uani 0.6978(6) 0.9641(8) -0.2269(6) 1.000 0.061(4) . .
C4 C Uani 0.6222(6) 1.0603(8) -0.2624(6) 1.000 0.054(3) . .
C5 C Uani 1.2372(6) 0.6273(8) 0.2027(6) 1.000 0.051(4) . .
C6 C Uani 1.2214(7) 0.5586(8) 0.1265(6) 1.000 0.077(5) . .
C7 C Uani 1.3264(6) 0.5823(8) 0.2676(6) 1.000 0.066(4) . .
C8 C Uani 1.1582(6) 0.6091(8) 0.2323(6) 1.000 0.070(4) . .
C9 C Uani 0.6585(6) 1.0839(8) -0.0374(6) 1.000 0.051(4) . .
C10 C Uani 0.6877(6) 0.9769(9) 0.0149(6) 1.000 0.065(4) . .
C11 C Uani 0.5541(5) 1.1088(9) -0.0543(6) 1.000 0.069(4) . .
C12 C Uani 0.7155(6) 1.1904(9) 0.0059(6) 1.000 0.063(4) . .
C13 C Uani 0.7334(6) 0.8714(8) -0.2696(6) 1.000 0.056(4) . .
C14 C Uani 0.7737(7) 0.7713(8) -0.2111(6) 1.000 0.066(4) . .
C15 C Uani 0.8135(6) 0.9228(8) -0.2912(6) 1.000 0.071(4) . .
C16 C Uani 0.6625(6) 0.8145(8) -0.3443(6) 1.000 0.075(4) . .
C17 C Uani 0.5529(6) 1.0808(8) -0.3486(6) 1.000 0.060(4) . .
C18 C Uani 0.4934(7) 1.1822(10) -0.3506(6) 1.000 0.093(5) . .
C19 C Uani 0.4841(6) 0.9799(9) -0.3821(6) 1.000 0.079(4) . .
C20 C Uani 0.6078(8) 1.1056(9) -0.4009(6) 1.000 0.082(5) . .
C100 C Uani 1.0109(6) 0.8664(8) 0.3078(7) 1.000 0.046(3) . .
C101 C Uani 1.0288(6) 0.8897(8) 0.3905(6) 1.000 0.067(4) . .
H6A H Uiso 1.22650 0.47630 0.13900 1.000 0.1150 calc R
H6B H Uiso 1.26810 0.58000 0.10420 1.000 0.1150 calc R
H6C H Uiso 1.15940 0.57520 0.08750 1.000 0.1150 calc R
H7A H Uiso 1.31890 0.50080 0.27750 1.000 0.0980 calc R
H7B H Uiso 1.33850 0.62600 0.31690 1.000 0.0980 calc R
H7C H Uiso 1.37860 0.59160 0.24960 1.000 0.0980 calc R
H8A H Uiso 1.15690 0.52860 0.24760 1.000 0.1050 calc R
H8B H Uiso 1.09930 0.62870 0.18970 1.000 0.1050 calc R
H8C H Uiso 1.16730 0.65850 0.27870 1.000 0.1050 calc R
H10A H Uiso 0.67350 0.98750 0.06330 1.000 0.0980 calc R
H10B H Uiso 0.75440 0.96460 0.02980 1.000 0.0980 calc R
H10C H Uiso 0.65390 0.91000 -0.01460 1.000 0.0980 calc R
H10D H Uiso 0.97780 0.85960 0.40470 1.000 0.1010 calc R
H10E H Uiso 1.03390 0.97290 0.39960 1.000 0.1010 calc R
H10F H Uiso 1.08690 0.85260 0.42360 1.000 0.1010 calc R
H11A H Uiso 0.54500 1.11900 -0.00360 1.000 0.1040 calc R
H11B H Uiso 0.51650 1.04410 -0.08350 1.000 0.1040 calc R
H11C H Uiso 0.53540 1.17890 -0.08630 1.000 0.1040 calc R
H12A H Uiso 0.70810 1.20110 0.05720 1.000 0.0940 calc R
H12B H Uiso 0.69310 1.25890 -0.02730 1.000 0.0940 calc R
H12C H Uiso 0.78110 1.17830 0.01490 1.000 0.0940 calc R
H14A H Uiso 0.78890 0.70730 -0.23950 1.000 0.0990 calc R
H14B H Uiso 0.72790 0.74600 -0.18880 1.000 0.0990 calc R
H14C H Uiso 0.82990 0.79700 -0.16780 1.000 0.0990 calc R
H15A H Uiso 0.83910 0.86330 -0.31570 1.000 0.1080 calc R
H15B H Uiso 0.86210 0.95120 -0.24260 1.000 0.1080 calc R
H15C H Uiso 0.78980 0.98640 -0.32880 1.000 0.1080 calc R
H16A H Uiso 0.69330 0.75430 -0.36360 1.000 0.1120 calc R
H16B H Uiso 0.63690 0.87250 -0.38610 1.000 0.1120 calc R
H16C H Uiso 0.61240 0.78050 -0.33070 1.000 0.1120 calc R
H18A H Uiso 0.45850 1.16800 -0.31580 1.000 0.1390 calc R
H18B H Uiso 0.45020 1.19480 -0.40530 1.000 0.1390 calc R
H18C H Uiso 0.53250 1.25030 -0.33190 1.000 0.1390 calc R
H19A H Uiso 0.50860 0.92760 -0.41220 1.000 0.1180 calc R
H19B H Uiso 0.42410 1.01030 -0.41730 1.000 0.1180 calc R
H19C H Uiso 0.47600 0.93820 -0.33770 1.000 0.1180 calc R
H20A H Uiso 0.63430 1.03400 -0.41160 1.000 0.1240 calc R
H20B H Uiso 0.65780 1.15970 -0.37360 1.000 0.1240 calc R
H20C H Uiso 0.56690 1.13930 -0.45130 1.000 0.1240 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0545(4) 0.0368(4) 0.0556(4) 0.0023(3) 0.0242(3) -0.0044(3)
I2 0.0410(3) 0.0359(4) 0.0566(4) -0.0008(3) 0.0233(3) 0.0010(3)
Cu1 0.0465(7) 0.0457(8) 0.0617(9) 0.0026(7) 0.0267(7) -0.0016(6)
Cu2 0.0466(7) 0.0397(8) 0.0625(10) 0.0045(7) 0.0245(7) 0.0003(6)
P1 0.0426(13) 0.0378(14) 0.0638(17) 0.0041(13) 0.0260(12) -0.0004(11)
P2 0.0429(13) 0.0380(14) 0.0516(16) 0.0016(12) 0.0237(12) 0.0000(11)
P3 0.0503(15) 0.0568(17) 0.075(2) 0.0016(15) 0.0208(14) -0.0053(13)
P4 0.0420(13) 0.0491(15) 0.0550(17) 0.0013(13) 0.0195(12) -0.0001(12)
N1 0.051(5) 0.046(5) 0.055(6) 0.009(5) 0.028(5) 0.006(4)
C1 0.039(5) 0.038(5) 0.049(6) 0.004(5) 0.017(4) 0.003(4)
C2 0.035(5) 0.050(6) 0.055(6) 0.001(5) 0.015(5) 0.002(4)
C3 0.055(6) 0.046(6) 0.080(8) -0.021(6) 0.024(6) -0.006(5)
C4 0.046(5) 0.049(6) 0.055(7) -0.001(5) 0.006(5) -0.001(5)
C5 0.054(6) 0.044(6) 0.058(7) 0.006(6) 0.025(5) 0.011(5)
C6 0.107(9) 0.044(7) 0.072(8) 0.002(6) 0.025(7) -0.006(6)
C7 0.058(6) 0.054(7) 0.081(8) 0.015(6) 0.020(6) -0.001(5)
C8 0.059(6) 0.057(7) 0.101(9) 0.016(6) 0.036(6) 0.004(5)
C9 0.047(6) 0.054(6) 0.062(7) 0.016(6) 0.031(5) 0.015(5)
C10 0.061(6) 0.080(8) 0.069(7) 0.016(6) 0.040(6) 0.018(6)
C11 0.047(6) 0.085(8) 0.086(8) 0.014(7) 0.036(6) 0.013(6)
C12 0.059(6) 0.079(8) 0.050(7) -0.006(6) 0.019(5) 0.014(6)
C13 0.059(6) 0.055(7) 0.057(7) -0.010(6) 0.025(5) -0.008(5)
C14 0.074(7) 0.046(6) 0.085(8) -0.006(6) 0.037(6) 0.002(5)
C15 0.074(7) 0.075(8) 0.078(8) -0.016(6) 0.043(6) -0.011(6)
C16 0.065(7) 0.056(7) 0.090(9) -0.027(6) 0.013(6) 0.003(6)
C17 0.060(6) 0.054(7) 0.065(7) -0.005(6) 0.021(6) -0.011(6)
C18 0.088(8) 0.071(8) 0.075(9) -0.008(7) -0.022(6) 0.013(7)
C19 0.059(7) 0.070(8) 0.092(8) 0.001(7) 0.008(6) 0.001(6)
C20 0.102(8) 0.083(9) 0.055(7) 0.006(6) 0.020(7) -0.023(7)
C100 0.041(5) 0.050(6) 0.052(7) -0.001(6) 0.023(6) -0.007(5)
C101 0.085(7) 0.041(6) 0.082(9) -0.018(6) 0.038(7) -0.012(5)
#===============================================================================
# 10. MOLECULAR GEOMETRY
_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
I1 Cu1 2.5993(16) . . yes
I1 Cu2 2.5871(14) . . yes
I2 Cu1 2.7392(15) . . yes
I2 Cu2 2.7245(15) . . yes
I2 Cu2 2.7037(15) . 3_775 yes
Cu1 P1 2.233(3) . . yes
Cu1 N1 2.017(8) . . yes
Cu2 P2 2.256(3) . . yes
P1 C1 1.693(9) . . yes
P1 P2 2.180(3) . 3_775 yes
P2 C2 1.842(9) . . yes
P2 C3 1.863(10) . . yes
P3 C2 1.956(9) . . yes
P3 C3 1.905(10) . . yes
P3 C4 1.897(10) . . yes
P4 C1 1.862(9) . . yes
P4 C2 1.840(9) . 3_775 yes
P4 C4 1.889(10) . 3_775 yes
N1 C100 1.101(14) . . yes
C1 C5 1.523(12) . . no
C2 C9 1.510(13) . . no
C3 C4 1.578(14) . . no
C3 C13 1.540(14) . . no
C4 C17 1.550(14) . . no
C5 C6 1.528(14) . . no
C5 C7 1.540(14) . . no
C5 C8 1.519(14) . . no
C9 C10 1.527(14) . . no
C9 C11 1.561(13) . . no
C9 C12 1.556(14) . . no
C13 C14 1.542(14) . . no
C13 C15 1.551(14) . . no
C13 C16 1.541(14) . . no
C17 C18 1.491(15) . . no
C17 C19 1.553(14) . . no
C17 C20 1.510(16) . . no
C100 C101 1.437(15) . . no
C6 H6A 0.9800 . . no
C6 H6B 0.9800 . . no
C6 H6C 0.9800 . . no
C7 H7A 0.9800 . . no
C7 H7B 0.9800 . . no
C7 H7C 0.9800 . . no
C8 H8A 0.9800 . . no
C8 H8B 0.9800 . . no
C8 H8C 0.9800 . . no
C10 H10A 0.9800 . . no
C10 H10B 0.9800 . . no
C10 H10C 0.9800 . . no
C11 H11A 0.9800 . . no
C11 H11B 0.9800 . . no
C11 H11C 0.9800 . . no
C12 H12A 0.9800 . . no
C12 H12B 0.9800 . . no
C12 H12C 0.9800 . . no
C14 H14A 0.9800 . . no
C14 H14B 0.9800 . . no
C14 H14C 0.9800 . . no
C15 H15A 0.9800 . . no
C15 H15B 0.9800 . . no
C15 H15C 0.9800 . . no
C16 H16A 0.9800 . . no
C16 H16B 0.9800 . . no
C16 H16C 0.9800 . . no
C18 H18A 0.9800 . . no
C18 H18B 0.9800 . . no
C18 H18C 0.9800 . . no
C19 H19A 0.9800 . . no
C19 H19B 0.9800 . . no
C19 H19C 0.9800 . . no
C20 H20A 0.9800 . . no
C20 H20B 0.9800 . . no
C20 H20C 0.9800 . . no
C101 H10D 0.9800 . . no
C101 H10E 0.9800 . . no
C101 H10F 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
Cu1 I1 Cu2 69.77(5) . . . yes
Cu1 I2 Cu2 65.77(4) . . . yes
Cu1 I2 Cu2 93.90(4) . . 3_775 yes
Cu2 I2 Cu2 84.58(5) . . 3_775 yes
I1 Cu1 I2 107.96(5) . . . yes
I1 Cu1 P1 119.44(8) . . . yes
I1 Cu1 N1 115.6(2) . . . yes
I2 Cu1 P1 99.33(8) . . . yes
I2 Cu1 N1 101.5(2) . . . yes
P1 Cu1 N1 110.0(3) . . . yes
I1 Cu2 I2 108.77(5) . . . yes
I1 Cu2 P2 126.30(8) . . . yes
I1 Cu2 I2 114.40(5) . . 3_775 yes
I2 Cu2 P2 104.19(8) . . . yes
I2 Cu2 I2 95.42(5) . . 3_775 yes
I2 Cu2 P2 103.08(8) 3_775 . . yes
Cu1 P1 C1 138.9(3) . . . yes
Cu1 P1 P2 121.02(13) . . 3_775 yes
P2 P1 C1 99.1(3) 3_775 . . yes
Cu2 P2 C2 128.2(3) . . . yes
Cu2 P2 C3 132.0(3) . . . yes
Cu2 P2 P1 102.01(12) . . 3_775 yes
C2 P2 C3 84.7(4) . . . yes
P1 P2 C2 101.6(3) 3_775 . . yes
P1 P2 C3 103.9(3) 3_775 . . yes
C2 P3 C3 80.5(4) . . . yes
C2 P3 C4 79.8(4) . . . yes
C3 P3 C4 49.0(4) . . . yes
C1 P4 C2 103.7(4) . . 3_775 yes
C1 P4 C4 104.6(4) . . 3_775 yes
C2 P4 C4 83.0(4) 3_775 . 3_775 yes
Cu1 N1 C100 163.9(8) . . . yes
P1 C1 P4 115.8(5) . . . yes
P1 C1 C5 122.1(7) . . . yes
P4 C1 C5 121.9(6) . . . yes
P2 C2 P3 90.3(4) . . . yes
P2 C2 C9 124.7(6) . . . yes
P2 C2 P4 103.4(4) . . 3_775 yes
P3 C2 C9 118.5(6) . . . yes
P3 C2 P4 92.0(4) . . 3_775 yes
P4 C2 C9 120.1(6) 3_775 . . yes
P2 C3 P3 91.2(5) . . . yes
P2 C3 C4 109.7(6) . . . yes
P2 C3 C13 116.5(7) . . . yes
P3 C3 C4 65.2(5) . . . yes
P3 C3 C13 128.7(7) . . . yes
C4 C3 C13 130.1(8) . . . no
P3 C4 C3 65.7(5) . . . yes
P3 C4 C17 121.7(7) . . . yes
P3 C4 P4 92.4(5) . . 3_775 yes
C3 C4 C17 131.0(8) . . . no
P4 C4 C3 111.2(7) 3_775 . . yes
P4 C4 C17 116.4(7) 3_775 . . yes
C1 C5 C6 106.7(8) . . . no
C1 C5 C7 111.7(8) . . . no
C1 C5 C8 112.0(8) . . . no
C6 C5 C7 107.9(8) . . . no
C6 C5 C8 110.9(8) . . . no
C7 C5 C8 107.6(8) . . . no
C2 C9 C10 111.4(8) . . . no
C2 C9 C11 109.6(8) . . . no
C2 C9 C12 108.1(8) . . . no
C10 C9 C11 108.9(8) . . . no
C10 C9 C12 110.8(8) . . . no
C11 C9 C12 108.0(8) . . . no
C3 C13 C14 108.6(8) . . . no
C3 C13 C15 108.7(8) . . . no
C3 C13 C16 117.7(8) . . . no
C14 C13 C15 107.5(8) . . . no
C14 C13 C16 104.7(8) . . . no
C15 C13 C16 109.2(8) . . . no
C4 C17 C18 110.1(8) . . . no
C4 C17 C19 113.5(8) . . . no
C4 C17 C20 108.1(8) . . . no
C18 C17 C19 105.0(8) . . . no
C18 C17 C20 108.6(8) . . . no
C19 C17 C20 111.5(8) . . . no
N1 C100 C101 179.3(13) . . . yes
C5 C6 H6A 109.00 . . . no
C5 C6 H6B 110.00 . . . no
C5 C6 H6C 109.00 . . . no
H6A C6 H6B 109.00 . . . no
H6A C6 H6C 109.00 . . . no
H6B C6 H6C 110.00 . . . no
C5 C7 H7A 110.00 . . . no
C5 C7 H7B 109.00 . . . no
C5 C7 H7C 109.00 . . . no
H7A C7 H7B 110.00 . . . no
H7A C7 H7C 109.00 . . . no
H7B C7 H7C 109.00 . . . no
C5 C8 H8A 110.00 . . . no
C5 C8 H8B 109.00 . . . no
C5 C8 H8C 109.00 . . . no
H8A C8 H8B 109.00 . . . no
H8A C8 H8C 109.00 . . . no
H8B C8 H8C 109.00 . . . no
C9 C10 H10A 109.00 . . . no
C9 C10 H10B 109.00 . . . no
C9 C10 H10C 110.00 . . . no
H10A C10 H10B 109.00 . . . no
H10A C10 H10C 109.00 . . . no
H10B C10 H10C 110.00 . . . no
C9 C11 H11A 109.00 . . . no
C9 C11 H11B 109.00 . . . no
C9 C11 H11C 109.00 . . . no
H11A C11 H11B 109.00 . . . no
H11A C11 H11C 110.00 . . . no
H11B C11 H11C 110.00 . . . no
C9 C12 H12A 109.00 . . . no
C9 C12 H12B 109.00 . . . no
C9 C12 H12C 109.00 . . . no
H12A C12 H12B 109.00 . . . no
H12A C12 H12C 110.00 . . . no
H12B C12 H12C 109.00 . . . no
C13 C14 H14A 109.00 . . . no
C13 C14 H14B 109.00 . . . no
C13 C14 H14C 109.00 . . . no
H14A C14 H14B 109.00 . . . no
H14A C14 H14C 109.00 . . . no
H14B C14 H14C 109.00 . . . no
C13 C15 H15A 109.00 . . . no
C13 C15 H15B 109.00 . . . no
C13 C15 H15C 109.00 . . . no
H15A C15 H15B 110.00 . . . no
H15A C15 H15C 110.00 . . . no
H15B C15 H15C 109.00 . . . no
C13 C16 H16A 109.00 . . . no
C13 C16 H16B 109.00 . . . no
C13 C16 H16C 109.00 . . . no
H16A C16 H16B 109.00 . . . no
H16A C16 H16C 109.00 . . . no
H16B C16 H16C 110.00 . . . no
C17 C18 H18A 109.00 . . . no
C17 C18 H18B 109.00 . . . no
C17 C18 H18C 109.00 . . . no
H18A C18 H18B 109.00 . . . no
H18A C18 H18C 109.00 . . . no
H18B C18 H18C 110.00 . . . no
C17 C19 H19A 110.00 . . . no
C17 C19 H19B 109.00 . . . no
C17 C19 H19C 109.00 . . . no
H19A C19 H19B 110.00 . . . no
H19A C19 H19C 110.00 . . . no
H19B C19 H19C 109.00 . . . no
C17 C20 H20A 109.00 . . . no
C17 C20 H20B 109.00 . . . no
C17 C20 H20C 109.00 . . . no
H20A C20 H20B 109.00 . . . no
H20A C20 H20C 110.00 . . . no
H20B C20 H20C 109.00 . . . no
C100 C101 H10D 109.00 . . . no
C100 C101 H10E 109.00 . . . no
C100 C101 H10F 109.00 . . . no
H10D C101 H10E 109.00 . . . no
H10D C101 H10F 109.00 . . . no
H10E C101 H10F 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
Cu2 I1 Cu1 I2 21.62(5) . . . . no
Cu2 I1 Cu1 P1 -90.63(10) . . . . no
Cu2 I1 Cu1 N1 134.5(3) . . . . no
Cu1 I1 Cu2 I2 83.44(6) . . . 3_775 no
Cu1 I1 Cu2 I2 -21.85(5) . . . . no
Cu1 I1 Cu2 P2 -146.66(11) . . . . no
Cu2 I2 Cu1 I1 -103.37(6) 3_775 . . . no
Cu2 I2 Cu1 N1 -143.1(3) . . . . no
Cu2 I2 Cu1 P1 104.13(9) . . . . no
Cu2 I2 Cu1 P1 21.86(8) 3_775 . . . no
Cu2 I2 Cu1 I1 -21.11(5) . . . . no
Cu1 I2 Cu2 I1 21.31(5) . . . . no
Cu2 I2 Cu2 I1 118.07(6) 3_775 . . . no
Cu1 I2 Cu2 P2 158.27(9) . . . . no
Cu2 I2 Cu2 P2 -104.97(8) 3_775 . . . no
Cu2 I2 Cu1 N1 134.6(2) 3_775 . . . no
Cu2 I2 Cu2 I2 0.00(7) 3_775 . . 3_775 no
Cu2 I2 Cu2 P2 105.95(8) 3_775 3_775 . . no
Cu1 I2 Cu2 I2 -65.18(5) 3_775 3_775 . . no
Cu1 I2 Cu2 I1 -178.63(6) 3_775 3_775 . . no
Cu2 I2 Cu2 I1 -113.45(6) 3_775 3_775 . . no
Cu1 I2 Cu2 I2 -96.75(5) . . . 3_775 no
Cu1 I2 Cu2 P2 40.77(8) 3_775 3_775 . . no
Cu2 I2 Cu2 I2 -0.02(8) 3_775 3_775 . . no
I2 Cu1 P1 C1 168.7(5) . . . . no
I1 Cu1 P1 P2 119.78(13) . . . 3_775 no
N1 Cu1 P1 P2 -103.0(3) . . . 3_775 no
N1 Cu1 P1 C1 62.7(5) . . . . no
I2 Cu1 P1 P2 2.93(16) . . . 3_775 no
I1 Cu1 P1 C1 -74.5(5) . . . . no
I1 Cu2 P2 C3 -57.1(5) . . . . no
I1 Cu2 P2 C2 66.1(4) . . . . no
I2 Cu2 P2 P1 -44.30(12) 3_775 . . 3_775 no
I1 Cu2 P2 P1 -178.47(9) . . . 3_775 no
I2 Cu2 P2 C2 -60.6(4) . . . . no
I2 Cu2 P2 C3 176.2(4) . . . . no
I2 Cu2 P2 P1 54.84(12) . . . 3_775 no
I2 Cu2 P2 C2 -159.7(3) 3_775 . . . no
I2 Cu2 P2 C3 77.1(4) 3_775 . . . no
Cu1 P1 C1 P4 -167.6(2) . . . . no
Cu1 P1 C1 C5 16.7(10) . . . . no
P2 P1 C1 P4 0.1(5) 3_775 . . . no
P2 P1 C1 C5 -175.6(7) 3_775 . . . no
Cu1 P1 P2 Cu2 -32.06(17) . . 3_775 3_775 no
Cu1 P1 P2 C2 -165.6(3) . . 3_775 3_775 no
Cu1 P1 P2 C3 107.1(3) . . 3_775 3_775 no
C1 P1 P2 Cu2 157.4(3) . . 3_775 3_775 no
C1 P1 P2 C2 23.9(4) . . 3_775 3_775 no
C1 P1 P2 C3 -63.5(4) . . 3_775 3_775 no
Cu2 P2 C2 P3 -114.1(3) . . . . no
Cu2 P2 C2 C9 11.6(9) . . . . no
Cu2 P2 C2 P4 153.8(2) . . . 3_775 no
C3 P2 C2 P3 27.2(4) . . . . no
C3 P2 C2 C9 152.9(8) . . . . no
C3 P2 C2 P4 -64.9(4) . . . 3_775 no
P1 P2 C2 P3 130.4(2) 3_775 . . . no
P1 P2 C2 C9 -104.0(7) 3_775 . . . no
P1 P2 C2 P4 38.3(4) 3_775 . . 3_775 no
Cu2 P2 C3 P3 110.6(4) . . . . no
Cu2 P2 C3 C4 174.7(5) . . . . no
Cu2 P2 C3 C13 -24.6(9) . . . . no
C2 P2 C3 P3 -28.0(4) . . . . no
C2 P2 C3 C4 36.0(7) . . . . no
C2 P2 C3 C13 -163.2(8) . . . . no
P1 P2 C3 P3 -128.7(3) 3_775 . . . no
P1 P2 C3 C4 -64.7(7) 3_775 . . . no
P1 P2 C3 C13 96.1(7) 3_775 . . . no
C3 P3 C2 P2 -26.9(4) . . . . no
C3 P3 C2 C9 -157.4(7) . . . . no
C3 P3 C2 P4 76.5(4) . . . 3_775 no
C4 P3 C2 P2 -76.7(4) . . . . no
C4 P3 C2 C9 152.8(7) . . . . no
C4 P3 C2 P4 26.7(4) . . . 3_775 no
C2 P3 C3 P2 26.5(4) . . . . no
C2 P3 C3 C4 -84.7(5) . . . . no
C2 P3 C3 C13 152.7(9) . . . . no
C4 P3 C3 P2 111.2(6) . . . . no
C4 P3 C3 C13 -122.6(11) . . . . no
C2 P3 C4 C3 86.2(5) . . . . no
C2 P3 C4 C17 -149.2(8) . . . . no
C2 P3 C4 P4 -26.0(4) . . . 3_775 no
C3 P3 C4 C17 124.5(10) . . . . no
C3 P3 C4 P4 -112.2(6) . . . 3_775 no
C2 P4 C1 P1 -24.2(6) 3_775 . . . no
C2 P4 C1 C5 151.5(7) 3_775 . . . no
C4 P4 C1 P1 62.1(6) 3_775 . . . no
C4 P4 C1 C5 -122.3(7) 3_775 . . . no
C1 P4 C2 P2 39.3(5) . . 3_775 3_775 no
C1 P4 C2 P3 130.0(4) . . 3_775 3_775 no
C1 P4 C2 C9 -105.2(7) . . 3_775 3_775 no
C1 P4 C4 P3 -129.9(4) . . 3_775 3_775 no
C1 P4 C4 C3 -65.0(7) . . 3_775 3_775 no
C1 P4 C4 C17 102.7(7) . . 3_775 3_775 no
P1 C1 C5 C6 88.3(9) . . . . no
P1 C1 C5 C7 -154.0(7) . . . . no
P1 C1 C5 C8 -33.2(11) . . . . no
P4 C1 C5 C6 -87.1(9) . . . . no
P4 C1 C5 C7 30.6(11) . . . . no
P4 C1 C5 C8 151.4(7) . . . . no
P2 C2 C9 C10 -45.0(11) . . . . no
P2 C2 C9 C11 -165.6(6) . . . . no
P2 C2 C9 C12 77.0(9) . . . . no
P3 C2 C9 C10 67.5(9) . . . . no
P3 C2 C9 C11 -53.2(9) . . . . no
P3 C2 C9 C12 -170.6(6) . . . . no
P4 C2 C9 C10 178.6(6) 3_775 . . . no
P4 C2 C9 C11 57.9(9) 3_775 . . . no
P4 C2 C9 C12 -59.5(9) 3_775 . . . no
P2 C3 C4 P3 -81.9(5) . . . . no
P2 C3 C4 C17 166.3(8) . . . . no
P2 C3 C4 P4 0.9(8) . . . 3_775 no
P3 C3 C4 C17 -111.8(10) . . . . no
P3 C3 C4 P4 82.8(5) . . . 3_775 no
C13 C3 C4 P3 120.8(10) . . . . no
C13 C3 C4 C17 9.0(17) . . . . no
C13 C3 C4 P4 -156.5(8) . . . 3_775 no
P2 C3 C13 C14 47.6(10) . . . . no
P2 C3 C13 C15 -69.1(9) . . . . no
P2 C3 C13 C16 166.2(7) . . . . no
P3 C3 C13 C14 -67.9(11) . . . . no
P3 C3 C13 C15 175.5(7) . . . . no
P3 C3 C13 C16 50.7(12) . . . . no
C4 C3 C13 C14 -156.3(10) . . . . no
C4 C3 C13 C15 87.0(12) . . . . no
C4 C3 C13 C16 -37.7(14) . . . . no
P3 C4 C17 C18 94.0(9) . . . . no
P3 C4 C17 C19 -23.3(11) . . . . no
P3 C4 C17 C20 -147.5(7) . . . . no
C3 C4 C17 C18 178.1(10) . . . . no
C3 C4 C17 C19 60.8(13) . . . . no
C3 C4 C17 C20 -63.5(13) . . . . no
P4 C4 C17 C18 -17.1(11) 3_775 . . . no
P4 C4 C17 C19 -134.4(7) 3_775 . . . no
P4 C4 C17 C20 101.3(8) 3_775 . . . 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
I2 P1 3.805(3) . . no
I2 P2 3.940(3) . . no
I2 C101 3.745(9) . 2_755 no
I2 C12 3.872(10) . . no
I2 I2 4.0156(11) . 3_775 no
I2 N1 3.712(8) . . no
I2 P2 3.894(3) . 3_775 no
I2 Cu1 4.3021(17) . 3_775 no
I1 H10D 3.2300 . 4_564 no
I1 H10E 3.1600 . 2_745 no
I1 H15A 3.2300 . 4_565 no
I2 H10B 3.2900 . . no
I2 H12C 2.9600 . . no
I2 H14C 3.3500 . 3_775 no
I2 H15B 3.0900 . 3_775 no
Cu1 C8 3.643(10) . . no
Cu1 C15 4.155(10) . 3_775 no
Cu1 I2 4.3021(17) . 3_775 no
Cu2 C14 3.496(10) . . no
Cu2 P1 4.200(3) . . no
Cu2 C10 3.682(10) . . no
Cu1 H8C 3.6100 . . no
Cu1 H15B 3.2600 . 3_775 no
Cu1 H8B 2.9100 . . no
Cu2 H10B 2.8500 . . no
Cu2 H14B 3.6200 . . no
Cu2 H14C 2.6500 . . no
Cu2 H15B 3.6700 . . no
P1 I2 3.805(3) . . no
P1 Cu2 4.200(3) . . no
P1 N1 3.483(9) . . no
P1 Cu2 3.448(3) . 3_775 no
P2 Cu1 3.842(3) . 3_775 no
P2 I2 3.894(3) . 3_775 no
P2 I2 3.940(3) . . no
P3 C18 3.674(12) . 2_644 no
P1 H8C 3.1400 . . no
P1 H15B 3.0500 . 3_775 no
P1 H8B 2.8100 . . no
P2 H10B 2.9800 . . no
P2 H14C 2.7700 . . no
P2 H15B 2.9400 . . no
P3 H10C 3.0400 . . no
P3 H14B 3.1800 . . no
P3 H19C 2.6100 . . no
P3 H11B 2.8500 . . no
P3 H7C 3.1900 . 4_464 no
P4 H7C 2.8000 . . no
P4 H11C 2.9000 . 3_775 no
P4 H12B 2.8800 . 3_775 no
P4 H18A 2.9000 . 3_775 no
P4 H18C 2.6000 . 3_775 no
N1 I2 3.712(8) . . no
N1 P1 3.483(9) . . no
C8 Cu1 3.643(10) . . no
C10 Cu2 3.682(10) . . no
C12 I2 3.872(10) . . no
C14 Cu2 3.496(10) . . no
C15 Cu1 4.155(10) . 3_775 no
C16 C17 3.523(13) . . no
C16 C19 3.232(14) . . no
C16 C20 3.551(14) . . no
C17 C16 3.523(13) . . no
C18 P3 3.674(12) . 2_654 no
C19 C16 3.232(14) . . no
C20 C16 3.551(14) . . no
C101 I2 3.745(9) . 2_745 no
C7 H18C 2.8400 . 3_775 no
C13 H20A 3.1000 . . no
C16 H19A 2.6100 . . no
C16 H20A 2.7900 . . no
C17 H16B 2.9500 . . no
C19 H16C 2.9800 . . no
C19 H16B 2.7000 . . no
C20 H15C 2.9800 . . no
C20 H12A 2.9800 . 4_574 no
C20 H16B 2.7500 . . no
C100 H8A 3.0700 . 2_755 no
H6A H7A 2.4000 . . no
H6B H7C 2.5500 . . no
H6B H12B 2.5300 . 3_775 no
H6C H8B 2.4300 . . no
H7A H6A 2.4000 . . no
H7A H8A 2.3900 . . no
H7B H8C 2.5200 . . no
H7B H18C 2.4000 . 3_775 no
H7C P4 2.8000 . . no
H7C H6B 2.5500 . . no
H7C H18C 2.4500 . 3_775 no
H7C P3 3.1900 . 4_665 no
H7C H19C 2.5700 . 4_665 no
H8A H7A 2.3900 . . no
H8A C100 3.0700 . 2_745 no
H8B Cu1 2.9100 . . no
H8B P1 2.8100 . . no
H8B H6C 2.4300 . . no
H8C Cu1 3.6100 . . no
H8C P1 3.1400 . . no
H8C H7B 2.5200 . . no
H10A H11A 2.4500 . . no
H10A H12A 2.5500 . . no
H10B I2 3.2900 . . no
H10B Cu2 2.8500 . . no
H10B P2 2.9800 . . no
H10B H12C 2.5500 . . no
H10C P3 3.0400 . . no
H10C H11B 2.5700 . . no
H10D I1 3.2300 . 4_565 no
H10E I1 3.1600 . 2_755 no
H11A H10A 2.4500 . . no
H11A H12A 2.5500 . . no
H11B P3 2.8500 . . no
H11B H10C 2.5700 . . no
H11C H12B 2.4700 . . no
H11C H16C 2.5300 . 2_654 no
H11C P4 2.9000 . 3_775 no
H12A H10A 2.5500 . . no
H12A H11A 2.5500 . . no
H12A C20 2.9800 . 4_575 no
H12A H20B 2.3400 . 4_575 no
H12B H11C 2.4700 . . no
H12B P4 2.8800 . 3_775 no
H12B H6B 2.5300 . 3_775 no
H12C I2 2.9600 . . no
H12C H10B 2.5500 . . no
H14A H15A 2.5600 . . no
H14A H16A 2.2500 . . no
H14B Cu2 3.6200 . . no
H14B P3 3.1800 . . no
H14B H16C 2.5600 . . no
H14C Cu2 2.6500 . . no
H14C P2 2.7700 . . no
H14C H15B 2.4000 . . no
H14C I2 3.3500 . 3_775 no
H15A H14A 2.5600 . . no
H15A H16A 2.4600 . . no
H15A I1 3.2300 . 4_564 no
H15B Cu2 3.6700 . . no
H15B P2 2.9400 . . no
H15B H14C 2.4000 . . no
H15B I2 3.0900 . 3_775 no
H15B Cu1 3.2600 . 3_775 no
H15B P1 3.0500 . 3_775 no
H15C C20 2.9800 . . no
H15C H16B 2.5800 . . no
H15C H20A 2.3900 . . no
H16A H14A 2.2500 . . no
H16A H15A 2.4600 . . no
H16B C17 2.9500 . . no
H16B C19 2.7000 . . no
H16B C20 2.7500 . . no
H16B H15C 2.5800 . . no
H16B H19A 1.9800 . . no
H16B H20A 1.9300 . . no
H16C C19 2.9800 . . no
H16C H14B 2.5600 . . no
H16C H19A 2.4400 . . no
H16C H11C 2.5300 . 2_644 no
H18A H19B 2.5100 . . no
H18A P4 2.9000 . 3_775 no
H18B H19B 2.1800 . . no
H18B H20C 2.3400 . . no
H18C H20B 2.5500 . . no
H18C P4 2.6000 . 3_775 no
H18C C7 2.8400 . 3_775 no
H18C H7B 2.4000 . 3_775 no
H18C H7C 2.4500 . 3_775 no
H19A C16 2.6100 . . no
H19A H16B 1.9800 . . no
H19A H16C 2.4400 . . no
H19A H20A 2.3100 . . no
H19A H20C 2.4300 . 3_674 no
H19B H18A 2.5100 . . no
H19B H18B 2.1800 . . no
H19C P3 2.6100 . . no
H19C H7C 2.5700 . 4_464 no
H20A C13 3.1000 . . no
H20A C16 2.7900 . . no
H20A H15C 2.3900 . . no
H20A H16B 1.9300 . . no
H20A H19A 2.3100 . . no
H20B H18C 2.5500 . . no
H20B H12A 2.3400 . 4_574 no
H20C H18B 2.3400 . . no
H20C H19A 2.4300 . 3_674 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
#
#D H A D - H H...A D...A D - H...A symm(A)
#
C7 H7C P4 0.9800 2.8000 3.182(10) 104.00 . yes
C11 H11B P3 0.9800 2.8500 3.298(10) 109.00 . yes
C12 H12C I2 0.9800 2.9600 3.872(10) 156.00 . yes
C18 H18C P4 0.9800 2.6000 2.951(11) 101.00 3_775 yes
C19 H19C P3 0.9800 2.6100 3.230(10) 121.00 . yes
# Loop Mechanism for Extra Tables(s)
#loop_
#_publ_manuscript_incl_extra_item
#'_geom_extra_tableA_col_1'
#'_geom_extra_tableA_col_2'
#'_geom_extra_tableA_col_3'
#'_geom_extra_table_head_A'
#'_geom_table_footnote_A'
#'_geom_extra_tableB_col_1'
#'_geom_extra_tableB_col_2'
#'_geom_extra_tableB_col_3'
#'_geom_extra_table_head_B'
#'_geom_table_footnote_B'
#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
# ? ? ?
#
#loop_
#_geom_extra_tableB_col_1
#_geom_extra_tableB_col_2
#_geom_extra_tableB_col_3
# ? ? ?
#
#_geom_table_footnote_A
#;
# ?
#;
#
#_geom_table_footnote_B
#;
# ?
#;
#
#_geom_table_footnote_A
#;
# ?
#;
#
#_geom_table_footnote_B
#;
# ?
#;
#===END
# Attachment 'compound6.cif'
data_u512_2
_database_code_depnum_ccdc_archive 'CCDC 656703'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C20 H37 P5, 0.5(C7 H8)'
_chemical_formula_structural '(P5 H C4)(C4 H9)4 * 0.5(C7 H8)'
_chemical_formula_sum 'C23.50 H41 P5'
_chemical_formula_weight 478.41
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/m'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
_cell_length_a 23.7888(3)
_cell_length_b 11.2636(2)
_cell_length_c 10.38680(10)
_cell_angle_alpha 90.00
_cell_angle_beta 108.2020(10)
_cell_angle_gamma 90.00
_cell_volume 2643.85(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 123(2)
_cell_measurement_reflns_used 16404
_cell_measurement_theta_min 1.9472
_cell_measurement_theta_max 65.3244
_exptl_crystal_description block
_exptl_crystal_colour 'light yellow'
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.202
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1028
_exptl_absorpt_coefficient_mu 3.259
_exptl_absorpt_correction_T_min 0.208
_exptl_absorpt_correction_T_max 0.613
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 123(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Oxford Gemini R-Ultra'
_diffrn_measurement_method 'combined phi- and omega-scans'
_diffrn_detector_area_resol_mean 10.5431
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 25696
_diffrn_reflns_av_R_equivalents 0.1366
_diffrn_reflns_av_sigmaI/netI 0.0440
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_theta_min 3.91
_diffrn_reflns_theta_max 65.50
_reflns_number_total 2385
_reflns_number_gt 2156
_reflns_threshold_expression >2sigma(I)
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics Siemens-XP
_computing_publication_material SHELXL-97
_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^)+(0.1503P)^2^+10.0028P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2385
_refine_ls_number_parameters 158
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0850
_refine_ls_R_factor_gt 0.0810
_refine_ls_wR_factor_ref 0.2363
_refine_ls_wR_factor_gt 0.2302
_refine_ls_goodness_of_fit_ref 1.098
_refine_ls_restrained_S_all 1.098
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.82551(4) 0.37921(8) 0.16827(9) 0.0276(4) Uani 1 1 d . . .
P3 P 0.80058(6) 0.5000 0.37558(13) 0.0306(4) Uani 1 2 d S . .
P4 P 0.91659(6) 0.5000 0.42535(14) 0.0346(5) Uani 1 2 d S . .
P5 P 0.94957(7) 0.5000 0.25403(16) 0.0497(6) Uani 1 2 d S . .
H1 H 0.9586 0.6095 0.2447 0.050 Uiso 0.50 1 d PR . .
C1 C 0.85654(16) 0.3850(3) 0.3599(4) 0.0287(9) Uani 1 1 d . . .
C2 C 0.7731(2) 0.5000 0.1860(5) 0.0236(10) Uani 1 2 d S . .
C3 C 0.8729(2) 0.5000 0.1280(5) 0.0266(11) Uani 1 2 d S . .
C4 C 0.86377(18) 0.2653(4) 0.4348(4) 0.0356(9) Uani 1 1 d . . .
C5 C 0.8054(2) 0.1972(4) 0.3913(5) 0.0459(11) Uani 1 1 d . . .
H5A H 0.7925 0.1859 0.2928 0.069 Uiso 1 1 calc R . .
H5B H 0.7753 0.2423 0.4169 0.069 Uiso 1 1 calc R . .
H5C H 0.8109 0.1196 0.4362 0.069 Uiso 1 1 calc R . .
C6 C 0.8809(2) 0.2853(5) 0.5882(4) 0.0492(12) Uani 1 1 d . . .
H6A H 0.8885 0.2086 0.6350 0.074 Uiso 1 1 calc R . .
H6B H 0.8485 0.3258 0.6098 0.074 Uiso 1 1 calc R . .
H6C H 0.9167 0.3343 0.6180 0.074 Uiso 1 1 calc R . .
C7 C 0.9122(2) 0.1934(5) 0.4013(6) 0.0589(14) Uani 1 1 d . . .
H7A H 0.9003 0.1778 0.3037 0.088 Uiso 1 1 calc R . .
H7B H 0.9181 0.1179 0.4506 0.088 Uiso 1 1 calc R . .
H7C H 0.9493 0.2386 0.4283 0.088 Uiso 1 1 calc R . .
C8 C 0.7058(2) 0.5000 0.1169(6) 0.0299(12) Uani 1 2 d S . .
C9 C 0.6888(3) 0.5000 -0.0368(6) 0.0473(16) Uani 1 2 d S . .
H9A H 0.7056 0.5714 -0.0597 0.050 Uiso 1 1 d R . .
H9B H 0.6457 0.5000 -0.0697 0.050 Uiso 1 2 d SR . .
C10 C 0.68004(19) 0.6110(4) 0.1615(5) 0.0480(12) Uani 1 1 d . . .
H10A H 0.6378 0.6169 0.1108 0.072 Uiso 1 1 calc R . .
H10B H 0.7007 0.6814 0.1437 0.072 Uiso 1 1 calc R . .
H10C H 0.6851 0.6060 0.2587 0.072 Uiso 1 1 calc R . .
C11 C 0.8788(2) 0.5000 -0.0176(5) 0.0328(12) Uani 1 2 d S . .
C12 C 0.9122(2) 0.3885(5) -0.0373(5) 0.0469(12) Uani 1 1 d . . .
H12A H 0.9528 0.3913 0.0245 0.070 Uiso 1 1 calc R . .
H12B H 0.9128 0.3852 -0.1311 0.070 Uiso 1 1 calc R . .
H12C H 0.8922 0.3179 -0.0178 0.070 Uiso 1 1 calc R . .
C13 C 0.8176(3) 0.5000 -0.1249(6) 0.0437(15) Uani 1 2 d S . .
H13A H 0.8220 0.5000 -0.2135 0.052 Uiso 1 2 d SR . .
H13B H 0.7962 0.4305 -0.1142 0.052 Uiso 1 1 d R . .
C1S C 0.4954(5) 0.5000 -0.0764(16) 0.048(3) Uani 0.50 2 d SP . .
C2S C 0.4979(4) 0.3943(10) 0.1258(13) 0.061(3) Uani 0.50 1 d P . .
H2SA H 0.4924 0.3195 0.1648 0.074 Uiso 0.50 1 d PR . .
C3S C 0.4970(4) 0.5000 -0.2070(10) 0.074(2) Uani 1 2 d S . .
H3SA H 0.4933 0.5799 -0.2407 0.111 Uiso 0.25 1 d PR . .
H3SB H 0.5339 0.4671 -0.2094 0.111 Uiso 0.25 1 d PR . .
H3SC H 0.4649 0.4529 -0.2626 0.111 Uiso 0.25 1 d PR . .
H3SD H 0.4908 0.5000 -0.3029 0.089 Uiso 0.50 2 d SPR . .
C4S C 0.5000 0.3953(6) 0.0000 0.0519(18) Uani 1 2 d S . .
H4SA H 0.5050 0.3212 -0.0408 0.062 Uiso 0.50 1 d PR . .
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
P1 0.0290(6) 0.0282(6) 0.0295(6) 0.0001(4) 0.0147(4) 0.0013(3)
P3 0.0361(8) 0.0317(8) 0.0263(7) 0.000 0.0131(6) 0.000
P4 0.0307(8) 0.0420(9) 0.0320(8) 0.000 0.0110(6) 0.000
P5 0.0294(9) 0.0875(14) 0.0344(9) 0.000 0.0129(7) 0.000
C1 0.0216(18) 0.033(2) 0.0328(19) 0.0054(15) 0.0107(15) 0.0005(14)
C2 0.020(2) 0.027(3) 0.026(2) 0.000 0.0091(19) 0.000
C3 0.024(2) 0.036(3) 0.024(2) 0.000 0.013(2) 0.000
C4 0.038(2) 0.030(2) 0.040(2) 0.0085(17) 0.0147(17) 0.0043(17)
C5 0.059(3) 0.037(2) 0.045(2) 0.0065(19) 0.021(2) -0.008(2)
C6 0.059(3) 0.050(3) 0.037(2) 0.013(2) 0.013(2) -0.001(2)
C7 0.060(3) 0.054(3) 0.068(3) 0.024(3) 0.028(3) 0.027(3)
C8 0.023(3) 0.029(3) 0.038(3) 0.000 0.010(2) 0.000
C9 0.028(3) 0.071(5) 0.039(3) 0.000 0.004(3) 0.000
C10 0.024(2) 0.055(3) 0.063(3) -0.012(2) 0.0091(19) 0.0073(19)
C11 0.033(3) 0.046(3) 0.025(3) 0.000 0.017(2) 0.000
C12 0.050(3) 0.058(3) 0.042(2) -0.009(2) 0.028(2) 0.005(2)
C13 0.046(4) 0.063(4) 0.023(3) 0.000 0.011(2) 0.000
C1S 0.022(6) 0.051(8) 0.074(9) 0.000 0.018(6) 0.000
C2S 0.039(5) 0.051(6) 0.085(9) 0.026(6) 0.008(5) -0.001(4)
C3S 0.057(5) 0.091(7) 0.077(6) 0.000 0.024(4) 0.000
C4S 0.040(4) 0.032(3) 0.083(6) 0.000 0.018(3) 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C2 1.893(3) . ?
P1 C3 1.895(3) . ?
P1 C1 1.896(4) . ?
P3 C2 1.871(5) . ?
P3 C1 1.901(4) . ?
P3 C1 1.901(4) 6_565 ?
P3 P4 2.644(2) . ?
P4 C1 1.891(4) . ?
P4 C1 1.891(4) 6_565 ?
P4 P5 2.157(2) . ?
P5 C3 1.884(5) . ?
P5 H1 1.2609 . ?
C1 C4 1.539(5) . ?
C2 C8 1.536(7) . ?
C2 P1 1.893(3) 6_565 ?
C3 C11 1.562(7) . ?
C3 P1 1.895(3) 6_565 ?
C4 C5 1.527(6) . ?
C4 C6 1.533(6) . ?
C4 C7 1.535(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.519(8) . ?
C8 C10 1.527(5) 6_565 ?
C8 C10 1.527(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9751 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.533(8) . ?
C11 C12 1.533(5) 6_565 ?
C11 C12 1.533(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9586 . ?
C13 H13B 0.9587 . ?
C1S C2S 1.326(12) 2_655 ?
C1S C2S 1.326(12) 5_665 ?
C1S C3S 1.369(17) . ?
C1S C4S 1.406(10) . ?
C1S C4S 1.406(10) 5_665 ?
C1S C1S 1.53(3) 5_665 ?
C2S C4S 1.324(13) . ?
C2S C1S 1.326(12) 5_665 ?
C2S C3S 1.442(14) 5_665 ?
C2S H2SA 0.9601 . ?
C3S C2S 1.442(14) 2_655 ?
C3S C2S 1.442(14) 5_665 ?
C3S H3SA 0.9600 . ?
C3S H3SB 0.9600 . ?
C3S H3SC 0.9601 . ?
C3S H3SD 0.9600 . ?
C4S C2S 1.324(13) 2_655 ?
C4S C1S 1.406(10) 5_665 ?
C4S H4SA 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 P1 C3 87.74(16) . . ?
C2 P1 C1 85.74(19) . . ?
C3 P1 C1 98.26(19) . . ?
C2 P3 C1 86.21(16) . . ?
C2 P3 C1 86.21(16) . 6_565 ?
C1 P3 C1 85.9(2) . 6_565 ?
C2 P3 P4 101.90(16) . . ?
C1 P3 P4 45.62(12) . . ?
C1 P3 P4 45.62(12) 6_565 . ?
C1 P4 C1 86.5(2) . 6_565 ?
C1 P4 P5 97.59(13) . . ?
C1 P4 P5 97.59(13) 6_565 . ?
C1 P4 P3 45.93(12) . . ?
C1 P4 P3 45.93(12) 6_565 . ?
P5 P4 P3 117.71(8) . . ?
C3 P5 P4 92.88(16) . . ?
C3 P5 H1 95.6 . . ?
P4 P5 H1 100.2 . . ?
C4 C1 P4 117.8(3) . . ?
C4 C1 P1 116.5(3) . . ?
P4 C1 P1 113.80(19) . . ?
C4 C1 P3 121.6(3) . . ?
P4 C1 P3 88.45(17) . . ?
P1 C1 P3 93.42(17) . . ?
C8 C2 P3 117.5(4) . . ?
C8 C2 P1 125.2(2) . . ?
P3 C2 P1 94.47(19) . . ?
C8 C2 P1 125.2(2) . 6_565 ?
P3 C2 P1 94.47(19) . 6_565 ?
P1 C2 P1 91.9(2) . 6_565 ?
C11 C3 P5 108.2(3) . . ?
C11 C3 P1 117.0(2) . . ?
P5 C3 P1 111.1(2) . . ?
C11 C3 P1 117.0(2) . 6_565 ?
P5 C3 P1 111.1(2) . 6_565 ?
P1 C3 P1 91.8(2) . 6_565 ?
C5 C4 C6 107.7(3) . . ?
C5 C4 C7 110.2(4) . . ?
C6 C4 C7 109.8(4) . . ?
C5 C4 C1 110.0(3) . . ?
C6 C4 C1 110.4(4) . . ?
C7 C4 C1 108.7(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C10 108.6(3) . 6_565 ?
C9 C8 C10 108.6(3) . . ?
C10 C8 C10 110.0(5) 6_565 . ?
C9 C8 C2 112.8(4) . . ?
C10 C8 C2 108.5(3) 6_565 . ?
C10 C8 C2 108.5(3) . . ?
C8 C9 H9A 105.4 . . ?
C8 C9 H9B 105.9 . . ?
H9A C9 H9B 112.7 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C12 108.5(3) . 6_565 ?
C13 C11 C12 108.5(3) . . ?
C12 C11 C12 110.0(5) 6_565 . ?
C13 C11 C3 110.6(4) . . ?
C12 C11 C3 109.7(3) 6_565 . ?
C12 C11 C3 109.7(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.4 . . ?
C2S C1S C2S 127.8(17) 2_655 5_665 ?
C2S C1S C3S 64.7(9) 2_655 . ?
C2S C1S C3S 64.7(9) 5_665 . ?
C2S C1S C4S 57.9(6) 2_655 . ?
C2S C1S C4S 166.9(13) 5_665 . ?
C3S C1S C4S 122.5(5) . . ?
C2S C1S C4S 166.9(13) 2_655 5_665 ?
C2S C1S C4S 57.9(6) 5_665 5_665 ?
C3S C1S C4S 122.5(5) . 5_665 ?
C4S C1S C4S 114.0(11) . 5_665 ?
C2S C1S C1S 113.9(9) 2_655 5_665 ?
C2S C1S C1S 113.9(9) 5_665 5_665 ?
C3S C1S C1S 170.8(14) . 5_665 ?
C4S C1S C1S 57.0(5) . 5_665 ?
C4S C1S C1S 57.0(5) 5_665 5_665 ?
C4S C2S C1S 64.1(9) . 5_665 ?
C4S C2S C3S 123.2(9) . 5_665 ?
C1S C2S C3S 59.1(8) 5_665 5_665 ?
C4S C2S H2SA 118.4 . . ?
C1S C2S H2SA 177.4 5_665 . ?
C3S C2S H2SA 118.4 5_665 . ?
C1S C3S C2S 56.2(6) . 2_655 ?
C1S C3S C2S 56.2(6) . 5_665 ?
C2S C3S C2S 111.3(11) 2_655 5_665 ?
C1S C3S H3SA 109.5 . . ?
C2S C3S H3SA 165.7 2_655 . ?
C2S C3S H3SA 54.5 5_665 . ?
C1S C3S H3SB 109.4 . . ?
C2S C3S H3SB 77.6 2_655 . ?
C2S C3S H3SB 115.0 5_665 . ?
H3SA C3S H3SB 109.5 . . ?
C1S C3S H3SC 109.5 . . ?
C2S C3S H3SC 78.6 2_655 . ?
C2S C3S H3SC 135.6 5_665 . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
C1S C3S H3SD 170.2 . . ?
C2S C3S H3SD 124.3 2_655 . ?
C2S C3S H3SD 124.3 5_665 . ?
H3SA C3S H3SD 69.8 . . ?
H3SB C3S H3SD 79.5 . . ?
H3SC C3S H3SD 62.7 . . ?
C2S C4S C2S 179.0(11) . 2_655 ?
C2S C4S C1S 123.0(8) . . ?
C2S C4S C1S 58.0(7) 2_655 . ?
C2S C4S C1S 58.0(7) . 5_665 ?
C2S C4S C1S 123.0(8) 2_655 5_665 ?
C1S C4S C1S 66.0(11) . 5_665 ?
C2S C4S H4SA 118.4 . . ?
C2S C4S H4SA 60.6 2_655 . ?
C1S C4S H4SA 118.6 . . ?
C1S C4S H4SA 168.4 5_665 . ?
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full 65.50
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max 1.973
_refine_diff_density_min -0.560
_refine_diff_density_rms 0.122