# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_journal_year ?
_journal_volume ?
_journal_page_first ?
loop_
_publ_author_name
'Housecroft, Catherine'
'Constable, Edwin'
'Meuwly, Markus'
'Rudd, Jennifer'
'Chaurin, Valerie'
'Bozic-Weber, Biljana'
'Neuburger, Markus'
'Schoenhofer, Ewald'
'Siegfried, Liselott'
_publ_contact_author_name 'Housecroft, Catherine'
_publ_contact_author_email Catherine.Housecroft@unibas.ch
data_Cu(Me2bpy)2
_database_code_depnum_ccdc_archive 'CCDC 885553'
#TrackingRef '- Cu(Me2bpy)2.cif'
_audit_creation_date 11-10-10
_audit_creation_method CRYSTALS_ver_14.23
_oxford_structure_analysis_title 'jar95_123k_0ma in P2(1)/c'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 12.7104(6)
_cell_length_b 21.9632(11)
_cell_length_c 8.7001(5)
_cell_angle_alpha 90
_cell_angle_beta 94.692(2)
_cell_angle_gamma 90
_cell_volume 2420.6(2)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C24 H24 Cu1 F6 N4 P1
# Dc = 1.58 Fooo = 1176.00 Mu = 10.36 M = 576.99
# Found Formula = C24 H24 Cu1 F6 N4 P1
# Dc = 1.58 FOOO = 1176.00 Mu = 10.36 M = 576.99
_chemical_formula_sum 'C24 H24 Cu1 F6 N4 P1'
_chemical_formula_moiety 'C24 H24 Cu1 N4, F6 P'
_chemical_compound_source ?
_chemical_formula_weight 576.99
_cell_measurement_reflns_used 9888
_cell_measurement_theta_min 3
_cell_measurement_theta_max 36
_cell_measurement_temperature 123
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_min 0.060
_exptl_crystal_size_mid 0.130
_exptl_crystal_size_max 0.210
_exptl_crystal_density_diffrn 1.583
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1176
_exptl_absorpt_coefficient_mu 1.036
# Sheldrick geometric approximatio 0.87 0.94
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.87
_exptl_absorpt_correction_T_max 0.94
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 123
_diffrn_reflns_number 35645
_reflns_number_total 8817
_diffrn_reflns_av_R_equivalents 0.030
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 8817
# Theoretical number of reflections is about 17649
_diffrn_reflns_theta_min 1.856
_diffrn_reflns_theta_max 32.588
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 32.588
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -33
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -19
_reflns_limit_h_max 19
_reflns_limit_k_min 0
_reflns_limit_k_max 33
_reflns_limit_l_min 0
_reflns_limit_l_max 13
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.35
_refine_diff_density_max 0.54
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns 6818
_refine_ls_number_restraints 0
_refine_ls_number_parameters 325
_oxford_refine_ls_R_factor_ref 0.0274
_refine_ls_wR_factor_ref 0.0293
_refine_ls_goodness_of_fit_ref 1.0891
_refine_ls_shift/su_max 0.0016108
_refine_ls_shift/su_mean 0.0000845
# The values computed from all data
_oxford_reflns_number_all 8801
_refine_ls_R_factor_all 0.0370
_refine_ls_wR_factor_all 0.0450
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 7537
_refine_ls_R_factor_gt 0.0301
_refine_ls_wR_factor_gt 0.0312
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.186 0.186 0.100 0.310E-01 0.455E-02
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.797948(10) 0.623983(6) 0.414035(15) 0.0159 1.0000 Uani . . . . . .
N1 N 0.67509(7) 0.67277(4) 0.48301(10) 0.0153 1.0000 Uani . . . . . .
N2 N 0.72406(7) 0.55652(4) 0.52680(10) 0.0149 1.0000 Uani . . . . . .
N3 N 0.82863(7) 0.60298(4) 0.19315(10) 0.0151 1.0000 Uani . . . . . .
N4 N 0.95102(7) 0.65169(4) 0.42438(10) 0.0140 1.0000 Uani . . . . . .
C1 C 0.65649(9) 0.73250(5) 0.45918(13) 0.0191 1.0000 Uani . . . . . .
C2 C 0.56662(10) 0.76054(6) 0.50752(15) 0.0262 1.0000 Uani . . . . . .
C3 C 0.49521(10) 0.72664(6) 0.58280(16) 0.0290 1.0000 Uani . . . . . .
C4 C 0.51463(9) 0.66519(6) 0.60907(15) 0.0244 1.0000 Uani . . . . . .
C5 C 0.60552(8) 0.63963(5) 0.55808(12) 0.0157 1.0000 Uani . . . . . .
C6 C 0.63282(8) 0.57457(5) 0.58262(12) 0.0149 1.0000 Uani . . . . . .
C7 C 0.56960(8) 0.53437(5) 0.65813(13) 0.0187 1.0000 Uani . . . . . .
C8 C 0.60070(9) 0.47396(5) 0.67356(14) 0.0220 1.0000 Uani . . . . . .
C9 C 0.69278(9) 0.45532(5) 0.61311(14) 0.0214 1.0000 Uani . . . . . .
C10 C 0.75349(8) 0.49773(5) 0.54050(13) 0.0174 1.0000 Uani . . . . . .
C11 C 0.73682(10) 0.76728(6) 0.37838(15) 0.0249 1.0000 Uani . . . . . .
C12 C 0.85482(9) 0.48051(6) 0.47528(16) 0.0246 1.0000 Uani . . . . . .
C13 C 0.76352(8) 0.57470(5) 0.08605(13) 0.0180 1.0000 Uani . . . . . .
C14 C 0.79976(10) 0.55375(5) -0.05161(13) 0.0216 1.0000 Uani . . . . . .
C15 C 0.90481(10) 0.56090(6) -0.07697(14) 0.0256 1.0000 Uani . . . . . .
C16 C 0.97245(9) 0.58969(6) 0.03347(14) 0.0226 1.0000 Uani . . . . . .
C17 C 0.93138(8) 0.61088(5) 0.16695(12) 0.0150 1.0000 Uani . . . . . .
C18 C 0.99680(8) 0.64273(5) 0.29051(12) 0.0143 1.0000 Uani . . . . . .
C19 C 1.09834(8) 0.66295(5) 0.27024(13) 0.0176 1.0000 Uani . . . . . .
C20 C 1.15521(8) 0.69258(5) 0.39105(14) 0.0192 1.0000 Uani . . . . . .
C21 C 1.10937(8) 0.70103(5) 0.52846(14) 0.0189 1.0000 Uani . . . . . .
C22 C 1.00629(8) 0.68063(5) 0.54111(12) 0.0160 1.0000 Uani . . . . . .
C23 C 0.65157(9) 0.56521(6) 0.12203(16) 0.0261 1.0000 Uani . . . . . .
C24 C 0.95203(9) 0.69151(6) 0.68489(13) 0.0227 1.0000 Uani . . . . . .
P1 P 0.29951(2) 0.632972(13) -0.07919(3) 0.0184 1.0000 Uani . . . . . .
F1 F 0.30415(9) 0.66872(5) 0.08121(12) 0.0502 1.0000 Uani . . . . . .
F2 F 0.26007(8) 0.57415(4) 0.00577(13) 0.0425 1.0000 Uani . . . . . .
F3 F 0.29674(9) 0.59734(6) -0.23808(12) 0.0511 1.0000 Uani . . . . . .
F4 F 0.33844(7) 0.69273(4) -0.16159(12) 0.0368 1.0000 Uani . . . . . .
F5 F 0.17971(6) 0.65360(5) -0.11454(12) 0.0426 1.0000 Uani . . . . . .
F6 F 0.41977(7) 0.61292(5) -0.04272(13) 0.0454 1.0000 Uani . . . . . .
H21 H 0.5553 0.8025 0.4876 0.0328 1.0000 Uiso R . . . . .
H31 H 0.4333 0.7449 0.6162 0.0350 1.0000 Uiso R . . . . .
H41 H 0.4667 0.6415 0.6596 0.0296 1.0000 Uiso R . . . . .
H71 H 0.5062 0.5485 0.6967 0.0232 1.0000 Uiso R . . . . .
H81 H 0.5596 0.4460 0.7268 0.0279 1.0000 Uiso R . . . . .
H91 H 0.7159 0.4142 0.6221 0.0270 1.0000 Uiso R . . . . .
H113 H 0.7133 0.8069 0.3518 0.0405 1.0000 Uiso R . . . . .
H112 H 0.8018 0.7692 0.4412 0.0406 1.0000 Uiso R . . . . .
H111 H 0.7514 0.7463 0.2851 0.0403 1.0000 Uiso R . . . . .
H123 H 0.8767 0.4408 0.5058 0.0403 1.0000 Uiso R . . . . .
H122 H 0.9091 0.5090 0.5055 0.0407 1.0000 Uiso R . . . . .
H121 H 0.8456 0.4817 0.3643 0.0400 1.0000 Uiso R . . . . .
H141 H 0.7523 0.5342 -0.1275 0.0266 1.0000 Uiso R . . . . .
H151 H 0.9301 0.5466 -0.1704 0.0316 1.0000 Uiso R . . . . .
H161 H 1.0456 0.5945 0.0188 0.0276 1.0000 Uiso R . . . . .
H191 H 1.1275 0.6569 0.1755 0.0207 1.0000 Uiso R . . . . .
H201 H 1.2238 0.7074 0.3789 0.0235 1.0000 Uiso R . . . . .
H211 H 1.1459 0.7212 0.6128 0.0238 1.0000 Uiso R . . . . .
H233 H 0.6071 0.5599 0.0304 0.0408 1.0000 Uiso R . . . . .
H232 H 0.6273 0.5997 0.1771 0.0403 1.0000 Uiso R . . . . .
H231 H 0.6474 0.5300 0.1873 0.0411 1.0000 Uiso R . . . . .
H243 H 0.9994 0.6896 0.7733 0.0369 1.0000 Uiso R . . . . .
H242 H 0.9193 0.7313 0.6782 0.0366 1.0000 Uiso R . . . . .
H241 H 0.8968 0.6620 0.6908 0.0358 1.0000 Uiso 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
Cu1 0.01191(5) 0.01870(6) 0.01788(6) -0.00057(5) 0.00635(4) -0.00072(4)
N1 0.0138(4) 0.0173(4) 0.0154(4) 0.0014(3) 0.0041(3) 0.0007(3)
N2 0.0118(3) 0.0173(4) 0.0159(4) 0.0005(3) 0.0028(3) 0.0003(3)
N3 0.0135(4) 0.0163(4) 0.0157(4) 0.0006(3) 0.0023(3) -0.0004(3)
N4 0.0124(3) 0.0148(4) 0.0152(4) 0.0002(3) 0.0033(3) 0.0005(3)
C1 0.0194(5) 0.0196(5) 0.0189(5) 0.0030(4) 0.0049(4) 0.0029(4)
C2 0.0271(6) 0.0215(5) 0.0313(6) 0.0060(4) 0.0111(5) 0.0097(4)
C3 0.0249(6) 0.0291(6) 0.0354(7) 0.0081(5) 0.0161(5) 0.0131(5)
C4 0.0189(5) 0.0272(6) 0.0290(6) 0.0069(4) 0.0132(4) 0.0067(4)
C5 0.0135(4) 0.0185(4) 0.0158(4) 0.0022(3) 0.0045(3) 0.0021(3)
C6 0.0115(4) 0.0186(4) 0.0149(4) 0.0012(3) 0.0021(3) -0.0002(3)
C7 0.0141(4) 0.0222(5) 0.0202(5) 0.0034(4) 0.0037(3) -0.0028(4)
C8 0.0187(5) 0.0218(5) 0.0256(5) 0.0042(4) 0.0025(4) -0.0057(4)
C9 0.0199(5) 0.0173(5) 0.0269(5) 0.0022(4) 0.0011(4) -0.0018(4)
C10 0.0145(4) 0.0171(4) 0.0204(5) -0.0003(4) 0.0009(3) 0.0006(3)
C11 0.0249(5) 0.0200(5) 0.0309(6) 0.0078(4) 0.0087(4) 0.0000(4)
C12 0.0190(5) 0.0205(5) 0.0353(6) -0.0004(4) 0.0080(4) 0.0045(4)
C13 0.0166(4) 0.0184(5) 0.0187(5) 0.0018(4) 0.0001(3) -0.0013(3)
C14 0.0260(5) 0.0218(5) 0.0169(5) -0.0018(4) 0.0008(4) -0.0038(4)
C15 0.0303(6) 0.0289(6) 0.0188(5) -0.0058(4) 0.0086(4) -0.0048(5)
C16 0.0215(5) 0.0271(5) 0.0204(5) -0.0046(4) 0.0096(4) -0.0038(4)
C17 0.0142(4) 0.0159(4) 0.0152(4) 0.0005(3) 0.0039(3) -0.0010(3)
C18 0.0126(4) 0.0140(4) 0.0168(4) 0.0006(3) 0.0040(3) 0.0001(3)
C19 0.0138(4) 0.0189(5) 0.0211(5) 0.0011(4) 0.0066(3) -0.0012(3)
C20 0.0132(4) 0.0179(5) 0.0269(5) 0.0005(4) 0.0043(4) -0.0025(3)
C21 0.0155(4) 0.0178(5) 0.0234(5) -0.0019(4) 0.0012(4) -0.0017(3)
C22 0.0151(4) 0.0159(4) 0.0173(4) -0.0008(3) 0.0027(3) 0.0004(3)
C23 0.0160(5) 0.0333(6) 0.0287(6) -0.0034(5) 0.0001(4) -0.0042(4)
C24 0.0212(5) 0.0297(6) 0.0178(5) -0.0057(4) 0.0049(4) -0.0030(4)
P1 0.01460(11) 0.01899(12) 0.02216(13) 0.00175(10) 0.00534(9) -0.00150(9)
F1 0.0497(6) 0.0676(7) 0.0367(5) -0.0236(5) 0.0235(4) -0.0306(5)
F2 0.0389(5) 0.0309(4) 0.0586(6) 0.0193(4) 0.0100(4) -0.0083(4)
F3 0.0515(6) 0.0639(7) 0.0402(5) -0.0278(5) 0.0180(4) -0.0227(5)
F4 0.0338(4) 0.0267(4) 0.0535(5) 0.0140(4) 0.0257(4) 0.0018(3)
F5 0.0163(3) 0.0609(6) 0.0514(6) 0.0231(5) 0.0084(3) 0.0070(4)
F6 0.0181(4) 0.0546(6) 0.0634(7) 0.0204(5) 0.0030(4) 0.0064(4)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.11903(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . N1 . 2.0248(9) yes
Cu1 . N2 . 2.0472(9) yes
Cu1 . N3 . 2.0447(9) yes
Cu1 . N4 . 2.0335(9) yes
N1 . C1 . 1.3461(14) yes
N1 . C5 . 1.3538(13) yes
N2 . C6 . 1.3527(13) yes
N2 . C10 . 1.3469(14) yes
N3 . C13 . 1.3464(14) yes
N3 . C17 . 1.3551(13) yes
N4 . C18 . 1.3581(13) yes
N4 . C22 . 1.3462(14) yes
C1 . C2 . 1.3927(15) yes
C1 . C11 . 1.4958(16) yes
C2 . C3 . 1.3800(18) yes
C2 . H21 . 0.946 no
C3 . C4 . 1.3876(18) yes
C3 . H31 . 0.950 no
C4 . C5 . 1.3894(14) yes
C4 . H41 . 0.937 no
C5 . C6 . 1.4819(15) yes
C6 . C7 . 1.3939(14) yes
C7 . C8 . 1.3878(16) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.3838(16) yes
C8 . H81 . 0.952 no
C9 . C10 . 1.3935(15) yes
C9 . H91 . 0.950 no
C10 . C12 . 1.4978(15) yes
C11 . H113 . 0.943 no
C11 . H112 . 0.953 no
C11 . H111 . 0.964 no
C12 . H123 . 0.947 no
C12 . H122 . 0.953 no
C12 . H121 . 0.963 no
C13 . C14 . 1.3958(16) yes
C13 . C23 . 1.4964(16) yes
C14 . C15 . 1.3801(17) yes
C14 . H141 . 0.959 no
C15 . C16 . 1.3881(17) yes
C15 . H151 . 0.951 no
C16 . C17 . 1.3916(15) yes
C16 . H161 . 0.954 no
C17 . C18 . 1.4800(15) yes
C18 . C19 . 1.3897(14) yes
C19 . C20 . 1.3879(16) yes
C19 . H191 . 0.941 no
C20 . C21 . 1.3846(16) yes
C20 . H201 . 0.945 no
C21 . C22 . 1.3975(15) yes
C21 . H211 . 0.946 no
C22 . C24 . 1.4962(15) yes
C23 . H233 . 0.946 no
C23 . H232 . 0.961 no
C23 . H231 . 0.963 no
C24 . H243 . 0.938 no
C24 . H242 . 0.969 no
C24 . H241 . 0.959 no
P1 . F1 . 1.5981(10) yes
P1 . F2 . 1.5897(9) yes
P1 . F3 . 1.5864(10) yes
P1 . F4 . 1.5935(8) yes
P1 . F5 . 1.5943(9) yes
P1 . F6 . 1.5974(9) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Cu1 . N2 . 81.13(4) yes
N1 . Cu1 . N3 . 127.51(4) yes
N2 . Cu1 . N3 . 114.67(4) yes
N1 . Cu1 . N4 . 125.93(4) yes
N2 . Cu1 . N4 . 132.08(4) yes
N3 . Cu1 . N4 . 81.59(3) yes
Cu1 . N1 . C1 . 126.88(7) yes
Cu1 . N1 . C5 . 114.11(7) yes
C1 . N1 . C5 . 119.00(9) yes
Cu1 . N2 . C6 . 113.60(7) yes
Cu1 . N2 . C10 . 126.97(7) yes
C6 . N2 . C10 . 119.29(9) yes
Cu1 . N3 . C13 . 126.93(7) yes
Cu1 . N3 . C17 . 112.94(7) yes
C13 . N3 . C17 . 119.27(9) yes
Cu1 . N4 . C18 . 113.22(7) yes
Cu1 . N4 . C22 . 127.81(7) yes
C18 . N4 . C22 . 118.78(9) yes
N1 . C1 . C2 . 121.51(10) yes
N1 . C1 . C11 . 116.87(9) yes
C2 . C1 . C11 . 121.62(10) yes
C1 . C2 . C3 . 119.49(11) yes
C1 . C2 . H21 . 119.4 no
C3 . C2 . H21 . 121.1 no
C2 . C3 . C4 . 119.21(11) yes
C2 . C3 . H31 . 120.7 no
C4 . C3 . H31 . 120.1 no
C3 . C4 . C5 . 118.79(11) yes
C3 . C4 . H41 . 120.2 no
C5 . C4 . H41 . 121.0 no
C4 . C5 . N1 . 122.00(10) yes
C4 . C5 . C6 . 122.31(9) yes
N1 . C5 . C6 . 115.69(9) yes
C5 . C6 . N2 . 115.37(9) yes
C5 . C6 . C7 . 122.78(9) yes
N2 . C6 . C7 . 121.86(10) yes
C6 . C7 . C8 . 118.71(10) yes
C6 . C7 . H71 . 119.9 no
C8 . C7 . H71 . 121.4 no
C7 . C8 . C9 . 119.29(10) yes
C7 . C8 . H81 . 120.1 no
C9 . C8 . H81 . 120.6 no
C8 . C9 . C10 . 119.43(10) yes
C8 . C9 . H91 . 121.0 no
C10 . C9 . H91 . 119.6 no
C9 . C10 . N2 . 121.39(10) yes
C9 . C10 . C12 . 121.89(10) yes
N2 . C10 . C12 . 116.72(10) yes
C1 . C11 . H113 . 111.8 no
C1 . C11 . H112 . 110.2 no
H113 . C11 . H112 . 110.0 no
C1 . C11 . H111 . 109.7 no
H113 . C11 . H111 . 108.3 no
H112 . C11 . H111 . 106.7 no
C10 . C12 . H123 . 111.6 no
C10 . C12 . H122 . 110.8 no
H123 . C12 . H122 . 109.9 no
C10 . C12 . H121 . 109.6 no
H123 . C12 . H121 . 108.3 no
H122 . C12 . H121 . 106.6 no
N3 . C13 . C14 . 121.24(10) yes
N3 . C13 . C23 . 117.43(10) yes
C14 . C13 . C23 . 121.32(10) yes
C13 . C14 . C15 . 119.41(11) yes
C13 . C14 . H141 . 120.3 no
C15 . C14 . H141 . 120.2 no
C14 . C15 . C16 . 119.58(11) yes
C14 . C15 . H151 . 119.9 no
C16 . C15 . H151 . 120.6 no
C15 . C16 . C17 . 118.46(11) yes
C15 . C16 . H161 . 120.8 no
C17 . C16 . H161 . 120.7 no
C16 . C17 . N3 . 122.01(10) yes
C16 . C17 . C18 . 122.51(9) yes
N3 . C17 . C18 . 115.48(9) yes
C17 . C18 . N4 . 115.89(8) yes
C17 . C18 . C19 . 122.09(9) yes
N4 . C18 . C19 . 122.01(10) yes
C18 . C19 . C20 . 119.03(10) yes
C18 . C19 . H191 . 120.2 no
C20 . C19 . H191 . 120.8 no
C19 . C20 . C21 . 119.13(10) yes
C19 . C20 . H201 . 120.4 no
C21 . C20 . H201 . 120.5 no
C20 . C21 . C22 . 119.24(10) yes
C20 . C21 . H211 . 121.2 no
C22 . C21 . H211 . 119.5 no
C21 . C22 . N4 . 121.78(10) yes
C21 . C22 . C24 . 120.92(10) yes
N4 . C22 . C24 . 117.28(9) yes
C13 . C23 . H233 . 110.7 no
C13 . C23 . H232 . 110.1 no
H233 . C23 . H232 . 108.9 no
C13 . C23 . H231 . 109.5 no
H233 . C23 . H231 . 109.9 no
H232 . C23 . H231 . 107.7 no
C22 . C24 . H243 . 111.7 no
C22 . C24 . H242 . 108.6 no
H243 . C24 . H242 . 109.5 no
C22 . C24 . H241 . 109.1 no
H243 . C24 . H241 . 110.4 no
H242 . C24 . H241 . 107.4 no
F1 . P1 . F2 . 89.07(6) yes
F1 . P1 . F3 . 179.15(6) yes
F2 . P1 . F3 . 91.08(6) yes
F1 . P1 . F4 . 89.86(6) yes
F2 . P1 . F4 . 178.88(6) yes
F3 . P1 . F4 . 89.99(6) yes
F1 . P1 . F5 . 89.73(6) yes
F2 . P1 . F5 . 89.32(5) yes
F3 . P1 . F5 . 91.11(6) yes
F4 . P1 . F5 . 90.34(5) yes
F1 . P1 . F6 . 89.75(6) yes
F2 . P1 . F6 . 90.95(5) yes
F3 . P1 . F6 . 89.41(6) yes
F4 . P1 . F6 . 89.37(5) yes
F5 . P1 . F6 . 179.41(6) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 10/10/11 at 17:04:46
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 11,X'S) H ( 113,X'S) H ( 112,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 123,X'S) H ( 122,X'S) H ( 121,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 23,X'S) H ( 233,X'S) H ( 232,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 243,X'S) H ( 242,X'S) H ( 241,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 10/10/11 at 17:04:46
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
# Attachment '- Cu_complex-squeeze.cif'
data_Cu_complex-squeeze
_database_code_depnum_ccdc_archive 'CCDC 885554'
#TrackingRef '- Cu_complex-squeeze.cif'
_audit_creation_date 12-01-04
_audit_creation_method CRYSTALS_ver_14.23
_oxford_structure_analysis_title 'bb164a_123k_0ma in P4/n'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 15.1209(2)
_cell_length_b 15.1209(2)
_cell_length_c 18.2971(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4183.48(12)
_symmetry_cell_setting Tetragonal
_symmetry_space_group_name_H-M 'P 4/n'
_symmetry_space_group_name_Hall '-P 4a'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-y+1/2,x,z
y+1/2,-x,-z
-x+1/2,-y+1/2,z
x+1/2,y+1/2,-z
y,-x+1/2,z
-y,x+1/2,-z
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C101 H84 Cu1 F6 N8 O3 P1
# Dc = 1.32 Fooo = 1660.00 Mu = 3.52 M = 416.58
# Found Formula = C100 H76 Cu1 F6 N8 P1
# Dc = 1.27 FOOO = 1660.00 Mu = 3.47 M = 399.57
_chemical_formula_sum 'C100 H76 Cu1 F6 N8 P1'
_chemical_formula_moiety 'C100 H76 Cu1 N8, F6 P'
_chemical_compound_source ?
_chemical_formula_weight 1598.28
_cell_measurement_reflns_used 8009
_cell_measurement_theta_min 4
_cell_measurement_theta_max 32
_cell_measurement_temperature 123
_exptl_crystal_description plate
_exptl_crystal_colour orange
_exptl_crystal_size_min 0.030
_exptl_crystal_size_mid 0.170
_exptl_crystal_size_max 0.210
_exptl_crystal_density_diffrn 1.27
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1660
_exptl_absorpt_coefficient_mu 0.347
# Sheldrick geometric approximatio 0.94 0.99
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.94
_exptl_absorpt_correction_T_max 0.99
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 123
_diffrn_reflns_number 49103
_reflns_number_total 7090
_diffrn_reflns_av_R_equivalents 0.062
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 7090
# Theoretical number of reflections is about 14133
_diffrn_reflns_theta_min 1.747
_diffrn_reflns_theta_max 31.714
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 31.714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 27
_reflns_limit_h_min -15
_reflns_limit_h_max 15
_reflns_limit_k_min 0
_reflns_limit_k_max 22
_reflns_limit_l_min 0
_reflns_limit_l_max 27
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.35
_refine_diff_density_max 0.48
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns 3503
_refine_ls_number_restraints 27
_refine_ls_number_parameters 276
_oxford_refine_ls_R_factor_ref 0.0413
_refine_ls_wR_factor_ref 0.0465
_refine_ls_goodness_of_fit_ref 1.0236
_refine_ls_shift/su_max 0.0003856
_refine_ls_shift/su_mean 0.0000426
# The values computed from all data
_oxford_reflns_number_all 7074
_refine_ls_R_factor_all 0.0902
_refine_ls_wR_factor_all 0.1193
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 4382
_refine_ls_R_factor_gt 0.0494
_refine_ls_wR_factor_gt 0.0524
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.231 0.211 0.800E-01
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
;
_vrf_PLAT051_I
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 16.88 Perc.
RESPONSE: Checkcif seems not to recognize that P1 is on a special position.
;
# end Validation Reply Form
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.7500 0.2500 0.0000 0.0245 1.0000 Uani S T . . . .
N1 N 0.83167(11) 0.28016(11) 0.08502(8) 0.0245 1.0000 Uani . . . . . .
N2 N 1.04143(12) 0.51115(14) -0.30362(10) 0.0362 1.0000 Uani . . . . . .
C1 C 0.91775(14) 0.30283(14) 0.07886(10) 0.0290 1.0000 Uani . . . . . .
C2 C 0.97332(15) 0.30253(15) 0.14010(11) 0.0340 1.0000 Uani . . . . . .
C3 C 0.93850(15) 0.28230(15) 0.20753(11) 0.0348 1.0000 Uani . . . . . .
C4 C 0.84973(15) 0.26263(14) 0.21439(10) 0.0301 1.0000 Uani . . . . . .
C5 C 0.79763(14) 0.26143(12) 0.15162(9) 0.0241 1.0000 Uani . . . . . .
C6 C 0.94367(14) 0.32949(15) 0.00508(11) 0.0334 1.0000 Uani . . . . . .
C7 C 1.01892(15) 0.36355(16) -0.01820(12) 0.0373 1.0000 Uani . . . . . .
C8 C 1.03093(14) 0.39528(16) -0.09320(12) 0.0362 1.0000 Uani . . . . . .
C9 C 1.09857(16) 0.45362(17) -0.11155(13) 0.0414 1.0000 Uani . . . . . .
C10 C 1.10445(15) 0.49068(16) -0.18071(12) 0.0384 1.0000 Uani . . . . . .
C11 C 1.04177(14) 0.47021(15) -0.23392(11) 0.0336 1.0000 Uani . . . . . .
C12 C 0.97598(14) 0.40912(16) -0.21740(11) 0.0345 1.0000 Uani . . . . . .
C13 C 0.97108(15) 0.37247(16) -0.14872(11) 0.0361 1.0000 Uani . . . . . .
C14 C 1.12023(15) 0.53681(17) -0.33911(12) 0.0379 1.0000 Uani . . . . . .
C15 C 1.19521(17) 0.4838(2) -0.33615(15) 0.0558 1.0000 Uani . . . . . .
C16 C 1.27181(18) 0.5103(3) -0.37208(17) 0.0734 1.0000 Uani . . . . . .
C17 C 1.27391(18) 0.5882(3) -0.41064(16) 0.0701 1.0000 Uani . . . . . .
C18 C 1.19888(19) 0.6398(2) -0.41465(14) 0.0543 1.0000 Uani . . . . . .
C19 C 1.12187(17) 0.61531(17) -0.37933(12) 0.0406 1.0000 Uani . . . . . .
C20 C 0.95878(14) 0.53145(14) -0.33724(12) 0.0326 1.0000 Uani . . . . . .
C21 C 0.89223(15) 0.57273(15) -0.29794(13) 0.0365 1.0000 Uani . . . . . .
C22 C 0.81267(16) 0.59361(16) -0.33161(15) 0.0428 1.0000 Uani . . . . . .
C23 C 0.79879(16) 0.57357(17) -0.40444(16) 0.0463 1.0000 Uani . . . . . .
C24 C 0.86512(17) 0.53274(18) -0.44354(14) 0.0459 1.0000 Uani . . . . . .
C25 C 0.94507(16) 0.51103(15) -0.41018(12) 0.0372 1.0000 Uani . . . . . .
H21 H 1.0343 0.3157 0.1351 0.0433 1.0000 Uiso R . . . . .
H31 H 0.9752 0.2812 0.2485 0.0430 1.0000 Uiso R . . . . .
H41 H 0.8253 0.2499 0.2596 0.0378 1.0000 Uiso R . . . . .
H61 H 0.8996 0.3214 -0.0310 0.0414 1.0000 Uiso R . . . . .
H71 H 1.0676 0.3676 0.0148 0.0464 1.0000 Uiso R . . . . .
H91 H 1.1418 0.4685 -0.0760 0.0492 1.0000 Uiso R . . . . .
H101 H 1.1516 0.5301 -0.1919 0.0459 1.0000 Uiso R . . . . .
H121 H 0.9350 0.3933 -0.2531 0.0431 1.0000 Uiso R . . . . .
H131 H 0.9259 0.3307 -0.1388 0.0442 1.0000 Uiso R . . . . .
H151 H 1.1934 0.4326 -0.3103 0.0652 1.0000 Uiso R . . . . .
H161 H 1.3221 0.4749 -0.3697 0.0882 1.0000 Uiso R . . . . .
H171 H 1.3260 0.6064 -0.4336 0.0844 1.0000 Uiso R . . . . .
H181 H 1.1996 0.6920 -0.4416 0.0671 1.0000 Uiso R . . . . .
H191 H 1.0712 0.6510 -0.3827 0.0523 1.0000 Uiso R . . . . .
H211 H 0.9007 0.5862 -0.2479 0.0452 1.0000 Uiso R . . . . .
H221 H 0.7673 0.6214 -0.3043 0.0544 1.0000 Uiso R . . . . .
H231 H 0.7455 0.5871 -0.4271 0.0560 1.0000 Uiso R . . . . .
H241 H 0.8561 0.5186 -0.4923 0.0540 1.0000 Uiso R . . . . .
H251 H 0.9898 0.4833 -0.4364 0.0474 1.0000 Uiso R . . . . .
P1 P 0.7500 0.7500 -0.12402(8) 0.0385 1.0000 Uani DS TU . 1 -1 .
F1 F 0.7862(3) 0.6885(2) -0.1866(2) 0.1033 0.5000 Uani D U . 1 -1 .
F2 F 0.8400(2) 0.80307(18) -0.1241(3) 0.0780 0.5000 Uani D U . 1 -1 .
F3 F 0.7880(3) 0.6856(2) -0.0657(2) 0.0879 0.5000 Uani D U . 1 -1 .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.03065(16) 0.03065(16) 0.01215(17) 0.0000 0.0000 0.0000
N1 0.0293(8) 0.0278(8) 0.0165(7) 0.0000(6) -0.0007(6) 0.0007(7)
N2 0.0262(9) 0.0522(12) 0.0303(9) 0.0150(8) -0.0017(7) -0.0054(8)
C1 0.0317(10) 0.0338(10) 0.0214(8) -0.0014(7) -0.0007(7) -0.0009(8)
C2 0.0311(11) 0.0431(12) 0.0279(10) -0.0021(9) -0.0058(8) 0.0000(9)
C3 0.0406(12) 0.0399(12) 0.0240(9) -0.0001(8) -0.0110(8) -0.0002(9)
C4 0.0429(12) 0.0320(10) 0.0154(8) 0.0002(7) -0.0044(8) -0.0020(9)
C5 0.0349(10) 0.0223(9) 0.0150(7) -0.0014(6) -0.0016(7) 0.0006(8)
C6 0.0322(10) 0.0475(12) 0.0206(9) 0.0004(9) -0.0017(8) -0.0045(8)
C7 0.0342(11) 0.0500(13) 0.0277(10) 0.0071(9) -0.0066(8) -0.0110(10)
C8 0.0317(11) 0.0495(13) 0.0275(9) 0.0084(9) -0.0046(8) -0.0107(9)
C9 0.0339(12) 0.0559(15) 0.0343(11) 0.0098(10) -0.0088(9) -0.0152(11)
C10 0.0304(11) 0.0502(14) 0.0346(11) 0.0121(10) -0.0051(9) -0.0130(10)
C11 0.0295(11) 0.0446(13) 0.0267(9) 0.0076(9) -0.0017(8) -0.0031(9)
C12 0.0300(11) 0.0470(13) 0.0263(10) 0.0044(9) -0.0059(8) -0.0091(9)
C13 0.0328(11) 0.0488(13) 0.0268(10) 0.0068(9) -0.0028(8) -0.0145(10)
C14 0.0308(11) 0.0554(14) 0.0276(10) 0.0100(10) -0.0036(8) -0.0109(10)
C15 0.0338(13) 0.087(2) 0.0469(14) 0.0286(15) 0.0004(11) -0.0001(13)
C16 0.0282(13) 0.139(3) 0.0530(16) 0.033(2) 0.0010(12) 0.0007(16)
C17 0.0343(14) 0.129(3) 0.0473(15) 0.0355(18) -0.0056(12) -0.0258(16)
C18 0.0545(16) 0.0730(19) 0.0353(12) 0.0165(12) -0.0084(11) -0.0324(14)
C19 0.0447(13) 0.0485(14) 0.0287(10) 0.0042(9) -0.0043(9) -0.0176(11)
C20 0.0292(11) 0.0360(11) 0.0327(10) 0.0087(9) -0.0041(8) -0.0060(9)
C21 0.0328(11) 0.0386(12) 0.0382(11) 0.0052(9) -0.0025(9) -0.0070(9)
C22 0.0321(12) 0.0371(12) 0.0590(15) 0.0094(11) -0.0018(11) -0.0043(9)
C23 0.0332(12) 0.0442(14) 0.0614(16) 0.0137(12) -0.0165(12) -0.0059(10)
C24 0.0474(14) 0.0498(14) 0.0405(13) 0.0043(11) -0.0164(11) -0.0083(12)
C25 0.0371(12) 0.0394(12) 0.0351(11) 0.0046(9) -0.0063(9) -0.0030(9)
P1 0.0304(4) 0.0304(4) 0.0546(7) 0.0000 0.0000 0.0000
F1 0.142(5) 0.076(3) 0.091(3) -0.027(3) 0.039(4) 0.004(3)
F2 0.0313(16) 0.0328(16) 0.170(5) -0.007(3) 0.015(3) -0.0029(13)
F3 0.090(3) 0.068(3) 0.106(3) 0.036(2) -0.040(3) 0.008(2)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.08390(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . N1 4_565 2.0379(15) yes
Cu1 . N1 5_655 2.0379(15) yes
Cu1 . N1 8_645 2.0379(15) yes
Cu1 . N1 . 2.0379(15) yes
N1 . C1 . 1.351(3) yes
N1 . C5 . 1.353(2) yes
N2 . C11 . 1.418(3) yes
N2 . C14 . 1.411(3) yes
N2 . C20 . 1.426(3) yes
C1 . C2 . 1.401(3) yes
C1 . C6 . 1.462(3) yes
C2 . C3 . 1.376(3) yes
C2 . H21 . 0.948 no
C3 . C4 . 1.380(3) yes
C3 . H31 . 0.933 no
C4 . C5 . 1.393(3) yes
C4 . H41 . 0.926 no
C5 . C5 5_655 1.481(4) yes
C6 . C7 . 1.320(3) yes
C6 . H61 . 0.946 no
C7 . C8 . 1.465(3) yes
C7 . H71 . 0.954 no
C8 . C9 . 1.392(3) yes
C8 . C13 . 1.404(3) yes
C9 . C10 . 1.387(3) yes
C9 . H91 . 0.949 no
C10 . C11 . 1.393(3) yes
C10 . H101 . 0.952 no
C11 . C12 . 1.391(3) yes
C12 . C13 . 1.375(3) yes
C12 . H121 . 0.931 no
C13 . H131 . 0.948 no
C14 . C15 . 1.390(4) yes
C14 . C19 . 1.397(3) yes
C15 . C16 . 1.391(4) yes
C15 . H151 . 0.909 no
C16 . C17 . 1.373(5) yes
C16 . H161 . 0.930 no
C17 . C18 . 1.379(5) yes
C17 . H171 . 0.934 no
C18 . C19 . 1.382(3) yes
C18 . H181 . 0.931 no
C19 . H191 . 0.939 no
C20 . C21 . 1.385(3) yes
C20 . C25 . 1.385(3) yes
C21 . C22 . 1.388(3) yes
C21 . H211 . 0.947 no
C22 . C23 . 1.383(4) yes
C22 . H221 . 0.947 no
C23 . C24 . 1.378(4) yes
C23 . H231 . 0.929 no
C24 . C25 . 1.394(3) yes
C24 . H241 . 0.928 no
C25 . H251 . 0.930 no
P1 . F1 . 1.574(4) yes
P1 . F2 . 1.580(3) yes
P1 . F3 . 1.555(3) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 4_565 Cu1 . N1 5_655 125.64(5) yes
N1 4_565 Cu1 . N1 8_645 80.48(9) yes
N1 5_655 Cu1 . N1 8_645 125.64(5) yes
N1 4_565 Cu1 . N1 . 125.64(5) yes
N1 5_655 Cu1 . N1 . 80.48(9) yes
N1 8_645 Cu1 . N1 . 125.64(5) yes
Cu1 . N1 . C1 . 125.25(12) yes
Cu1 . N1 . C5 . 114.21(13) yes
C1 . N1 . C5 . 119.66(16) yes
C11 . N2 . C14 . 122.07(18) yes
C11 . N2 . C20 . 119.02(17) yes
C14 . N2 . C20 . 118.82(17) yes
N1 . C1 . C2 . 120.70(18) yes
N1 . C1 . C6 . 113.90(17) yes
C2 . C1 . C6 . 125.36(19) yes
C1 . C2 . C3 . 119.2(2) yes
C1 . C2 . H21 . 120.4 no
C3 . C2 . H21 . 120.4 no
C2 . C3 . C4 . 120.10(19) yes
C2 . C3 . H31 . 119.7 no
C4 . C3 . H31 . 120.2 no
C3 . C4 . C5 . 118.55(18) yes
C3 . C4 . H41 . 120.9 no
C5 . C4 . H41 . 120.5 no
C5 5_655 C5 . C4 . 123.58(12) yes
C5 5_655 C5 . N1 . 114.76(11) yes
C4 . C5 . N1 . 121.66(19) yes
C1 . C6 . C7 . 129.5(2) yes
C1 . C6 . H61 . 114.9 no
C7 . C6 . H61 . 115.6 no
C6 . C7 . C8 . 122.5(2) yes
C6 . C7 . H71 . 119.1 no
C8 . C7 . H71 . 118.4 no
C7 . C8 . C9 . 121.65(19) yes
C7 . C8 . C13 . 121.17(19) yes
C9 . C8 . C13 . 117.06(19) yes
C8 . C9 . C10 . 121.6(2) yes
C8 . C9 . H91 . 119.4 no
C10 . C9 . H91 . 119.0 no
C9 . C10 . C11 . 120.3(2) yes
C9 . C10 . H101 . 119.8 no
C11 . C10 . H101 . 119.9 no
N2 . C11 . C10 . 122.27(19) yes
N2 . C11 . C12 . 118.88(19) yes
C10 . C11 . C12 . 118.83(19) yes
C11 . C12 . C13 . 120.32(19) yes
C11 . C12 . H121 . 119.6 no
C13 . C12 . H121 . 120.1 no
C8 . C13 . C12 . 121.8(2) yes
C8 . C13 . H131 . 119.3 no
C12 . C13 . H131 . 118.9 no
N2 . C14 . C15 . 120.8(2) yes
N2 . C14 . C19 . 119.4(2) yes
C15 . C14 . C19 . 119.8(2) yes
C14 . C15 . C16 . 119.7(3) yes
C14 . C15 . H151 . 119.2 no
C16 . C15 . H151 . 121.1 no
C15 . C16 . C17 . 120.6(3) yes
C15 . C16 . H161 . 119.5 no
C17 . C16 . H161 . 119.9 no
C16 . C17 . C18 . 119.6(2) yes
C16 . C17 . H171 . 120.2 no
C18 . C17 . H171 . 120.3 no
C17 . C18 . C19 . 121.1(3) yes
C17 . C18 . H181 . 119.9 no
C19 . C18 . H181 . 119.0 no
C14 . C19 . C18 . 119.2(3) yes
C14 . C19 . H191 . 120.6 no
C18 . C19 . H191 . 120.2 no
N2 . C20 . C21 . 120.6(2) yes
N2 . C20 . C25 . 119.9(2) yes
C21 . C20 . C25 . 119.5(2) yes
C20 . C21 . C22 . 120.1(2) yes
C20 . C21 . H211 . 120.0 no
C22 . C21 . H211 . 119.9 no
C21 . C22 . C23 . 120.6(2) yes
C21 . C22 . H221 . 119.6 no
C23 . C22 . H221 . 119.7 no
C22 . C23 . C24 . 119.2(2) yes
C22 . C23 . H231 . 120.9 no
C24 . C23 . H231 . 119.9 no
C23 . C24 . C25 . 120.6(2) yes
C23 . C24 . H241 . 119.7 no
C25 . C24 . H241 . 119.7 no
C24 . C25 . C20 . 120.0(2) yes
C24 . C25 . H251 . 120.7 no
C20 . C25 . H251 . 119.3 no
F1 . P1 . F2 . 90.001(10) yes
F1 . P1 . F3 . 89.997(10) yes
F2 . P1 . F3 . 90.002(10) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 04/01/12 at 15:37:58
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 04/01/12 at 15:37:58
#
#LIST 16
REM PF6
DIST 0.0, 0.01 = MEAN
CONT P(1) TO F(1) P(1) TO F(2) P(1) TO F(3)
ANGLE 90, 0.01 =
CONT F(1) TO P(1) TO F(2) F(1) TO P(1) TO F(3)
CONT F(2) TO P(1) TO F(3)
VIBRA 0.0,0.01 =
CONT P(1) TO F(1) P(1) TO F(2) P(1) TO F(3)
U(IJ)'S 0.0,0.02 =
CONT P(1) TO F(1) P(1) TO F(2) P(1) TO F(3)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE)
REM
REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE)
END
;
# Attachment '- Cu_complex.cif'
data_Cu_complex
_database_code_depnum_ccdc_archive 'CCDC 885555'
#TrackingRef '- Cu_complex.cif'
_audit_creation_date 12-01-03
_audit_creation_method CRYSTALS_ver_14.23
_oxford_structure_analysis_title 'bb164a_123k_0ma in P4/n'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 15.1209(2)
_cell_length_b 15.1209(2)
_cell_length_c 18.2971(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4183.48(12)
_symmetry_cell_setting Tetragonal
_symmetry_space_group_name_H-M 'P 4/n'
_symmetry_space_group_name_Hall '-P 4a'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-y+1/2,x,z
y+1/2,-x,-z
-x+1/2,-y+1/2,z
x+1/2,y+1/2,-z
y,-x+1/2,z
-y,x+1/2,-z
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C101 H84 Cu1 F6 N8 O3 P1
# Dc = 1.32 Fooo = 1720.00 Mu = 3.52 M = 416.58
# Found Formula = C101 H76 Cu1 F6 N8 O3 P1
# Dc = 1.32 FOOO = 1720.00 Mu = 3.52 M = 414.57
_chemical_formula_sum 'C101 H84 Cu1 F6 N8 O3 P1'
_chemical_formula_moiety 'C100 H76 Cu1 N8 O3, F6 P, C H4 O, 2(H2 O)'
_chemical_compound_source ?
_chemical_formula_weight 1666.32
_cell_measurement_reflns_used 8009
_cell_measurement_theta_min 4
_cell_measurement_theta_max 32
_cell_measurement_temperature 123
_exptl_crystal_description plate
_exptl_crystal_colour orange
_exptl_crystal_size_min 0.030
_exptl_crystal_size_mid 0.170
_exptl_crystal_size_max 0.210
_exptl_crystal_density_diffrn 1.316
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1720
_exptl_absorpt_coefficient_mu 0.352
# Sheldrick geometric approximatio 0.94 0.99
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.94
_exptl_absorpt_correction_T_max 0.99
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 123
_diffrn_reflns_number 49103
_reflns_number_total 7090
_diffrn_reflns_av_R_equivalents 0.062
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 7090
# Theoretical number of reflections is about 14133
_diffrn_reflns_theta_min 1.747
_diffrn_reflns_theta_max 31.714
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 31.714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 26
_reflns_limit_h_min -15
_reflns_limit_h_max 15
_reflns_limit_k_min 0
_reflns_limit_k_max 22
_reflns_limit_l_min 0
_reflns_limit_l_max 27
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.41
_refine_diff_density_max 0.64
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns 3509
_refine_ls_number_restraints 513
_refine_ls_number_parameters 321
_oxford_refine_ls_R_factor_ref 0.0453
_refine_ls_wR_factor_ref 0.0472
_refine_ls_goodness_of_fit_ref 1.0460
_refine_ls_shift/su_max 0.0084530
_refine_ls_shift/su_mean 0.0003181
# The values computed from all data
_oxford_reflns_number_all 7074
_refine_ls_R_factor_all 0.0965
_refine_ls_wR_factor_all 0.1233
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 4386
_refine_ls_R_factor_gt 0.0535
_refine_ls_wR_factor_gt 0.0533
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.231 0.211 0.800E-01
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
;
_vrf_PLAT051_I
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 16.88 Perc.
RESPONSE: Checkcif seems not to recognize that P1 is on a special position.
;
# end Validation Reply Form
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.7500 0.2500 0.0000 0.0245 1.0000 Uani S T . . . .
N1 N 0.83173(10) 0.28017(10) 0.08504(8) 0.0248 1.0000 Uani . . . . . .
N2 N 1.04150(11) 0.51116(13) -0.30367(9) 0.0365 1.0000 Uani . . . . . .
C1 C 0.91776(13) 0.30294(13) 0.07889(10) 0.0291 1.0000 Uani . . . . . .
C2 C 0.97336(14) 0.30262(14) 0.14011(11) 0.0344 1.0000 Uani . . . . . .
C3 C 0.93844(14) 0.28227(14) 0.20756(11) 0.0352 1.0000 Uani . . . . . .
C4 C 0.84984(14) 0.26269(13) 0.21434(9) 0.0304 1.0000 Uani . . . . . .
C5 C 0.79754(13) 0.26145(11) 0.15167(9) 0.0241 1.0000 Uani . . . . . .
C6 C 0.94357(13) 0.32948(14) 0.00508(11) 0.0337 1.0000 Uani . . . . . .
C7 C 1.01895(14) 0.36353(15) -0.01821(11) 0.0375 1.0000 Uani . . . . . .
C8 C 1.03095(14) 0.39523(15) -0.09324(11) 0.0363 1.0000 Uani . . . . . .
C9 C 1.09858(15) 0.45353(16) -0.11173(12) 0.0414 1.0000 Uani . . . . . .
C10 C 1.10455(14) 0.49068(15) -0.18066(12) 0.0386 1.0000 Uani . . . . . .
C11 C 1.04175(13) 0.47010(14) -0.23389(11) 0.0335 1.0000 Uani . . . . . .
C12 C 0.97604(13) 0.40921(15) -0.21738(11) 0.0348 1.0000 Uani . . . . . .
C13 C 0.97115(14) 0.37246(15) -0.14876(11) 0.0366 1.0000 Uani . . . . . .
C14 C 1.12019(14) 0.53680(16) -0.33908(11) 0.0382 1.0000 Uani . . . . . .
C15 C 1.19521(16) 0.4839(2) -0.33607(14) 0.0560 1.0000 Uani . . . . . .
C16 C 1.27178(17) 0.5104(3) -0.37197(15) 0.0733 1.0000 Uani . . . . . .
C17 C 1.27399(17) 0.5882(2) -0.41062(15) 0.0705 1.0000 Uani . . . . . .
C18 C 1.19879(17) 0.63966(19) -0.41469(13) 0.0543 1.0000 Uani . . . . . .
C19 C 1.12187(16) 0.61537(16) -0.37926(11) 0.0408 1.0000 Uani . . . . . .
C20 C 0.95884(13) 0.53137(14) -0.33715(11) 0.0328 1.0000 Uani . . . . . .
C21 C 0.89226(14) 0.57260(14) -0.29797(12) 0.0367 1.0000 Uani . . . . . .
C22 C 0.81259(15) 0.59354(15) -0.33164(14) 0.0427 1.0000 Uani . . . . . .
C23 C 0.79854(15) 0.57346(15) -0.40444(15) 0.0463 1.0000 Uani . . . . . .
C24 C 0.86524(16) 0.53280(16) -0.44363(13) 0.0462 1.0000 Uani . . . . . .
C25 C 0.94514(14) 0.51098(14) -0.41017(12) 0.0374 1.0000 Uani . . . . . .
H21 H 1.0344 0.3158 0.1351 0.0433 1.0000 Uiso R . . . . .
H31 H 0.9752 0.2812 0.2485 0.0430 1.0000 Uiso R . . . . .
H41 H 0.8254 0.2500 0.2595 0.0378 1.0000 Uiso R . . . . .
H61 H 0.8995 0.3214 -0.0310 0.0414 1.0000 Uiso R . . . . .
H71 H 1.0676 0.3676 0.0148 0.0464 1.0000 Uiso R . . . . .
H91 H 1.1418 0.4684 -0.0762 0.0492 1.0000 Uiso R . . . . .
H101 H 1.1517 0.5301 -0.1918 0.0459 1.0000 Uiso R . . . . .
H121 H 0.9351 0.3934 -0.2530 0.0431 1.0000 Uiso R . . . . .
H131 H 0.9259 0.3307 -0.1388 0.0442 1.0000 Uiso R . . . . .
H151 H 1.1934 0.4327 -0.3102 0.0652 1.0000 Uiso R . . . . .
H161 H 1.3220 0.4750 -0.3696 0.0882 1.0000 Uiso R . . . . .
H171 H 1.3261 0.6064 -0.4335 0.0844 1.0000 Uiso R . . . . .
H181 H 1.1995 0.6919 -0.4416 0.0671 1.0000 Uiso R . . . . .
H191 H 1.0712 0.6511 -0.3826 0.0523 1.0000 Uiso R . . . . .
H211 H 0.9008 0.5860 -0.2479 0.0452 1.0000 Uiso R . . . . .
H221 H 0.7672 0.6213 -0.3043 0.0544 1.0000 Uiso R . . . . .
H231 H 0.7452 0.5870 -0.4271 0.0560 1.0000 Uiso R . . . . .
H241 H 0.8562 0.5186 -0.4924 0.0540 1.0000 Uiso R . . . . .
H251 H 0.9899 0.4833 -0.4364 0.0474 1.0000 Uiso R . . . . .
P1 P 0.7500 0.7500 -0.12417(7) 0.0383 1.0000 Uani DS TU . 1 -1 .
F1 F 0.7858(2) 0.6887(2) -0.1869(2) 0.1030 0.5000 Uani D U . 1 -1 .
F2 F 0.84000(17) 0.80321(16) -0.1246(2) 0.0791 0.5000 Uani D U . 1 -1 .
F3 F 0.7886(2) 0.68536(18) -0.0660(2) 0.0890 0.5000 Uani D U . 1 -1 .
O1 O 0.7508(8) 0.7502(9) 0.09193(18) 0.0396 0.2500 Uani . U . . . .
C26 C 0.7612(6) 0.7984(5) 0.1953(5) 0.0496 0.2500 Uani . U . 2 -2 .
O2 O 0.7258(4) 0.7406(8) 0.2487(3) 0.0599 0.2500 Uani . U . 2 -2 .
O3 O 0.7007(7) 0.7137(7) 0.4324(6) 0.0564 0.1250 Uani . U . 3 -3 .
O4 O 0.6957(7) 0.6466(7) 0.4174(6) 0.0508 0.1250 Uani . U . 3 -3 .
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
Cu1 0.03069(14) 0.03069(14) 0.01220(16) 0.0000 0.0000 0.0000
N1 0.0298(5) 0.0277(6) 0.0168(5) 0.0001(5) -0.0004(5) 0.0009(5)
N2 0.0268(5) 0.0527(7) 0.0300(6) 0.0143(6) -0.0018(5) -0.0056(6)
C1 0.0311(5) 0.0341(7) 0.0220(6) -0.0011(6) -0.0007(6) -0.0011(6)
C2 0.0318(6) 0.0434(7) 0.0281(6) -0.0023(6) -0.0060(6) 0.0000(6)
C3 0.0416(6) 0.0398(7) 0.0241(6) 0.0005(6) -0.0111(6) -0.0002(6)
C4 0.0441(6) 0.0318(7) 0.0155(6) 0.0000(6) -0.0039(6) -0.0015(6)
C5 0.0348(5) 0.0225(6) 0.0150(5) -0.0017(5) -0.0017(5) 0.0006(6)
C6 0.0327(5) 0.0472(7) 0.0213(6) 0.0005(6) -0.0017(6) -0.0047(6)
C7 0.0345(6) 0.0502(8) 0.0278(7) 0.0074(6) -0.0071(6) -0.0107(7)
C8 0.0318(6) 0.0492(7) 0.0279(6) 0.0084(6) -0.0043(6) -0.0102(6)
C9 0.0336(6) 0.0561(8) 0.0345(7) 0.0098(7) -0.0093(6) -0.0148(7)
C10 0.0303(6) 0.0508(8) 0.0346(7) 0.0126(7) -0.0048(6) -0.0135(7)
C11 0.0296(6) 0.0441(7) 0.0267(6) 0.0080(6) -0.0014(6) -0.0026(6)
C12 0.0303(6) 0.0476(7) 0.0264(6) 0.0048(6) -0.0059(6) -0.0099(6)
C13 0.0332(6) 0.0489(7) 0.0278(7) 0.0069(6) -0.0032(6) -0.0148(6)
C14 0.0311(6) 0.0560(8) 0.0275(6) 0.0098(7) -0.0038(6) -0.0104(7)
C15 0.0340(6) 0.0874(8) 0.0465(8) 0.0277(8) 0.0009(7) 0.0005(7)
C16 0.0292(6) 0.1377(9) 0.0531(8) 0.0331(8) 0.0007(7) 0.0007(8)
C17 0.0350(6) 0.1291(9) 0.0474(8) 0.0353(8) -0.0057(7) -0.0256(8)
C18 0.0549(6) 0.0734(8) 0.0345(7) 0.0162(7) -0.0083(7) -0.0330(7)
C19 0.0452(6) 0.0483(8) 0.0288(7) 0.0041(7) -0.0044(6) -0.0171(7)
C20 0.0294(6) 0.0360(7) 0.0330(7) 0.0084(6) -0.0044(6) -0.0058(6)
C21 0.0324(6) 0.0399(7) 0.0379(7) 0.0056(7) -0.0018(6) -0.0067(6)
C22 0.0332(6) 0.0366(7) 0.0583(8) 0.0090(7) -0.0012(7) -0.0039(6)
C23 0.0328(6) 0.0441(8) 0.0618(8) 0.0138(7) -0.0163(7) -0.0059(7)
C24 0.0472(6) 0.0503(8) 0.0411(7) 0.0047(7) -0.0159(7) -0.0088(7)
C25 0.0369(6) 0.0402(7) 0.0352(7) 0.0044(7) -0.0061(6) -0.0029(7)
P1 0.0306(3) 0.0306(3) 0.0539(6) 0.0000 0.0000 0.0000
F1 0.1427(7) 0.0782(9) 0.0883(9) -0.0271(9) 0.0394(9) 0.0041(9)
F2 0.0340(6) 0.0323(8) 0.1710(9) -0.0067(9) 0.0190(9) -0.0032(8)
F3 0.0891(6) 0.0691(9) 0.1087(9) 0.0383(8) -0.0387(9) 0.0108(8)
O1 0.0481(6) 0.0366(9) 0.0341(8) 0.0068(9) 0.0258(9) 0.0036(9)
C26 0.0635(7) 0.0249(9) 0.0604(9) -0.0092(9) 0.0250(9) -0.0100(9)
O2 0.0539(7) 0.0635(9) 0.0623(9) 0.0118(9) 0.0499(9) 0.0067(9)
O3 0.0585(7) 0.0635(9) 0.0471(9) 0.0009(9) 0.0311(9) -0.0117(9)
O4 0.0647(7) 0.0518(9) 0.0361(9) 0.0132(9) 0.0199(9) 0.0213(9)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.08417(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . N1 4_565 2.0386(15) yes
Cu1 . N1 8_645 2.0386(15) yes
Cu1 . N1 5_655 2.0386(15) yes
Cu1 . N1 . 2.0386(15) yes
N1 . C1 . 1.350(2) yes
N1 . C5 . 1.354(2) yes
N2 . C11 . 1.420(3) yes
N2 . C14 . 1.409(3) yes
N2 . C20 . 1.425(3) yes
C1 . C2 . 1.401(3) yes
C1 . C6 . 1.462(3) yes
C2 . C3 . 1.377(3) yes
C2 . H21 . 0.948 no
C3 . C4 . 1.378(3) yes
C3 . H31 . 0.933 no
C4 . C5 . 1.393(2) yes
C4 . H41 . 0.926 no
C5 . C5 5_655 1.479(4) yes
C6 . C7 . 1.321(3) yes
C6 . H61 . 0.946 no
C7 . C8 . 1.465(3) yes
C7 . H71 . 0.954 no
C8 . C9 . 1.392(3) yes
C8 . C13 . 1.403(3) yes
C9 . C10 . 1.383(3) yes
C9 . H91 . 0.949 no
C10 . C11 . 1.395(3) yes
C10 . H101 . 0.952 no
C11 . C12 . 1.388(3) yes
C12 . C13 . 1.375(3) yes
C12 . H121 . 0.931 no
C13 . H131 . 0.948 no
C14 . C15 . 1.389(3) yes
C14 . C19 . 1.397(3) yes
C15 . C16 . 1.390(3) yes
C15 . H151 . 0.909 no
C16 . C17 . 1.373(4) yes
C16 . H161 . 0.930 no
C17 . C18 . 1.380(4) yes
C17 . H171 . 0.934 no
C18 . C19 . 1.381(3) yes
C18 . H181 . 0.931 no
C19 . H191 . 0.939 no
C20 . C21 . 1.384(3) yes
C20 . C25 . 1.387(3) yes
C21 . C22 . 1.389(3) yes
C21 . H211 . 0.947 no
C22 . C23 . 1.383(4) yes
C22 . H221 . 0.947 no
C23 . C24 . 1.382(4) yes
C23 . H231 . 0.929 no
C24 . C25 . 1.394(3) yes
C24 . H241 . 0.928 no
C25 . H251 . 0.930 no
P1 . F1 . 1.570(4) yes
P1 . F2 . 1.581(3) yes
P1 . F3 . 1.559(3) yes
C26 . O2 . 1.416(10) yes
O3 . O4 . 1.054(14) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 4_565 Cu1 . N1 8_645 80.50(8) yes
N1 4_565 Cu1 . N1 5_655 125.63(5) yes
N1 8_645 Cu1 . N1 5_655 125.63(5) yes
N1 4_565 Cu1 . N1 . 125.63(5) yes
N1 8_645 Cu1 . N1 . 125.63(5) yes
N1 5_655 Cu1 . N1 . 80.50(8) yes
Cu1 . N1 . C1 . 125.27(12) yes
Cu1 . N1 . C5 . 114.14(12) yes
C1 . N1 . C5 . 119.73(15) yes
C11 . N2 . C14 . 122.11(17) yes
C11 . N2 . C20 . 118.86(16) yes
C14 . N2 . C20 . 118.94(16) yes
N1 . C1 . C2 . 120.72(17) yes
N1 . C1 . C6 . 113.83(16) yes
C2 . C1 . C6 . 125.41(18) yes
C1 . C2 . C3 . 119.17(19) yes
C1 . C2 . H21 . 120.4 no
C3 . C2 . H21 . 120.4 no
C2 . C3 . C4 . 120.11(18) yes
C2 . C3 . H31 . 119.7 no
C4 . C3 . H31 . 120.2 no
C3 . C4 . C5 . 118.74(17) yes
C3 . C4 . H41 . 120.9 no
C5 . C4 . H41 . 120.4 no
C5 5_655 C5 . C4 . 123.72(12) yes
C5 5_655 C5 . N1 . 114.84(11) yes
C4 . C5 . N1 . 121.44(18) yes
C1 . C6 . C7 . 129.43(19) yes
C1 . C6 . H61 . 114.9 no
C7 . C6 . H61 . 115.6 no
C6 . C7 . C8 . 122.44(19) yes
C6 . C7 . H71 . 119.1 no
C8 . C7 . H71 . 118.4 no
C7 . C8 . C9 . 121.73(18) yes
C7 . C8 . C13 . 121.21(18) yes
C9 . C8 . C13 . 116.94(18) yes
C8 . C9 . C10 . 121.78(19) yes
C8 . C9 . H91 . 119.3 no
C10 . C9 . H91 . 118.9 no
C9 . C10 . C11 . 120.09(19) yes
C9 . C10 . H101 . 119.9 no
C11 . C10 . H101 . 120.0 no
N2 . C11 . C10 . 122.14(18) yes
N2 . C11 . C12 . 118.95(18) yes
C10 . C11 . C12 . 118.89(18) yes
C11 . C12 . C13 . 120.36(18) yes
C11 . C12 . H121 . 119.6 no
C13 . C12 . H121 . 120.0 no
C8 . C13 . C12 . 121.82(19) yes
C8 . C13 . H131 . 119.3 no
C12 . C13 . H131 . 118.9 no
N2 . C14 . C15 . 120.9(2) yes
N2 . C14 . C19 . 119.4(2) yes
C15 . C14 . C19 . 119.7(2) yes
C14 . C15 . C16 . 119.7(3) yes
C14 . C15 . H151 . 119.2 no
C16 . C15 . H151 . 121.1 no
C15 . C16 . C17 . 120.7(3) yes
C15 . C16 . H161 . 119.5 no
C17 . C16 . H161 . 119.8 no
C16 . C17 . C18 . 119.4(2) yes
C16 . C17 . H171 . 120.3 no
C18 . C17 . H171 . 120.3 no
C17 . C18 . C19 . 121.2(2) yes
C17 . C18 . H181 . 119.8 no
C19 . C18 . H181 . 118.9 no
C14 . C19 . C18 . 119.2(2) yes
C14 . C19 . H191 . 120.6 no
C18 . C19 . H191 . 120.2 no
N2 . C20 . C21 . 120.79(19) yes
N2 . C20 . C25 . 119.84(19) yes
C21 . C20 . C25 . 119.37(19) yes
C20 . C21 . C22 . 120.2(2) yes
C20 . C21 . H211 . 119.9 no
C22 . C21 . H211 . 119.8 no
C21 . C22 . C23 . 120.7(2) yes
C21 . C22 . H221 . 119.7 no
C23 . C22 . H221 . 119.6 no
C22 . C23 . C24 . 119.0(2) yes
C22 . C23 . H231 . 121.0 no
C24 . C23 . H231 . 120.0 no
C23 . C24 . C25 . 120.7(2) yes
C23 . C24 . H241 . 119.6 no
C25 . C24 . H241 . 119.7 no
C24 . C25 . C20 . 120.0(2) yes
C24 . C25 . H251 . 120.7 no
C20 . C25 . H251 . 119.3 no
F1 . P1 . F2 . 90.000(10) yes
F1 . P1 . F3 . 89.998(10) yes
F2 . P1 . F3 . 90.002(10) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 03/01/12 at 20:50:13
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 03/01/12 at 20:50:13
#
#LIST 16
REM PF6
DIST 0.0, 0.01 = MEAN
CONT P(1) TO F(1) P(1) TO F(2) P(1) TO F(3)
ANGLE 90, 0.01 =
CONT F(1) TO P(1) TO F(2) F(1) TO P(1) TO F(3)
CONT F(2) TO P(1) TO F(3)
VIBRA 0.0,0.01 =
CONT P(1) TO F(1) P(1) TO F(2) P(1) TO F(3)
U(IJ)'S 0.0,0.02 =
CONT P(1) TO F(1) P(1) TO F(2) P(1) TO F(3)
REM SOLVENT
VIBRA 0.0,0.01 =
CONT O(1) TO C(26) O(1) TO O(2) O(1) TO O(3) O(1) TO O(4)
CONT C(26) TO O(2) C(26) TO O(3) C(26) TO O(4)
CONT O(2) TO O(3) O(2) TO O(4)
CONT O(3) TO O(4)
U(IJ)'S 0.0,0.02 =
CONT O(1) TO C(26) O(1) TO O(2) O(1) TO O(3) O(1) TO O(4)
CONT C(26) TO O(2) C(26) TO O(3) C(26) TO O(4)
CONT O(2) TO O(3) O(2) TO O(4)
CONT O(3) TO O(4)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE)
LIMIT 0.00100000 U[ISO]
LIMIT 0.00100000 X
LIMIT 0.00100000 Y
LIMIT 0.00100000 Z
LIMIT 0.00100000 U[11]
LIMIT 0.00100000 U[22]
LIMIT 0.00100000 U[33]
LIMIT 0.00100000 U[12]
LIMIT 0.00100000 U[13]
LIMIT 0.00100000 U[23]
LIMIT 0.00100000 OCC
REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE)
END
;
# Attachment '- Ligand.cif'
data_Ligand
_database_code_depnum_ccdc_archive 'CCDC 885556'
#TrackingRef '- Ligand.cif'
_audit_creation_date 11-12-10
_audit_creation_method CRYSTALS_ver_14.23
_oxford_structure_analysis_title 'uba15a in Pbca'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 8.9360(3)
_cell_length_b 15.3904(5)
_cell_length_c 26.8164(9)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3688.0(2)
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M 'P b c a'
_symmetry_space_group_name_Hall '-P 2ac 2ab'
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+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C40 H70 N2
# Dc = 1.04 Fooo = 1464.00 Mu = 4.33 M = 289.50
# Found Formula = C50 H38 N4
# Dc = 1.25 FOOO = 1464.00 Mu = 5.65 M = 347.44
_chemical_formula_sum 'C50 H38 N4'
_chemical_formula_moiety 'C50 H38 N4'
_chemical_compound_source ?
_chemical_formula_weight 694.88
_cell_measurement_reflns_used 0
_cell_measurement_theta_min 0
_cell_measurement_theta_max 0
_cell_measurement_temperature 100
_exptl_crystal_description plate
_exptl_crystal_colour yellow
_exptl_crystal_size_min 0.020
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_max 0.220
_exptl_crystal_density_diffrn 1.251
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1464
_exptl_absorpt_coefficient_mu 0.565
# Sheldrick geometric approximatio 0.95 0.99
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.95
_exptl_absorpt_correction_T_max 0.99
_diffrn_measurement_device_type 'Bruker SMART'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54178
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SMART (Siemens, 1993)'
_computing_cell_refinement 'SAINT (Siemens ,1995)'
_computing_data_reduction 'SAINT (Siemens ,1995)'
_computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 100
_diffrn_reflns_number 35364
_reflns_number_total 3377
_diffrn_reflns_av_R_equivalents 0.068
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 3377
# Theoretical number of reflections is about 6786
_diffrn_reflns_theta_min 3.296
_diffrn_reflns_theta_max 68.471
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 67.102
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_limit_l_max 31
_reflns_limit_h_min 0
_reflns_limit_h_max 10
_reflns_limit_k_min 0
_reflns_limit_k_max 18
_reflns_limit_l_min 0
_reflns_limit_l_max 32
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.28
_refine_diff_density_max 0.22
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_refine_ls_number_reflns 2724
_refine_ls_number_restraints 0
_refine_ls_number_parameters 244
_oxford_refine_ls_R_factor_ref 0.0478
_refine_ls_wR_factor_ref 0.0384
_refine_ls_goodness_of_fit_ref 1.0410
_refine_ls_shift/su_max 0.0005364
_refine_ls_shift/su_mean 0.0000435
# The values computed from all data
_oxford_reflns_number_all 3362
_refine_ls_R_factor_all 0.0629
_refine_ls_wR_factor_all 0.0554
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 2724
_refine_ls_R_factor_gt 0.0478
_refine_ls_wR_factor_gt 0.0384
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.284 0.297 0.145
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Siemens Industrial Automation, Inc (1993).
SMART: Area-Detector Software Package; Madison, WI.
Siemens Industrial Automation, Inc (1995).
SAINT: Area-Detector Integration Software.; Madison, WI.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Sheldrick, G. M. (2008). Acta Cryst A64, 112-122.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
N1 N 0.07390(14) 0.60158(8) 0.02224(4) 0.0193 1.0000 Uani . . . . . .
N2 N 0.04242(15) 1.07410(8) 0.18803(4) 0.0218 1.0000 Uani . . . . . .
C1 C 0.07132(16) 0.52497(9) -0.00168(5) 0.0184 1.0000 Uani . . . . . .
C2 C 0.19393(17) 0.49296(10) -0.02813(6) 0.0210 1.0000 Uani . . . . . .
C3 C 0.32298(17) 0.54241(10) -0.02990(6) 0.0230 1.0000 Uani . . . . . .
C4 C 0.32727(17) 0.62120(11) -0.00522(6) 0.0225 1.0000 Uani . . . . . .
C5 C 0.20075(16) 0.64932(10) 0.02059(5) 0.0198 1.0000 Uani . . . . . .
C6 C 0.20186(18) 0.73245(10) 0.04735(6) 0.0215 1.0000 Uani . . . . . .
C7 C 0.09260(16) 0.75812(10) 0.07808(5) 0.0206 1.0000 Uani . . . . . .
C8 C 0.08505(16) 0.83924(10) 0.10623(5) 0.0197 1.0000 Uani . . . . . .
C9 C 0.16635(16) 0.91379(10) 0.09309(6) 0.0207 1.0000 Uani . . . . . .
C10 C 0.15263(17) 0.99023(10) 0.11983(6) 0.0205 1.0000 Uani . . . . . .
C11 C 0.05878(17) 0.99458(10) 0.16138(5) 0.0199 1.0000 Uani . . . . . .
C12 C -0.01945(17) 0.92020(10) 0.17559(6) 0.0224 1.0000 Uani . . . . . .
C13 C -0.00841(18) 0.84440(10) 0.14798(6) 0.0222 1.0000 Uani . . . . . .
C14 C 0.03326(17) 1.07222(10) 0.24081(5) 0.0207 1.0000 Uani . . . . . .
C15 C 0.12544(17) 1.01651(10) 0.26805(6) 0.0219 1.0000 Uani . . . . . .
C16 C 0.11676(17) 1.01425(11) 0.31953(6) 0.0236 1.0000 Uani . . . . . .
C17 C 0.01724(18) 1.06739(11) 0.34476(6) 0.0252 1.0000 Uani . . . . . .
C18 C -0.07468(18) 1.12291(11) 0.31781(6) 0.0242 1.0000 Uani . . . . . .
C19 C -0.06723(17) 1.12540(10) 0.26627(6) 0.0226 1.0000 Uani . . . . . .
C20 C 0.00931(17) 1.15147(10) 0.16156(5) 0.0210 1.0000 Uani . . . . . .
C21 C 0.06668(17) 1.23103(10) 0.17758(6) 0.0236 1.0000 Uani . . . . . .
C22 C 0.03248(18) 1.30668(10) 0.15206(6) 0.0272 1.0000 Uani . . . . . .
C23 C -0.05775(19) 1.30425(11) 0.11006(6) 0.0301 1.0000 Uani . . . . . .
C24 C -0.1142(2) 1.22517(11) 0.09385(6) 0.0295 1.0000 Uani . . . . . .
C25 C -0.08171(18) 1.14953(11) 0.11950(6) 0.0251 1.0000 Uani . . . . . .
H21 H 0.1865 0.4378 -0.0448 0.0242 1.0000 Uiso R . . . . .
H31 H 0.4095 0.5237 -0.0483 0.0277 1.0000 Uiso R . . . . .
H41 H 0.4157 0.6548 -0.0063 0.0267 1.0000 Uiso R . . . . .
H61 H 0.2894 0.7700 0.0426 0.0264 1.0000 Uiso R . . . . .
H71 H 0.0103 0.7200 0.0831 0.0244 1.0000 Uiso R . . . . .
H91 H 0.2302 0.9108 0.0643 0.0255 1.0000 Uiso R . . . . .
H101 H 0.2068 1.0424 0.1099 0.0243 1.0000 Uiso R . . . . .
H121 H -0.0842 0.9213 0.2047 0.0268 1.0000 Uiso R . . . . .
H131 H -0.0662 0.7947 0.1575 0.0269 1.0000 Uiso R . . . . .
H151 H 0.1961 0.9800 0.2507 0.0252 1.0000 Uiso R . . . . .
H161 H 0.1796 0.9755 0.3378 0.0290 1.0000 Uiso R . . . . .
H171 H 0.0104 1.0657 0.3805 0.0284 1.0000 Uiso R . . . . .
H181 H -0.1429 1.1600 0.3355 0.0280 1.0000 Uiso R . . . . .
H191 H -0.1298 1.1643 0.2479 0.0270 1.0000 Uiso R . . . . .
H211 H 0.1275 1.2320 0.2063 0.0281 1.0000 Uiso R . . . . .
H221 H 0.0701 1.3617 0.1634 0.0328 1.0000 Uiso R . . . . .
H231 H -0.0805 1.3555 0.0920 0.0353 1.0000 Uiso R . . . . .
H241 H -0.1757 1.2237 0.0646 0.0334 1.0000 Uiso R . . . . .
H251 H -0.1213 1.0942 0.1086 0.0291 1.0000 Uiso 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
N1 0.0194(6) 0.0215(7) 0.0168(6) 0.0001(5) -0.0013(5) 0.0003(5)
N2 0.0292(7) 0.0175(7) 0.0187(6) -0.0007(5) -0.0011(5) 0.0031(6)
C1 0.0207(7) 0.0201(8) 0.0143(7) 0.0007(6) -0.0017(6) 0.0010(6)
C2 0.0214(7) 0.0219(8) 0.0197(7) -0.0011(6) 0.0002(6) 0.0005(6)
C3 0.0195(8) 0.0271(8) 0.0223(8) -0.0031(7) 0.0030(6) 0.0018(6)
C4 0.0195(8) 0.0258(8) 0.0223(8) -0.0005(7) 0.0010(6) -0.0029(6)
C5 0.0195(7) 0.0229(8) 0.0171(7) 0.0022(6) -0.0019(6) -0.0004(6)
C6 0.0220(8) 0.0212(8) 0.0213(8) 0.0000(7) -0.0020(6) -0.0015(7)
C7 0.0205(7) 0.0210(8) 0.0202(8) 0.0013(6) -0.0023(6) -0.0012(6)
C8 0.0181(7) 0.0208(8) 0.0202(7) -0.0014(6) -0.0036(6) 0.0011(6)
C9 0.0193(8) 0.0240(8) 0.0186(7) -0.0007(6) -0.0013(6) 0.0019(6)
C10 0.0208(8) 0.0205(8) 0.0203(8) 0.0011(6) -0.0022(6) -0.0003(6)
C11 0.0224(8) 0.0179(8) 0.0193(7) -0.0008(6) -0.0045(6) 0.0029(6)
C12 0.0221(8) 0.0235(8) 0.0217(7) -0.0004(6) 0.0024(6) 0.0019(6)
C13 0.0215(8) 0.0201(8) 0.0249(8) 0.0002(6) 0.0006(6) -0.0012(7)
C14 0.0222(8) 0.0191(7) 0.0207(7) -0.0010(6) -0.0013(6) -0.0029(6)
C15 0.0208(7) 0.0206(8) 0.0242(8) -0.0015(7) -0.0001(6) 0.0007(6)
C16 0.0208(8) 0.0254(9) 0.0247(8) 0.0033(7) -0.0037(6) -0.0015(7)
C17 0.0265(8) 0.0296(9) 0.0195(7) 0.0002(7) 0.0009(7) -0.0038(7)
C18 0.0225(8) 0.0262(8) 0.0238(8) -0.0047(7) 0.0023(7) -0.0013(7)
C19 0.0195(7) 0.0233(8) 0.0249(8) -0.0006(6) -0.0024(7) -0.0003(7)
C20 0.0214(8) 0.0197(8) 0.0218(7) -0.0005(6) 0.0035(6) 0.0027(7)
C21 0.0222(8) 0.0240(8) 0.0245(8) -0.0009(7) 0.0007(7) 0.0010(7)
C22 0.0289(9) 0.0206(8) 0.0322(9) -0.0016(7) 0.0065(7) -0.0015(7)
C23 0.0338(9) 0.0261(9) 0.0303(9) 0.0085(7) 0.0055(8) 0.0083(8)
C24 0.0322(9) 0.0322(9) 0.0239(8) 0.0012(7) -0.0015(7) 0.0052(7)
C25 0.0282(8) 0.0229(8) 0.0243(8) -0.0014(6) -0.0018(7) 0.0033(7)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.09857(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 . C1 . 1.3424(19) yes
N1 . C5 . 1.3515(19) yes
N2 . C11 . 1.4247(19) yes
N2 . C14 . 1.4181(18) yes
N2 . C20 . 1.4175(19) yes
C1 . C1 2_565 1.491(3) yes
C1 . C2 . 1.395(2) yes
C2 . C3 . 1.382(2) yes
C2 . H21 . 0.962 no
C3 . C4 . 1.382(2) yes
C3 . H31 . 0.962 no
C4 . C5 . 1.394(2) yes
C4 . H41 . 0.945 no
C5 . C6 . 1.467(2) yes
C6 . C7 . 1.337(2) yes
C6 . H61 . 0.981 no
C7 . C8 . 1.461(2) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.403(2) yes
C8 . C13 . 1.399(2) yes
C9 . C10 . 1.383(2) yes
C9 . H91 . 0.961 no
C10 . C11 . 1.396(2) yes
C10 . H101 . 0.975 no
C11 . C12 . 1.394(2) yes
C12 . C13 . 1.385(2) yes
C12 . H121 . 0.971 no
C13 . H131 . 0.958 no
C14 . C15 . 1.395(2) yes
C14 . C19 . 1.394(2) yes
C15 . C16 . 1.383(2) yes
C15 . H151 . 0.964 no
C16 . C17 . 1.385(2) yes
C16 . H161 . 0.955 no
C17 . C18 . 1.388(2) yes
C17 . H171 . 0.960 no
C18 . C19 . 1.384(2) yes
C18 . H181 . 0.960 no
C19 . H191 . 0.956 no
C20 . C21 . 1.395(2) yes
C20 . C25 . 1.391(2) yes
C21 . C22 . 1.385(2) yes
C21 . H211 . 0.942 no
C22 . C23 . 1.386(2) yes
C22 . H221 . 0.960 no
C23 . C24 . 1.387(2) yes
C23 . H231 . 0.948 no
C24 . C25 . 1.383(2) yes
C24 . H241 . 0.959 no
C25 . H251 . 0.968 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 . N1 . C5 . 118.44(13) yes
C11 . N2 . C14 . 119.28(12) yes
C11 . N2 . C20 . 119.46(12) yes
C14 . N2 . C20 . 120.33(12) yes
C1 2_565 C1 . N1 . 116.01(16) yes
C1 2_565 C1 . C2 . 121.33(16) yes
N1 . C1 . C2 . 122.65(14) yes
C1 . C2 . C3 . 118.57(14) yes
C1 . C2 . H21 . 119.6 no
C3 . C2 . H21 . 121.8 no
C2 . C3 . C4 . 119.32(14) yes
C2 . C3 . H31 . 121.5 no
C4 . C3 . H31 . 119.1 no
C3 . C4 . C5 . 119.18(14) yes
C3 . C4 . H41 . 119.3 no
C5 . C4 . H41 . 121.5 no
C4 . C5 . N1 . 121.83(14) yes
C4 . C5 . C6 . 120.53(14) yes
N1 . C5 . C6 . 117.63(13) yes
C5 . C6 . C7 . 123.65(15) yes
C5 . C6 . H61 . 117.1 no
C7 . C6 . H61 . 119.2 no
C6 . C7 . C8 . 127.21(14) yes
C6 . C7 . H71 . 118.0 no
C8 . C7 . H71 . 114.8 no
C7 . C8 . C9 . 123.05(13) yes
C7 . C8 . C13 . 119.32(14) yes
C9 . C8 . C13 . 117.63(14) yes
C8 . C9 . C10 . 121.30(14) yes
C8 . C9 . H91 . 118.1 no
C10 . C9 . H91 . 120.6 no
C9 . C10 . C11 . 120.52(14) yes
C9 . C10 . H101 . 121.0 no
C11 . C10 . H101 . 118.5 no
N2 . C11 . C10 . 120.21(14) yes
N2 . C11 . C12 . 121.11(13) yes
C10 . C11 . C12 . 118.68(14) yes
C11 . C12 . C13 . 120.63(14) yes
C11 . C12 . H121 . 120.3 no
C13 . C12 . H121 . 119.1 no
C8 . C13 . C12 . 121.20(14) yes
C8 . C13 . H131 . 119.4 no
C12 . C13 . H131 . 119.4 no
N2 . C14 . C15 . 120.06(13) yes
N2 . C14 . C19 . 120.94(13) yes
C15 . C14 . C19 . 118.99(13) yes
C14 . C15 . C16 . 120.32(14) yes
C14 . C15 . H151 . 119.5 no
C16 . C15 . H151 . 120.2 no
C15 . C16 . C17 . 120.58(15) yes
C15 . C16 . H161 . 119.7 no
C17 . C16 . H161 . 119.8 no
C16 . C17 . C18 . 119.29(14) yes
C16 . C17 . H171 . 120.8 no
C18 . C17 . H171 . 119.9 no
C17 . C18 . C19 . 120.56(15) yes
C17 . C18 . H181 . 119.0 no
C19 . C18 . H181 . 120.5 no
C14 . C19 . C18 . 120.25(15) yes
C14 . C19 . H191 . 119.4 no
C18 . C19 . H191 . 120.3 no
N2 . C20 . C21 . 120.41(14) yes
N2 . C20 . C25 . 120.68(14) yes
C21 . C20 . C25 . 118.91(14) yes
C20 . C21 . C22 . 120.30(15) yes
C20 . C21 . H211 . 118.5 no
C22 . C21 . H211 . 121.2 no
C21 . C22 . C23 . 120.50(15) yes
C21 . C22 . H221 . 120.5 no
C23 . C22 . H221 . 119.0 no
C22 . C23 . C24 . 119.33(15) yes
C22 . C23 . H231 . 121.2 no
C24 . C23 . H231 . 119.4 no
C23 . C24 . C25 . 120.42(15) yes
C23 . C24 . H241 . 119.0 no
C25 . C24 . H241 . 120.5 no
C20 . C25 . C24 . 120.53(16) yes
C20 . C25 . H251 . 118.6 no
C24 . C25 . H251 . 120.9 no
_iucr_refine_instruction_details_constraints
;
#
# Punched on 10/12/11 at 12:05:29
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 10/12/11 at 12:05:29
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;