# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_is410qau
_database_code_depnum_ccdc_archive 'CCDC 1889116'
loop_
_audit_author_name
_audit_author_address
'ISHTIAQ KHAN'
;phd scholar
Pakistan
;
_audit_update_record
;
2019-01-07 deposited with the CCDC. 2019-11-27 downloaded from the CCDC.
;
_audit_creation_date 2019-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic
;
Bromo-(N-carbamothioylacetamide)-bis(triphenylphosphine)-copper(i)
;
_chemical_formula_moiety 'C39 H36 Br Cu N2 O P2 S'
_chemical_formula_sum 'C39 H36 Br Cu N2 O P2 S'
_chemical_formula_weight 786.15
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.782(5)
_cell_length_b 13.220(3)
_cell_length_c 19.395(6)
_cell_angle_alpha 90
_cell_angle_beta 97.260(14)
_cell_angle_gamma 90
_cell_volume 3759.6(19)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 4788
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 27.831
_cell_measurement_theta_min 2.619
_shelx_estimated_absorpt_T_max 0.630
_shelx_estimated_absorpt_T_min 0.561
_exptl_absorpt_coefficient_mu 1.817
_exptl_absorpt_correction_T_max 0.690
_exptl_absorpt_correction_T_min 0.580
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Bruker, 2005)'
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.389
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1608
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.28
_exptl_special_details
;
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0668
_diffrn_reflns_av_unetI/netI 0.0973
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 25501
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.831
_diffrn_reflns_theta_min 2.619
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type 'Bruker Kappa APEXII CCD'
_diffrn_measurement_method \w
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4788
_reflns_number_total 8784
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT (Bruker, 2007)'
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'SAINT (Bruker, 2007)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max 0.396
_refine_diff_density_min -0.316
_refine_diff_density_rms 0.065
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.959
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 425
_refine_ls_number_reflns 8784
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1123
_refine_ls_R_factor_gt 0.0461
_refine_ls_restrained_S_all 0.959
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0842
_refine_ls_wR_factor_ref 0.1024
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
N2(H2), C2(H2A), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20),
C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
2.b X=CH2 refined with riding coordinates:
N1(H1A,H1B)
2.c Idealised Me refined as rotating group:
C39(H39A,H39B,H39C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary iterative
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.67129(3) 0.48140(2) 0.36119(2) 0.05376(12) Uani 1 1 d . . . . .
Cu1 Cu 0.62258(3) 0.29776(3) 0.35216(2) 0.04289(12) Uani 1 1 d . . . . .
S1 S 0.68670(6) 0.22326(6) 0.25517(5) 0.0547(2) Uani 1 1 d . . . . .
P1 P 0.47261(6) 0.30287(6) 0.30687(4) 0.0412(2) Uani 1 1 d . . . . .
P2 P 0.68562(6) 0.21419(6) 0.45109(4) 0.0406(2) Uani 1 1 d . . . . .
O1 O 0.9848(2) 0.3123(2) 0.30845(18) 0.1002(11) Uani 1 1 d . . . . .
N1 N 0.8596(2) 0.1824(2) 0.25144(18) 0.0857(12) Uani 1 1 d . . . . .
H1A H 0.9168 0.1968 0.2591 0.103 Uiso 1 1 calc R . . . .
H1B H 0.8422 0.1264 0.2314 0.103 Uiso 1 1 calc R . . . .
N2 N 0.83141(19) 0.33378(19) 0.30181(14) 0.0533(8) Uani 1 1 d . . . . .
H2 H 0.7906 0.3747 0.3132 0.064 Uiso 1 1 calc R . . . .
C1 C 0.4450(2) 0.3942(2) 0.23521(17) 0.0484(9) Uani 1 1 d . . . . .
C2 C 0.5128(3) 0.4285(3) 0.1985(2) 0.0739(12) Uani 1 1 d . . . . .
H2A H 0.5715 0.4026 0.2086 0.089 Uiso 1 1 calc R . . . .
C3 C 0.4950(4) 0.5012(4) 0.1466(2) 0.0994(16) Uani 1 1 d . . . . .
H3 H 0.5414 0.5230 0.1220 0.119 Uiso 1 1 calc R . . . .
C4 C 0.4089(4) 0.5406(3) 0.1317(2) 0.0966(15) Uani 1 1 d . . . . .
H4 H 0.3973 0.5901 0.0977 0.116 Uiso 1 1 calc R . . . .
C5 C 0.3407(3) 0.5074(3) 0.1667(2) 0.0878(14) Uani 1 1 d . . . . .
H5 H 0.2818 0.5323 0.1558 0.105 Uiso 1 1 calc R . . . .
C6 C 0.3601(3) 0.4357(3) 0.2189(2) 0.0693(11) Uani 1 1 d . . . . .
H6 H 0.3135 0.4151 0.2437 0.083 Uiso 1 1 calc R . . . .
C7 C 0.4331(2) 0.1798(2) 0.27254(17) 0.0437(8) Uani 1 1 d . . . . .
C8 C 0.3795(2) 0.1644(3) 0.20978(19) 0.0608(10) Uani 1 1 d . . . . .
H8 H 0.3647 0.2189 0.1801 0.073 Uiso 1 1 calc R . . . .
C9 C 0.3474(3) 0.0683(3) 0.1905(2) 0.0778(12) Uani 1 1 d . . . . .
H9 H 0.3100 0.0589 0.1487 0.093 Uiso 1 1 calc R . . . .
C10 C 0.3711(3) -0.0130(3) 0.2333(3) 0.0710(12) Uani 1 1 d . . . . .
H10 H 0.3496 -0.0772 0.2203 0.085 Uiso 1 1 calc R . . . .
C11 C 0.4272(3) 0.0001(3) 0.2959(2) 0.0699(12) Uani 1 1 d . . . . .
H11 H 0.4437 -0.0549 0.3246 0.084 Uiso 1 1 calc R . . . .
C12 C 0.4579(2) 0.0958(2) 0.31476(18) 0.0569(9) Uani 1 1 d . . . . .
H12 H 0.4958 0.1048 0.3563 0.068 Uiso 1 1 calc R . . . .
C13 C 0.3861(2) 0.3349(2) 0.36362(16) 0.0432(8) Uani 1 1 d . . . . .
C14 C 0.4012(2) 0.4205(2) 0.40554(18) 0.0549(9) Uani 1 1 d . . . . .
H14 H 0.4531 0.4595 0.4032 0.066 Uiso 1 1 calc R . . . .
C15 C 0.3407(3) 0.4479(3) 0.4501(2) 0.0682(11) Uani 1 1 d . . . . .
H15 H 0.3520 0.5051 0.4777 0.082 Uiso 1 1 calc R . . . .
C16 C 0.2643(3) 0.3921(3) 0.4542(2) 0.0743(12) Uani 1 1 d . . . . .
H16 H 0.2243 0.4100 0.4855 0.089 Uiso 1 1 calc R . . . .
C17 C 0.2463(3) 0.3093(3) 0.4121(2) 0.0757(12) Uani 1 1 d . . . . .
H17 H 0.1928 0.2728 0.4134 0.091 Uiso 1 1 calc R . . . .
C18 C 0.3078(2) 0.2801(3) 0.36767(19) 0.0588(10) Uani 1 1 d . . . . .
H18 H 0.2960 0.2228 0.3402 0.071 Uiso 1 1 calc R . . . .
C19 C 0.6795(2) 0.0762(2) 0.44558(17) 0.0497(9) Uani 1 1 d . . . . .
C20 C 0.7179(3) 0.0280(3) 0.3920(2) 0.0732(12) Uani 1 1 d . . . . .
H20 H 0.7458 0.0663 0.3604 0.088 Uiso 1 1 calc R . . . .
C21 C 0.7145(4) -0.0765(3) 0.3856(2) 0.0961(16) Uani 1 1 d . . . . .
H21 H 0.7394 -0.1079 0.3494 0.115 Uiso 1 1 calc R . . . .
C22 C 0.6749(4) -0.1330(3) 0.4319(3) 0.1129(19) Uani 1 1 d . . . . .
H22 H 0.6746 -0.2032 0.4282 0.135 Uiso 1 1 calc R . . . .
C23 C 0.6351(4) -0.0872(3) 0.4846(3) 0.1152(19) Uani 1 1 d . . . . .
H23 H 0.6061 -0.1263 0.5151 0.138 Uiso 1 1 calc R . . . .
C24 C 0.6384(3) 0.0173(3) 0.4918(2) 0.0776(13) Uani 1 1 d . . . . .
H24 H 0.6129 0.0479 0.5280 0.093 Uiso 1 1 calc R . . . .
C25 C 0.6374(2) 0.2455(2) 0.53116(16) 0.0421(8) Uani 1 1 d . . . . .
C26 C 0.5536(2) 0.2908(2) 0.52637(19) 0.0567(9) Uani 1 1 d . . . . .
H26 H 0.5211 0.3014 0.4827 0.068 Uiso 1 1 calc R . . . .
C27 C 0.5161(3) 0.3213(3) 0.5848(2) 0.0722(11) Uani 1 1 d . . . . .
H27 H 0.4588 0.3514 0.5802 0.087 Uiso 1 1 calc R . . . .
C28 C 0.5636(3) 0.3070(3) 0.6498(2) 0.0735(12) Uani 1 1 d . . . . .
H28 H 0.5392 0.3289 0.6891 0.088 Uiso 1 1 calc R . . . .
C29 C 0.6469(3) 0.2605(3) 0.6564(2) 0.0742(12) Uani 1 1 d . . . . .
H29 H 0.6788 0.2498 0.7002 0.089 Uiso 1 1 calc R . . . .
C30 C 0.6837(3) 0.2294(3) 0.59752(18) 0.0601(10) Uani 1 1 d . . . . .
H30 H 0.7401 0.1972 0.6024 0.072 Uiso 1 1 calc R . . . .
C31 C 0.8073(2) 0.2378(2) 0.47852(16) 0.0449(8) Uani 1 1 d . . . . .
C32 C 0.8334(3) 0.3377(3) 0.4908(2) 0.0680(11) Uani 1 1 d . . . . .
H32 H 0.7900 0.3888 0.4835 0.082 Uiso 1 1 calc R . . . .
C33 C 0.9224(3) 0.3621(4) 0.5137(3) 0.0955(15) Uani 1 1 d . . . . .
H33 H 0.9379 0.4297 0.5215 0.115 Uiso 1 1 calc R . . . .
C34 C 0.9883(3) 0.2909(5) 0.5252(3) 0.1034(17) Uani 1 1 d . . . . .
H34 H 1.0485 0.3086 0.5402 0.124 Uiso 1 1 calc R . . . .
C35 C 0.9636(3) 0.1916(5) 0.5140(3) 0.1117(18) Uani 1 1 d . . . . .
H35 H 1.0078 0.1416 0.5224 0.134 Uiso 1 1 calc R . . . .
C36 C 0.8736(3) 0.1634(3) 0.4904(2) 0.0851(13) Uani 1 1 d . . . . .
H36 H 0.8585 0.0957 0.4828 0.102 Uiso 1 1 calc R . . . .
C37 C 0.7995(2) 0.2455(2) 0.27008(17) 0.0499(9) Uani 1 1 d . . . . .
C38 C 0.9214(3) 0.3652(3) 0.3178(2) 0.0710(12) Uani 1 1 d . . . . .
C39 C 0.9300(3) 0.4716(3) 0.3450(2) 0.0902(15) Uani 1 1 d . . . . .
H39A H 0.8815 0.4853 0.3723 0.135 Uiso 1 1 calc GR . . . .
H39B H 0.9265 0.5181 0.3067 0.135 Uiso 1 1 calc GR . . . .
H39C H 0.9876 0.4795 0.3735 0.135 Uiso 1 1 calc GR . . . .
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
Br1 0.0657(3) 0.03731(19) 0.0609(2) -0.00470(15) 0.01818(19) -0.00359(17)
Cu1 0.0398(3) 0.0436(2) 0.0448(3) 0.00114(17) 0.00350(18) -0.00318(19)
S1 0.0539(6) 0.0562(5) 0.0550(6) -0.0171(4) 0.0106(5) -0.0057(5)
P1 0.0381(5) 0.0426(5) 0.0422(5) -0.0008(4) 0.0023(4) -0.0010(4)
P2 0.0431(5) 0.0373(5) 0.0406(5) 0.0001(4) 0.0030(4) -0.0033(4)
O1 0.0508(19) 0.091(2) 0.164(3) -0.0260(19) 0.034(2) -0.0087(17)
N1 0.061(2) 0.064(2) 0.139(3) -0.038(2) 0.040(2) -0.0020(18)
N2 0.0481(19) 0.0500(17) 0.065(2) -0.0126(14) 0.0203(16) -0.0057(15)
C1 0.048(2) 0.050(2) 0.046(2) 0.0020(15) 0.0001(18) 0.0002(17)
C2 0.061(3) 0.096(3) 0.065(3) 0.027(2) 0.012(2) 0.011(2)
C3 0.092(4) 0.127(4) 0.082(3) 0.046(3) 0.021(3) -0.005(3)
C4 0.106(4) 0.092(4) 0.090(4) 0.043(3) 0.007(3) 0.020(3)
C5 0.078(3) 0.091(3) 0.095(4) 0.032(3) 0.010(3) 0.027(3)
C6 0.058(3) 0.072(3) 0.078(3) 0.022(2) 0.013(2) 0.012(2)
C7 0.0339(19) 0.050(2) 0.048(2) -0.0068(16) 0.0091(16) 0.0008(16)
C8 0.059(3) 0.062(2) 0.058(2) -0.0178(19) -0.008(2) 0.009(2)
C9 0.057(3) 0.089(3) 0.084(3) -0.044(3) -0.005(2) -0.001(3)
C10 0.055(3) 0.060(3) 0.102(4) -0.034(2) 0.023(3) -0.015(2)
C11 0.076(3) 0.053(2) 0.084(3) -0.005(2) 0.024(3) -0.010(2)
C12 0.062(3) 0.053(2) 0.054(2) -0.0040(17) 0.0032(19) -0.0098(19)
C13 0.042(2) 0.0423(19) 0.045(2) 0.0012(14) 0.0015(16) 0.0058(16)
C14 0.056(2) 0.049(2) 0.059(2) -0.0067(17) 0.005(2) 0.0017(18)
C15 0.073(3) 0.061(2) 0.071(3) -0.013(2) 0.010(2) 0.011(2)
C16 0.082(3) 0.073(3) 0.075(3) 0.007(2) 0.034(3) 0.024(3)
C17 0.071(3) 0.074(3) 0.090(3) -0.001(2) 0.042(3) -0.011(2)
C18 0.056(3) 0.053(2) 0.069(3) -0.0088(18) 0.018(2) -0.0083(19)
C19 0.060(2) 0.0367(18) 0.049(2) 0.0023(16) -0.0029(18) -0.0058(17)
C20 0.112(4) 0.046(2) 0.062(3) 0.0002(18) 0.014(3) 0.003(2)
C21 0.157(5) 0.051(3) 0.082(3) -0.014(2) 0.021(3) 0.007(3)
C22 0.167(6) 0.043(3) 0.127(5) -0.001(3) 0.014(4) -0.020(3)
C23 0.166(6) 0.055(3) 0.134(5) 0.009(3) 0.056(4) -0.028(3)
C24 0.105(4) 0.045(2) 0.086(3) -0.003(2) 0.024(3) -0.020(2)
C25 0.044(2) 0.0385(18) 0.044(2) 0.0002(14) 0.0046(16) -0.0103(16)
C26 0.048(2) 0.063(2) 0.059(3) -0.0014(18) 0.0048(19) 0.0032(19)
C27 0.056(3) 0.087(3) 0.077(3) -0.008(2) 0.022(3) 0.004(2)
C28 0.075(3) 0.087(3) 0.066(3) -0.015(2) 0.035(3) -0.020(3)
C29 0.073(3) 0.104(3) 0.047(3) 0.001(2) 0.011(2) -0.016(3)
C30 0.051(2) 0.084(3) 0.045(2) 0.0009(19) 0.0053(19) -0.004(2)
C31 0.041(2) 0.055(2) 0.0375(19) -0.0014(15) 0.0027(16) -0.0027(18)
C32 0.050(3) 0.065(3) 0.085(3) -0.005(2) -0.008(2) -0.009(2)
C33 0.070(3) 0.103(4) 0.108(4) 0.000(3) -0.010(3) -0.031(3)
C34 0.057(3) 0.153(5) 0.096(4) -0.004(4) -0.007(3) -0.031(4)
C35 0.050(3) 0.139(5) 0.142(5) -0.009(4) -0.006(3) 0.021(3)
C36 0.063(3) 0.078(3) 0.112(4) -0.005(3) 0.001(3) 0.012(3)
C37 0.059(2) 0.045(2) 0.050(2) -0.0034(16) 0.0226(19) -0.0009(18)
C38 0.061(3) 0.069(3) 0.088(3) -0.011(2) 0.034(3) -0.020(2)
C39 0.074(3) 0.081(3) 0.123(4) -0.036(3) 0.043(3) -0.033(2)
_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
Br1 Cu1 2.5320(8) . ?
Cu1 S1 2.4203(10) . ?
Cu1 P1 2.2800(12) . ?
Cu1 P2 2.3062(10) . ?
S1 C37 1.682(4) . ?
P1 C1 1.847(3) . ?
P1 C7 1.826(3) . ?
P1 C13 1.838(3) . ?
P2 C19 1.829(3) . ?
P2 C25 1.836(3) . ?
P2 C31 1.837(3) . ?
O1 C38 1.201(4) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C37 1.303(4) . ?
N2 H2 0.8600 . ?
N2 C37 1.374(4) . ?
N2 C38 1.391(5) . ?
C1 C2 1.377(4) . ?
C1 C6 1.370(5) . ?
C2 H2A 0.9300 . ?
C2 C3 1.394(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.371(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.357(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.390(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.381(4) . ?
C7 C12 1.400(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.391(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.376(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.391(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.378(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.395(4) . ?
C13 C18 1.376(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.368(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.360(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.370(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.384(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.399(5) . ?
C19 C24 1.385(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.387(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.357(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.382(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.389(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.369(4) . ?
C25 C30 1.395(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.384(5) . ?
C27 H27 0.9300 . ?
C27 C28 1.376(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.367(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.388(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.387(4) . ?
C31 C36 1.386(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.372(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.354(6) . ?
C34 H34 0.9300 . ?
C34 C35 1.372(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.402(6) . ?
C36 H36 0.9300 . ?
C38 C39 1.502(5) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 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
S1 Cu1 Br1 107.94(3) . . ?
P1 Cu1 Br1 104.62(3) . . ?
P1 Cu1 S1 99.78(4) . . ?
P1 Cu1 P2 127.28(3) . . ?
P2 Cu1 Br1 108.68(3) . . ?
P2 Cu1 S1 107.16(4) . . ?
C37 S1 Cu1 105.80(12) . . ?
C1 P1 Cu1 114.90(12) . . ?
C7 P1 Cu1 111.39(11) . . ?
C7 P1 C1 106.14(15) . . ?
C7 P1 C13 102.05(14) . . ?
C13 P1 Cu1 119.47(11) . . ?
C13 P1 C1 101.28(15) . . ?
C19 P2 Cu1 114.67(11) . . ?
C19 P2 C25 104.64(14) . . ?
C19 P2 C31 103.06(15) . . ?
C25 P2 Cu1 115.89(11) . . ?
C25 P2 C31 100.79(15) . . ?
C31 P2 Cu1 115.93(11) . . ?
H1A N1 H1B 120.0 . . ?
C37 N1 H1A 120.0 . . ?
C37 N1 H1B 120.0 . . ?
C37 N2 H2 115.9 . . ?
C37 N2 C38 128.2(3) . . ?
C38 N2 H2 115.9 . . ?
C2 C1 P1 119.8(3) . . ?
C6 C1 P1 123.0(3) . . ?
C6 C1 C2 117.0(3) . . ?
C1 C2 H2A 119.5 . . ?
C1 C2 C3 121.1(4) . . ?
C3 C2 H2A 119.5 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.5 . . ?
C4 C5 C6 119.1(4) . . ?
C6 C5 H5 120.5 . . ?
C1 C6 C5 122.7(4) . . ?
C1 C6 H6 118.6 . . ?
C5 C6 H6 118.6 . . ?
C8 C7 P1 125.0(3) . . ?
C8 C7 C12 118.5(3) . . ?
C12 C7 P1 116.4(3) . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.6(4) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 119.9(4) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.5(4) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.5 . . ?
C12 C11 C10 119.1(4) . . ?
C12 C11 H11 120.5 . . ?
C7 C12 H12 119.4 . . ?
C11 C12 C7 121.3(4) . . ?
C11 C12 H12 119.4 . . ?
C14 C13 P1 117.6(3) . . ?
C18 C13 P1 124.5(2) . . ?
C18 C13 C14 117.8(3) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 121.0(3) . . ?
C15 C14 H14 119.5 . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.4(4) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 119.9(4) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0(4) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 C17 120.8(3) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 P2 118.4(3) . . ?
C24 C19 P2 123.0(3) . . ?
C24 C19 C20 118.5(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.5(3) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.2(4) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 119.7 . . ?
C21 C22 C23 120.5(4) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 120.1 . . ?
C22 C23 C24 119.8(4) . . ?
C24 C23 H23 120.1 . . ?
C19 C24 C23 120.4(4) . . ?
C19 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C26 C25 P2 119.1(3) . . ?
C26 C25 C30 117.6(3) . . ?
C30 C25 P2 123.3(3) . . ?
C25 C26 H26 119.2 . . ?
C25 C26 C27 121.7(4) . . ?
C27 C26 H26 119.2 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 119.9(4) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.1 . . ?
C29 C28 C27 119.8(4) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 119.9(4) . . ?
C30 C29 H29 120.0 . . ?
C25 C30 H30 119.5 . . ?
C29 C30 C25 121.1(4) . . ?
C29 C30 H30 119.5 . . ?
C32 C31 P2 116.9(3) . . ?
C36 C31 P2 124.9(3) . . ?
C36 C31 C32 118.1(4) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 C31 120.9(4) . . ?
C33 C32 H32 119.5 . . ?
C32 C33 H33 119.0 . . ?
C34 C33 C32 122.0(5) . . ?
C34 C33 H33 119.0 . . ?
C33 C34 H34 121.1 . . ?
C33 C34 C35 117.9(5) . . ?
C35 C34 H34 121.1 . . ?
C34 C35 H35 119.0 . . ?
C34 C35 C36 121.9(5) . . ?
C36 C35 H35 119.0 . . ?
C31 C36 C35 119.1(4) . . ?
C31 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
N1 C37 S1 122.4(3) . . ?
N1 C37 N2 117.4(3) . . ?
N2 C37 S1 120.1(2) . . ?
O1 C38 N2 122.3(4) . . ?
O1 C38 C39 124.4(4) . . ?
N2 C38 C39 113.2(4) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
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
N1 H1A O1 0.86 2.00 2.660(4) 132.3 .
N1 H1B Br1 0.86 2.62 3.434(3) 158.8 2_645
N2 H2 Br1 0.86 2.53 3.380(3) 172.5 .
C2 H2A S1 0.93 2.99 3.802(4) 146.6 .
C20 H20 S1 0.93 2.96 3.689(4) 135.8 .
C32 H32 Br1 0.93 3.03 3.762(4) 137.3 .
C39 H39A Br1 0.96 3.09 3.879(4) 140.7 .
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
Cu1 S1 C37 N1 146.6(3) . . . . ?
Cu1 S1 C37 N2 -34.7(3) . . . . ?
Cu1 P1 C1 C2 20.6(3) . . . . ?
Cu1 P1 C1 C6 -155.0(3) . . . . ?
Cu1 P1 C7 C8 -135.9(3) . . . . ?
Cu1 P1 C7 C12 45.8(3) . . . . ?
Cu1 P1 C13 C14 49.2(3) . . . . ?
Cu1 P1 C13 C18 -130.7(3) . . . . ?
Cu1 P2 C19 C20 56.6(3) . . . . ?
Cu1 P2 C19 C24 -123.2(3) . . . . ?
Cu1 P2 C25 C26 18.5(3) . . . . ?
Cu1 P2 C25 C30 -158.6(2) . . . . ?
Cu1 P2 C31 C32 57.0(3) . . . . ?
Cu1 P2 C31 C36 -125.7(3) . . . . ?
P1 C1 C2 C3 -176.7(4) . . . . ?
P1 C1 C6 C5 177.4(3) . . . . ?
P1 C7 C8 C9 -175.3(3) . . . . ?
P1 C7 C12 C11 176.0(3) . . . . ?
P1 C13 C14 C15 -178.7(3) . . . . ?
P1 C13 C18 C17 179.7(3) . . . . ?
P2 C19 C20 C21 -179.7(3) . . . . ?
P2 C19 C24 C23 179.4(4) . . . . ?
P2 C25 C26 C27 -176.3(3) . . . . ?
P2 C25 C30 C29 175.6(3) . . . . ?
P2 C31 C32 C33 177.9(3) . . . . ?
P2 C31 C36 C35 -177.3(3) . . . . ?
C1 P1 C7 C8 -10.2(3) . . . . ?
C1 P1 C7 C12 171.6(3) . . . . ?
C1 P1 C13 C14 -78.1(3) . . . . ?
C1 P1 C13 C18 102.0(3) . . . . ?
C1 C2 C3 C4 0.7(8) . . . . ?
C2 C1 C6 C5 1.6(6) . . . . ?
C2 C3 C4 C5 -1.3(8) . . . . ?
C3 C4 C5 C6 2.0(8) . . . . ?
C4 C5 C6 C1 -2.3(7) . . . . ?
C6 C1 C2 C3 -0.8(6) . . . . ?
C7 P1 C1 C2 -102.9(3) . . . . ?
C7 P1 C1 C6 81.4(3) . . . . ?
C7 P1 C13 C14 172.5(3) . . . . ?
C7 P1 C13 C18 -7.4(3) . . . . ?
C7 C8 C9 C10 -1.7(6) . . . . ?
C8 C7 C12 C11 -2.4(5) . . . . ?
C8 C9 C10 C11 -0.1(6) . . . . ?
C9 C10 C11 C12 0.6(6) . . . . ?
C10 C11 C12 C7 0.6(5) . . . . ?
C12 C7 C8 C9 2.9(5) . . . . ?
C13 P1 C1 C2 150.8(3) . . . . ?
C13 P1 C1 C6 -24.8(3) . . . . ?
C13 P1 C7 C8 95.5(3) . . . . ?
C13 P1 C7 C12 -82.8(3) . . . . ?
C13 C14 C15 C16 -0.2(6) . . . . ?
C14 C13 C18 C17 -0.1(5) . . . . ?
C14 C15 C16 C17 -1.8(6) . . . . ?
C15 C16 C17 C18 2.8(6) . . . . ?
C16 C17 C18 C13 -1.8(6) . . . . ?
C18 C13 C14 C15 1.1(5) . . . . ?
C19 P2 C25 C26 -108.8(3) . . . . ?
C19 P2 C25 C30 74.1(3) . . . . ?
C19 P2 C31 C32 -176.9(3) . . . . ?
C19 P2 C31 C36 0.4(3) . . . . ?
C19 C20 C21 C22 -0.9(7) . . . . ?
C20 C19 C24 C23 -0.4(6) . . . . ?
C20 C21 C22 C23 2.0(9) . . . . ?
C21 C22 C23 C24 -2.3(9) . . . . ?
C22 C23 C24 C19 1.6(8) . . . . ?
C24 C19 C20 C21 0.1(6) . . . . ?
C25 P2 C19 C20 -175.3(3) . . . . ?
C25 P2 C19 C24 4.9(4) . . . . ?
C25 P2 C31 C32 -68.9(3) . . . . ?
C25 P2 C31 C36 108.3(3) . . . . ?
C25 C26 C27 C28 0.5(6) . . . . ?
C26 C25 C30 C29 -1.5(5) . . . . ?
C26 C27 C28 C29 -1.6(6) . . . . ?
C27 C28 C29 C30 1.0(6) . . . . ?
C28 C29 C30 C25 0.6(6) . . . . ?
C30 C25 C26 C27 1.0(5) . . . . ?
C31 P2 C19 C20 -70.3(3) . . . . ?
C31 P2 C19 C24 109.9(3) . . . . ?
C31 P2 C25 C26 144.5(3) . . . . ?
C31 P2 C25 C30 -32.7(3) . . . . ?
C31 C32 C33 C34 0.0(7) . . . . ?
C32 C31 C36 C35 -0.1(6) . . . . ?
C32 C33 C34 C35 -0.7(8) . . . . ?
C33 C34 C35 C36 1.0(8) . . . . ?
C34 C35 C36 C31 -0.6(8) . . . . ?
C36 C31 C32 C33 0.4(6) . . . . ?
C37 N2 C38 O1 -4.7(6) . . . . ?
C37 N2 C38 C39 173.3(3) . . . . ?
C38 N2 C37 S1 -179.5(3) . . . . ?
C38 N2 C37 N1 -0.8(5) . . . . ?
_shelx_res_file
;
is410qau.res created by SHELXL-2014/7
TITL IS410QAU_0m in P2(1)/n COLORLESS PRISM
CELL 0.71073 14.7821 13.2197 19.3948 90 97.26 90
ZERR 4 0.0045 0.0034 0.0056 0 0.014 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O P S Cu Br
UNIT 156 144 8 4 8 4 4 4
EQIV $1 1.5-X,-0.5+Y,0.5-Z
L.S. 40
PLAN 20
SIZE 0.36 0.32 0.28
TEMP 23
HTAB N1 O1
HTAB N1 Br1_$1
HTAB N2 Br1
HTAB C2 S1
HTAB C20 S1
HTAB C32 Br1
HTAB C39 Br1
BOND $H
HTAB
CONF
LIST 4
fmap 2
acta
OMIT 1 0 1
OMIT -1 1 1
OMIT -1 0 1
REM
REM
REM
WGHT 0.029800
FVAR 0.09875
BR1 8 0.671291 0.481402 0.361188 11.00000 0.06569 0.03731 =
0.06088 -0.00470 0.01818 -0.00359
CU1 7 0.622582 0.297761 0.352164 11.00000 0.03982 0.04362 =
0.04477 0.00114 0.00350 -0.00318
S1 6 0.686702 0.223265 0.255170 11.00000 0.05388 0.05620 =
0.05502 -0.01710 0.01058 -0.00569
P1 5 0.472613 0.302872 0.306870 11.00000 0.03814 0.04265 =
0.04218 -0.00077 0.00233 -0.00103
P2 5 0.685624 0.214189 0.451090 11.00000 0.04312 0.03730 =
0.04064 0.00015 0.00298 -0.00332
O1 4 0.984766 0.312322 0.308446 11.00000 0.05084 0.09127 =
0.16367 -0.02600 0.03421 -0.00871
N1 3 0.859627 0.182441 0.251436 11.00000 0.06060 0.06420 =
0.13918 -0.03841 0.03976 -0.00197
AFIX 93
H1A 2 0.916759 0.196784 0.259128 11.00000 -1.20000
H1B 2 0.842177 0.126447 0.231438 11.00000 -1.20000
AFIX 0
N2 3 0.831412 0.333782 0.301807 11.00000 0.04808 0.04997 =
0.06510 -0.01263 0.02028 -0.00570
AFIX 43
H2 2 0.790589 0.374711 0.313214 11.00000 -1.20000
AFIX 0
C1 1 0.444981 0.394213 0.235214 11.00000 0.04791 0.04999 =
0.04580 0.00203 0.00012 0.00024
C2 1 0.512824 0.428450 0.198537 11.00000 0.06126 0.09627 =
0.06525 0.02701 0.01231 0.01078
AFIX 43
H2A 2 0.571525 0.402618 0.208614 11.00000 -1.20000
AFIX 0
C3 1 0.494959 0.501175 0.146566 11.00000 0.09205 0.12687 =
0.08189 0.04563 0.02084 -0.00466
AFIX 43
H3 2 0.541404 0.522965 0.121960 11.00000 -1.20000
AFIX 0
C4 1 0.408936 0.540570 0.131728 11.00000 0.10627 0.09233 =
0.08968 0.04263 0.00693 0.02020
AFIX 43
H4 2 0.397325 0.590081 0.097695 11.00000 -1.20000
AFIX 0
C5 1 0.340690 0.507391 0.166656 11.00000 0.07754 0.09074 =
0.09485 0.03210 0.00972 0.02683
AFIX 43
H5 2 0.281762 0.532273 0.155809 11.00000 -1.20000
AFIX 0
C6 1 0.360071 0.435723 0.218855 11.00000 0.05834 0.07243 =
0.07800 0.02217 0.01252 0.01179
AFIX 43
H6 2 0.313477 0.415094 0.243704 11.00000 -1.20000
AFIX 0
C7 1 0.433098 0.179795 0.272538 11.00000 0.03393 0.04961 =
0.04845 -0.00683 0.00907 0.00076
C8 1 0.379483 0.164414 0.209775 11.00000 0.05860 0.06174 =
0.05831 -0.01779 -0.00773 0.00911
AFIX 43
H8 2 0.364673 0.218852 0.180116 11.00000 -1.20000
AFIX 0
C9 1 0.347418 0.068254 0.190497 11.00000 0.05742 0.08862 =
0.08402 -0.04385 -0.00460 -0.00066
AFIX 43
H9 2 0.309989 0.058901 0.148710 11.00000 -1.20000
AFIX 0
C10 1 0.371147 -0.012977 0.233326 11.00000 0.05461 0.06005 =
0.10170 -0.03389 0.02284 -0.01483
AFIX 43
H10 2 0.349559 -0.077163 0.220342 11.00000 -1.20000
AFIX 0
C11 1 0.427160 0.000140 0.295880 11.00000 0.07559 0.05346 =
0.08415 -0.00529 0.02364 -0.01016
AFIX 43
H11 2 0.443658 -0.054921 0.324584 11.00000 -1.20000
AFIX 0
C12 1 0.457888 0.095841 0.314757 11.00000 0.06235 0.05310 =
0.05417 -0.00397 0.00319 -0.00984
AFIX 43
H12 2 0.495828 0.104844 0.356343 11.00000 -1.20000
AFIX 0
C13 1 0.386138 0.334873 0.363618 11.00000 0.04165 0.04226 =
0.04472 0.00116 0.00146 0.00580
C14 1 0.401178 0.420469 0.405542 11.00000 0.05621 0.04867 =
0.05910 -0.00669 0.00464 0.00174
AFIX 43
H14 2 0.453068 0.459453 0.403182 11.00000 -1.20000
AFIX 0
C15 1 0.340736 0.447929 0.450080 11.00000 0.07270 0.06102 =
0.07102 -0.01329 0.00958 0.01128
AFIX 43
H15 2 0.351958 0.505144 0.477740 11.00000 -1.20000
AFIX 0
C16 1 0.264332 0.392068 0.454157 11.00000 0.08191 0.07281 =
0.07451 0.00680 0.03445 0.02426
AFIX 43
H16 2 0.224338 0.410009 0.485454 11.00000 -1.20000
AFIX 0
C17 1 0.246343 0.309328 0.412106 11.00000 0.07130 0.07423 =
0.08986 -0.00091 0.04207 -0.01089
AFIX 43
H17 2 0.192825 0.272794 0.413425 11.00000 -1.20000
AFIX 0
C18 1 0.307802 0.280123 0.367674 11.00000 0.05640 0.05320 =
0.06943 -0.00883 0.01835 -0.00827
AFIX 43
H18 2 0.296025 0.222791 0.340216 11.00000 -1.20000
AFIX 0
C19 1 0.679510 0.076155 0.445576 11.00000 0.06047 0.03671 =
0.04946 0.00227 -0.00285 -0.00578
C20 1 0.717862 0.027985 0.391991 11.00000 0.11218 0.04577 =
0.06225 0.00019 0.01389 0.00342
AFIX 43
H20 2 0.745811 0.066263 0.360448 11.00000 -1.20000
AFIX 0
C21 1 0.714497 -0.076505 0.385570 11.00000 0.15704 0.05124 =
0.08165 -0.01389 0.02128 0.00712
AFIX 43
H21 2 0.739440 -0.107893 0.349424 11.00000 -1.20000
AFIX 0
C22 1 0.674901 -0.133025 0.431901 11.00000 0.16717 0.04339 =
0.12702 -0.00077 0.01421 -0.01992
AFIX 43
H22 2 0.674554 -0.203162 0.428159 11.00000 -1.20000
AFIX 0
C23 1 0.635082 -0.087218 0.484606 11.00000 0.16624 0.05461 =
0.13426 0.00873 0.05619 -0.02837
AFIX 43
H23 2 0.606120 -0.126276 0.515149 11.00000 -1.20000
AFIX 0
C24 1 0.638427 0.017294 0.491846 11.00000 0.10530 0.04521 =
0.08551 -0.00260 0.02444 -0.02047
AFIX 43
H24 2 0.612910 0.047934 0.528001 11.00000 -1.20000
AFIX 0
C25 1 0.637428 0.245487 0.531162 11.00000 0.04362 0.03851 =
0.04384 0.00019 0.00457 -0.01025
C26 1 0.553611 0.290818 0.526371 11.00000 0.04753 0.06317 =
0.05898 -0.00140 0.00479 0.00323
AFIX 43
H26 2 0.521062 0.301400 0.482718 11.00000 -1.20000
AFIX 0
C27 1 0.516080 0.321301 0.584845 11.00000 0.05582 0.08702 =
0.07712 -0.00765 0.02202 0.00411
AFIX 43
H27 2 0.458778 0.351423 0.580232 11.00000 -1.20000
AFIX 0
C28 1 0.563600 0.307012 0.649793 11.00000 0.07489 0.08664 =
0.06553 -0.01532 0.03465 -0.02016
AFIX 43
H28 2 0.539173 0.328914 0.689098 11.00000 -1.20000
AFIX 0
C29 1 0.646857 0.260508 0.656375 11.00000 0.07285 0.10374 =
0.04707 0.00060 0.01144 -0.01582
AFIX 43
H29 2 0.678769 0.249757 0.700234 11.00000 -1.20000
AFIX 0
C30 1 0.683684 0.229367 0.597515 11.00000 0.05091 0.08411 =
0.04515 0.00088 0.00529 -0.00384
AFIX 43
H30 2 0.740101 0.197239 0.602379 11.00000 -1.20000
AFIX 0
C31 1 0.807339 0.237845 0.478525 11.00000 0.04127 0.05533 =
0.03747 -0.00135 0.00271 -0.00268
C32 1 0.833448 0.337681 0.490814 11.00000 0.04992 0.06495 =
0.08471 -0.00527 -0.00838 -0.00903
AFIX 43
H32 2 0.790046 0.388767 0.483466 11.00000 -1.20000
AFIX 0
C33 1 0.922391 0.362110 0.513653 11.00000 0.06951 0.10337 =
0.10817 0.00031 -0.00992 -0.03125
AFIX 43
H33 2 0.937857 0.429704 0.521457 11.00000 -1.20000
AFIX 0
C34 1 0.988337 0.290861 0.525180 11.00000 0.05704 0.15313 =
0.09583 -0.00447 -0.00710 -0.03071
AFIX 43
H34 2 1.048490 0.308617 0.540166 11.00000 -1.20000
AFIX 0
C35 1 0.963576 0.191623 0.514043 11.00000 0.04961 0.13882 =
0.14201 -0.00898 -0.00556 0.02138
AFIX 43
H35 2 1.007811 0.141571 0.522412 11.00000 -1.20000
AFIX 0
C36 1 0.873558 0.163423 0.490418 11.00000 0.06278 0.07779 =
0.11196 -0.00491 0.00081 0.01172
AFIX 43
H36 2 0.858462 0.095692 0.482824 11.00000 -1.20000
AFIX 0
C37 1 0.799514 0.245533 0.270076 11.00000 0.05900 0.04487 =
0.04996 -0.00339 0.02261 -0.00090
C38 1 0.921437 0.365239 0.317797 11.00000 0.06136 0.06948 =
0.08829 -0.01100 0.03385 -0.02029
C39 1 0.930049 0.471629 0.345024 11.00000 0.07393 0.08143 =
0.12302 -0.03609 0.04321 -0.03300
AFIX 137
H39A 2 0.881528 0.485277 0.372252 11.00000 -1.50000
H39B 2 0.926479 0.518099 0.306740 11.00000 -1.50000
H39C 2 0.987646 0.479509 0.373482 11.00000 -1.50000
AFIX 0
HKLF 4
REM IS410QAU_0m in P2(1)/n COLORLESS PRISM
REM R1 = 0.0461 for 4788 Fo > 4sig(Fo) and 0.1123 for all 8784 data
REM 425 parameters refined using 0 restraints
END
WGHT 0.0297 0.0000
REM Instructions for potential hydrogen bonds
HTAB N1 O1
HTAB N1 Br1_$1
HTAB N2 Br1
HTAB C2 S1
HTAB C20 S1
HTAB C32 Br1
HTAB C39 Br1
REM Highest difference peak 0.396, deepest hole -0.316, 1-sigma level 0.065
Q1 1 0.7365 0.4743 0.3653 11.00000 0.05 0.40
Q2 1 0.6919 0.4379 0.3974 11.00000 0.05 0.28
Q3 1 0.6245 0.4371 0.3300 11.00000 0.05 0.28
Q4 1 0.5442 0.2835 0.3319 11.00000 0.05 0.28
Q5 1 0.6618 0.2594 0.4149 11.00000 0.05 0.27
Q6 1 0.4517 0.3458 0.2634 11.00000 0.05 0.27
Q7 1 0.3873 -0.2108 0.2236 11.00000 0.05 0.27
Q8 1 0.4595 0.3655 0.1667 11.00000 0.05 0.27
Q9 1 0.8215 0.2762 0.5069 11.00000 0.05 0.26
Q10 1 0.5609 0.3100 0.2967 11.00000 0.05 0.25
Q11 1 0.4773 0.2201 0.2943 11.00000 0.05 0.25
Q12 1 0.7021 0.2995 0.3566 11.00000 0.05 0.25
Q13 1 0.6075 0.5221 0.3157 11.00000 0.05 0.25
Q14 1 0.8669 0.1881 0.5095 11.00000 0.05 0.25
Q15 1 0.5807 0.4888 0.3458 11.00000 0.05 0.25
Q16 1 0.5370 0.3308 0.3405 11.00000 0.05 0.24
Q17 1 0.7992 0.3994 0.4547 11.00000 0.05 0.24
Q18 1 0.7197 0.3275 0.7245 11.00000 0.05 0.24
Q19 1 0.2351 0.4812 0.2617 11.00000 0.05 0.24
Q20 1 0.8759 0.1968 0.4425 11.00000 0.05 0.24
;
_shelx_res_checksum 31491
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_IS411NEWQAU
_database_code_depnum_ccdc_archive 'CCDC 1889117'
loop_
_audit_author_name
_audit_author_address
'ISHTIAQ KHAN'
;phd scholar
Pakistan
;
_audit_update_record
;
2019-01-07 deposited with the CCDC. 2019-11-27 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_absolute_configuration .
_chemical_name_systematic
;
Iodo-(N-carbamothioylacetamide)-bis(triphenylphosphine)-copper(i)
;
_chemical_formula_moiety 'C39 H36 Cu I N2 O P2 S'
_chemical_formula_sum 'C39 H36 Cu I N2 O P2 S'
_chemical_formula_iupac 'C39 H36 Cu I N2 O P2 S'
_chemical_formula_weight 833.14
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/n'
_space_group_name_Hall '-P 2yn'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.149(3)
_cell_length_b 13.291(2)
_cell_length_c 20.563(5)
_cell_angle_alpha 90
_cell_angle_beta 100.843(12)
_cell_angle_gamma 90
_cell_volume 3798.0(13)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 4788
_cell_measurement_theta_min 2.226
_cell_measurement_theta_max 27.883
_cell_measurement_temperature 296(2)
_exptl_crystal_description plate
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.37
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.14
_exptl_crystal_density_diffrn 1.457
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1680
_exptl_absorpt_coefficient_mu 1.559
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Bruker, 2005)'
_exptl_absorpt_correction_T_min 0.630
_exptl_absorpt_correction_T_max 0.825
_exptl_special_details
;
;
_diffrn_ambient_temperature 296(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Kappa APEXII CCD'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean 0.76
_diffrn_reflns_number 26493
_diffrn_reflns_av_unetI/netI 0.0898
_diffrn_reflns_av_R_equivalents 0.0671
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 2.226
_diffrn_reflns_theta_max 27.831
_diffrn_reflns_theta_full 27.883
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_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^ >
\s(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.
;
_reflns_number_total 8949
_reflns_number_gt 4816
_reflns_threshold_expression I>2\s(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.1130
_refine_ls_R_factor_gt 0.0511
_refine_ls_wR_factor_ref 0.1243
_refine_ls_wR_factor_gt 0.1026
_refine_ls_goodness_of_fit_ref 0.992
_refine_ls_restrained_S_all 0.992
_refine_ls_number_reflns 8949
_refine_ls_number_parameters 390
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'SAINT (Bruker, 2007)'
_computing_data_reduction 'SAINT (Bruker, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material
;
WinGX (Farrugia, 1999) and PLATON (Spek, 2009)
;
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1626(3) 0.2795(3) 0.0153(2) 0.0544(11) Uani 1 1 d . . . . .
C2 C 0.0910(4) 0.3464(4) 0.0216(3) 0.0832(16) Uani 1 1 d . . . . .
H2 H 0.1070 0.4068 0.0437 0.100 Uiso 1 1 calc R U . . .
C3 C -0.0056(4) 0.3256(5) -0.0047(3) 0.103(2) Uani 1 1 d . . . . .
H3 H -0.0529 0.3720 0.0004 0.124 Uiso 1 1 calc R U . . .
C4 C -0.0303(4) 0.2395(5) -0.0370(4) 0.102(2) Uani 1 1 d . . . . .
H4 H -0.0943 0.2262 -0.0554 0.122 Uiso 1 1 calc R U . . .
C5 C 0.0399(5) 0.1715(5) -0.0427(4) 0.112(2) Uani 1 1 d . . . . .
H5 H 0.0232 0.1113 -0.0650 0.135 Uiso 1 1 calc R U . . .
C6 C 0.1359(4) 0.1906(4) -0.0159(3) 0.0855(18) Uani 1 1 d . . . . .
H6 H 0.1823 0.1423 -0.0192 0.103 Uiso 1 1 calc R U . . .
C7 C 0.3441(3) 0.2723(3) -0.0240(2) 0.0562(12) Uani 1 1 d . . . . .
C8 C 0.4281(4) 0.2190(3) -0.0166(3) 0.0703(14) Uani 1 1 d . . . . .
H8 H 0.4575 0.1984 0.0255 0.084 Uiso 1 1 calc R U . . .
C9 C 0.4710(4) 0.1946(4) -0.0703(3) 0.0870(18) Uani 1 1 d . . . . .
H9 H 0.5285 0.1587 -0.0639 0.104 Uiso 1 1 calc R U . . .
C10 C 0.4277(5) 0.2238(5) -0.1318(3) 0.0936(19) Uani 1 1 d . . . . .
H10 H 0.4555 0.2080 -0.1681 0.112 Uiso 1 1 calc R U . . .
C11 C 0.3438(5) 0.2763(5) -0.1405(3) 0.102(2) Uani 1 1 d . . . . .
H11 H 0.3147 0.2956 -0.1831 0.123 Uiso 1 1 calc R U . . .
C12 C 0.3007(4) 0.3018(4) -0.0875(3) 0.0804(15) Uani 1 1 d . . . . .
H12 H 0.2435 0.3382 -0.0944 0.096 Uiso 1 1 calc R U . . .
C13 C 0.3012(3) 0.4360(3) 0.0581(3) 0.0606(12) Uani 1 1 d . . . . .
C14 C 0.3433(4) 0.4971(4) 0.0168(4) 0.098(2) Uani 1 1 d . . . . .
H14 H 0.3674 0.4689 -0.0181 0.118 Uiso 1 1 calc R U . . .
C15 C 0.3495(6) 0.6005(5) 0.0277(5) 0.140(3) Uani 1 1 d . . . . .
H15 H 0.3764 0.6415 -0.0007 0.168 Uiso 1 1 calc R U . . .
C16 C 0.3162(6) 0.6418(5) 0.0798(5) 0.135(3) Uani 1 1 d . . . . .
H16 H 0.3209 0.7109 0.0866 0.162 Uiso 1 1 calc R U . . .
C17 C 0.2763(4) 0.5840(4) 0.1221(4) 0.110(2) Uani 1 1 d . . . . .
H17 H 0.2530 0.6128 0.1572 0.132 Uiso 1 1 calc R U . . .
C18 C 0.2713(4) 0.4799(4) 0.1114(3) 0.0887(18) Uani 1 1 d . . . . .
H18 H 0.2471 0.4392 0.1412 0.106 Uiso 1 1 calc R U . . .
C19A C 0.5493(5) 0.1063(4) 0.2567(3) 0.0695(8) Uani 0.542(12) 1 d G . P A 1
C20A C 0.6407(5) 0.0636(6) 0.2687(4) 0.0695(8) Uani 0.542(12) 1 d G . P A 1
H20A H 0.6849 0.0810 0.2424 0.083 Uiso 0.542(12) 1 calc R U P A 1
C21A C 0.6659(5) -0.0049(6) 0.3201(4) 0.0695(8) Uani 0.542(12) 1 d G . P A 1
H21A H 0.7270 -0.0335 0.3281 0.083 Uiso 0.542(12) 1 calc R U P A 1
C22A C 0.5998(5) -0.0309(4) 0.3594(3) 0.0695(8) Uani 0.542(12) 1 d G . P A 1
H22A H 0.6167 -0.0767 0.3938 0.083 Uiso 0.542(12) 1 calc R U P A 1
C23A C 0.5085(4) 0.0118(7) 0.3474(4) 0.0695(8) Uani 0.542(12) 1 d G . P A 1
H23A H 0.4643 -0.0056 0.3737 0.083 Uiso 0.542(12) 1 calc R U P A 1
C24A C 0.4832(4) 0.0803(7) 0.2960(4) 0.0695(8) Uani 0.542(12) 1 d G . P A 1
H24A H 0.4221 0.1089 0.2880 0.083 Uiso 0.542(12) 1 calc R U P A 1
C19B C 0.5499(6) 0.1105(5) 0.2529(4) 0.0695(8) Uani 0.458(12) 1 d G . P A 2
C20B C 0.6159(7) 0.0330(7) 0.2529(4) 0.0695(8) Uani 0.458(12) 1 d G . P A 2
H20B H 0.6492 0.0271 0.2182 0.083 Uiso 0.458(12) 1 calc R U P A 2
C21B C 0.6321(8) -0.0357(6) 0.3048(5) 0.0695(8) Uani 0.458(12) 1 d G . P A 2
H21B H 0.6762 -0.0875 0.3048 0.083 Uiso 0.458(12) 1 calc R U P A 2
C22B C 0.5823(6) -0.0268(5) 0.3567(4) 0.0695(8) Uani 0.458(12) 1 d G . P A 2
H22B H 0.5931 -0.0728 0.3914 0.083 Uiso 0.458(12) 1 calc R U P A 2
C23B C 0.5163(6) 0.0506(8) 0.3567(4) 0.0695(8) Uani 0.458(12) 1 d G . P A 2
H23B H 0.4830 0.0565 0.3914 0.083 Uiso 0.458(12) 1 calc R U P A 2
C24B C 0.5001(7) 0.1193(7) 0.3048(4) 0.0695(8) Uani 0.458(12) 1 d G . P A 2
H24B H 0.4559 0.1711 0.3048 0.083 Uiso 0.458(12) 1 calc R U P A 2
C25 C 0.5604(3) 0.3198(3) 0.2218(2) 0.0510(11) Uani 1 1 d . . . . .
C26 C 0.5294(3) 0.4048(3) 0.1864(3) 0.0810(17) Uani 1 1 d . . . . .
H26 H 0.4849 0.3992 0.1471 0.097 Uiso 1 1 calc R U . . .
C27 C 0.5631(4) 0.4983(4) 0.2082(4) 0.095(2) Uani 1 1 d . . . . .
H27 H 0.5422 0.5548 0.1830 0.115 Uiso 1 1 calc R U . . .
C28 C 0.6269(5) 0.5090(4) 0.2666(4) 0.0861(19) Uani 1 1 d . . . . .
H28 H 0.6496 0.5724 0.2810 0.103 Uiso 1 1 calc R U . . .
C29 C 0.6570(4) 0.4255(5) 0.3035(3) 0.0910(18) Uani 1 1 d . . . . .
H29 H 0.6999 0.4320 0.3435 0.109 Uiso 1 1 calc R U . . .
C30 C 0.6237(4) 0.3313(4) 0.2813(3) 0.0718(14) Uani 1 1 d . . . . .
H30 H 0.6443 0.2749 0.3068 0.086 Uiso 1 1 calc R U . . .
C31 C 0.6039(3) 0.1672(3) 0.1343(2) 0.0510(11) Uani 1 1 d . . . . .
C32 C 0.6845(3) 0.2244(3) 0.1309(3) 0.0685(14) Uani 1 1 d . . . . .
H32 H 0.6965 0.2825 0.1562 0.082 Uiso 1 1 calc R U . . .
C33 C 0.7475(4) 0.1963(4) 0.0901(3) 0.0823(17) Uani 1 1 d . . . . .
H33 H 0.8017 0.2353 0.0887 0.099 Uiso 1 1 calc R U . . .
C34 C 0.7306(4) 0.1115(4) 0.0521(3) 0.0782(15) Uani 1 1 d . . . . .
H34 H 0.7724 0.0935 0.0241 0.094 Uiso 1 1 calc R U . . .
C35 C 0.6517(4) 0.0532(4) 0.0555(3) 0.0716(14) Uani 1 1 d . . . . .
H35 H 0.6407 -0.0054 0.0304 0.086 Uiso 1 1 calc R U . . .
C36 C 0.5884(3) 0.0810(3) 0.0959(2) 0.0623(13) Uani 1 1 d . . . . .
H36 H 0.5347 0.0413 0.0974 0.075 Uiso 1 1 calc R U . . .
C37 C 0.1817(3) 0.2699(3) 0.2230(3) 0.0605(13) Uani 1 1 d . . . . .
C38 C 0.0397(4) 0.1724(4) 0.1679(3) 0.0816(17) Uani 1 1 d . . . . .
C39 C 0.0171(4) 0.0820(4) 0.1243(4) 0.117(3) Uani 1 1 d . . . . .
H39A H 0.0433 0.0230 0.1480 0.176 Uiso 1 1 calc R U . . .
H39B H 0.0450 0.0900 0.0855 0.176 Uiso 1 1 calc R U . . .
H39C H -0.0514 0.0750 0.1114 0.176 Uiso 1 1 calc R U . . .
Cu1 Cu 0.35668(4) 0.20910(4) 0.14202(3) 0.05096(16) Uani 1 1 d . . . . .
I1 I 0.29717(2) 0.01828(2) 0.12263(2) 0.06792(14) Uani 1 1 d . . . . .
N1 N 0.1280(3) 0.3318(3) 0.2490(2) 0.0898(15) Uani 1 1 d . . . . .
H1A H 0.0666 0.3238 0.2418 0.108 Uiso 1 1 calc R U . . .
H1B H 0.1539 0.3807 0.2735 0.108 Uiso 1 1 calc R U . . .
N2 N 0.1373(3) 0.1931(3) 0.1844(2) 0.0674(11) Uani 1 1 d . . . . .
H2A H 0.1747 0.1528 0.1685 0.081 Uiso 1 1 calc R U . . .
O1 O -0.0201(3) 0.2236(3) 0.1870(3) 0.1108(16) Uani 1 1 d . . . . .
P1 P 0.29122(8) 0.29908(8) 0.04849(6) 0.0514(3) Uani 1 1 d . . . . .
P2 P 0.51722(8) 0.19896(8) 0.18691(6) 0.0489(3) Uani 1 1 d . . . . .
S1 S 0.30225(9) 0.28210(9) 0.23525(7) 0.0694(4) Uani 1 1 d . . . . .
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
C1 0.056(3) 0.058(3) 0.048(3) 0.000(2) 0.007(2) -0.003(2)
C2 0.069(4) 0.083(4) 0.090(5) -0.014(3) -0.006(3) 0.011(3)
C3 0.058(4) 0.121(5) 0.126(7) -0.020(4) 0.005(4) 0.012(3)
C4 0.056(4) 0.130(5) 0.114(6) -0.012(4) 0.002(4) -0.024(4)
C5 0.077(4) 0.096(4) 0.157(7) -0.045(4) 0.001(4) -0.023(4)
C6 0.063(3) 0.074(3) 0.115(5) -0.024(3) 0.005(3) -0.012(3)
C7 0.052(3) 0.061(3) 0.054(3) 0.003(2) 0.005(2) -0.014(2)
C8 0.072(3) 0.083(3) 0.055(4) 0.008(3) 0.009(3) 0.003(3)
C9 0.081(4) 0.096(4) 0.093(5) -0.004(4) 0.040(4) -0.002(3)
C10 0.095(5) 0.125(5) 0.067(5) -0.012(4) 0.030(4) -0.034(4)
C11 0.086(5) 0.167(6) 0.052(4) 0.021(4) 0.006(4) -0.026(4)
C12 0.068(3) 0.121(4) 0.051(4) 0.014(3) 0.011(3) -0.008(3)
C13 0.061(3) 0.049(3) 0.065(4) -0.001(2) -0.006(3) -0.003(2)
C14 0.104(5) 0.067(4) 0.120(6) 0.011(3) 0.015(4) -0.021(3)
C15 0.196(8) 0.062(5) 0.159(9) 0.009(4) 0.024(7) -0.045(5)
C16 0.160(7) 0.051(4) 0.181(10) -0.014(5) -0.005(7) -0.019(4)
C17 0.112(5) 0.061(4) 0.150(7) -0.032(4) 0.009(5) -0.006(3)
C18 0.104(4) 0.054(3) 0.101(6) -0.003(3) 0.002(4) 0.000(3)
C19A 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C20A 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C21A 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C22A 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C23A 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C24A 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C19B 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C20B 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C21B 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C22B 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C23B 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C24B 0.0766(18) 0.0623(17) 0.068(2) 0.0144(14) 0.0089(15) 0.0042(14)
C25 0.048(3) 0.049(2) 0.054(3) -0.004(2) 0.006(2) -0.001(2)
C26 0.070(3) 0.061(3) 0.101(5) 0.001(3) -0.010(3) -0.014(3)
C27 0.082(4) 0.049(3) 0.152(7) 0.009(3) 0.013(4) -0.003(3)
C28 0.083(4) 0.065(4) 0.115(6) -0.037(4) 0.033(4) -0.022(3)
C29 0.105(5) 0.086(4) 0.081(5) -0.030(4) 0.016(4) -0.019(4)
C30 0.081(4) 0.066(3) 0.062(4) -0.010(3) -0.004(3) 0.002(3)
C31 0.049(3) 0.053(3) 0.049(3) 0.003(2) 0.004(2) 0.004(2)
C32 0.066(3) 0.070(3) 0.070(4) -0.007(3) 0.015(3) -0.003(3)
C33 0.056(3) 0.096(4) 0.100(5) -0.010(4) 0.028(3) -0.018(3)
C34 0.073(4) 0.096(4) 0.069(4) -0.008(3) 0.023(3) 0.011(3)
C35 0.074(3) 0.071(3) 0.070(4) -0.017(3) 0.011(3) 0.004(3)
C36 0.062(3) 0.064(3) 0.062(4) -0.010(2) 0.014(3) -0.001(2)
C37 0.071(3) 0.054(3) 0.061(3) 0.000(2) 0.025(3) -0.002(2)
C38 0.079(4) 0.085(4) 0.092(5) -0.014(3) 0.041(4) -0.023(3)
C39 0.087(4) 0.119(5) 0.157(8) -0.057(5) 0.051(5) -0.047(4)
Cu1 0.0509(3) 0.0536(3) 0.0466(4) -0.0002(2) 0.0044(3) -0.0012(2)
I1 0.0924(3) 0.04680(19) 0.0681(3) -0.00439(15) 0.0241(2) -0.00551(16)
N1 0.075(3) 0.083(3) 0.120(5) -0.044(3) 0.041(3) -0.007(2)
N2 0.062(3) 0.069(2) 0.077(3) -0.023(2) 0.029(2) -0.012(2)
O1 0.072(3) 0.103(3) 0.167(5) -0.037(3) 0.047(3) -0.014(2)
P1 0.0551(7) 0.0453(6) 0.0506(8) 0.0027(5) 0.0016(6) -0.0044(5)
P2 0.0488(7) 0.0502(6) 0.0458(7) -0.0022(5) 0.0041(5) 0.0010(5)
S1 0.0637(8) 0.0807(8) 0.0637(9) -0.0232(7) 0.0119(7) 0.0001(6)
_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
C1 C6 1.364(6) . ?
C1 C2 1.372(6) . ?
C1 P1 1.837(5) . ?
C2 C3 1.400(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.336(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.364(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.390(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.367(6) . ?
C7 C12 1.392(7) . ?
C7 P1 1.824(5) . ?
C8 C9 1.394(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.355(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.360(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.388(8) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.377(7) . ?
C13 C14 1.386(7) . ?
C13 P1 1.833(4) . ?
C14 C15 1.393(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.366(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.359(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.401(7) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19A C20A 1.3900 . ?
C19A C24A 1.3900 . ?
C19A P2 1.881(5) . ?
C20A C21A 1.3900 . ?
C20A H20A 0.9300 . ?
C21A C22A 1.3900 . ?
C21A H21A 0.9300 . ?
C22A C23A 1.3900 . ?
C22A H22A 0.9300 . ?
C23A C24A 1.3900 . ?
C23A H23A 0.9300 . ?
C24A H24A 0.9300 . ?
C19B C20B 1.3900 . ?
C19B C24B 1.3900 . ?
C19B P2 1.789(6) . ?
C20B C21B 1.3900 . ?
C20B H20B 0.9300 . ?
C21B C22B 1.3900 . ?
C21B H21B 0.9300 . ?
C22B C23B 1.3900 . ?
C22B H22B 0.9300 . ?
C23B C24B 1.3900 . ?
C23B H23B 0.9300 . ?
C24B H24B 0.9300 . ?
C25 C26 1.372(6) . ?
C25 C30 1.381(7) . ?
C25 P2 1.817(4) . ?
C26 C27 1.375(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.367(9) . ?
C27 H27 0.9300 . ?
C28 C29 1.366(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.385(7) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.383(6) . ?
C31 C36 1.385(6) . ?
C31 P2 1.831(4) . ?
C32 C33 1.384(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.367(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.372(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.382(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 N1 1.301(5) . ?
C37 N2 1.371(6) . ?
C37 S1 1.684(5) . ?
C38 O1 1.208(5) . ?
C38 N2 1.387(6) . ?
C38 C39 1.497(7) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
Cu1 P2 2.2893(13) . ?
Cu1 P1 2.3058(14) . ?
Cu1 S1 2.4009(14) . ?
Cu1 I1 2.6785(7) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N2 H2A 0.8600 . ?
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
C6 C1 C2 117.4(5) . . ?
C6 C1 P1 117.7(4) . . ?
C2 C1 P1 124.8(4) . . ?
C1 C2 C3 121.4(5) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C4 C3 C2 120.4(5) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 118.9(6) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C4 C5 C6 121.2(5) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 120.6(5) . . ?
C1 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C8 C7 C12 118.1(5) . . ?
C8 C7 P1 119.5(4) . . ?
C12 C7 P1 122.4(4) . . ?
C7 C8 C9 122.2(5) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C10 C9 C8 119.0(6) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C11 120.0(6) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 C12 121.6(6) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C7 119.1(5) . . ?
C11 C12 H12 120.4 . . ?
C7 C12 H12 120.5 . . ?
C18 C13 C14 118.1(5) . . ?
C18 C13 P1 118.5(4) . . ?
C14 C13 P1 123.3(4) . . ?
C13 C14 C15 120.1(7) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 120.1(7) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C17 C16 C15 121.5(7) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 118.2(7) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C13 C18 C17 122.0(6) . . ?
C13 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?
C20A C19A C24A 120.0 . . ?
C20A C19A P2 119.1(4) . . ?
C24A C19A P2 120.9(4) . . ?
C21A C20A C19A 120.0 . . ?
C21A C20A H20A 120.0 . . ?
C19A C20A H20A 120.0 . . ?
C20A C21A C22A 120.0 . . ?
C20A C21A H21A 120.0 . . ?
C22A C21A H21A 120.0 . . ?
C23A C22A C21A 120.0 . . ?
C23A C22A H22A 120.0 . . ?
C21A C22A H22A 120.0 . . ?
C22A C23A C24A 120.0 . . ?
C22A C23A H23A 120.0 . . ?
C24A C23A H23A 120.0 . . ?
C23A C24A C19A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C19A C24A H24A 120.0 . . ?
C20B C19B C24B 120.0 . . ?
C20B C19B P2 124.4(5) . . ?
C24B C19B P2 115.5(5) . . ?
C21B C20B C19B 120.0 . . ?
C21B C20B H20B 120.0 . . ?
C19B C20B H20B 120.0 . . ?
C22B C21B C20B 120.0 . . ?
C22B C21B H21B 120.0 . . ?
C20B C21B H21B 120.0 . . ?
C21B C22B C23B 120.0 . . ?
C21B C22B H22B 120.0 . . ?
C23B C22B H22B 120.0 . . ?
C22B C23B C24B 120.0 . . ?
C22B C23B H23B 120.0 . . ?
C24B C23B H23B 120.0 . . ?
C23B C24B C19B 120.0 . . ?
C23B C24B H24B 120.0 . . ?
C19B C24B H24B 120.0 . . ?
C26 C25 C30 117.9(4) . . ?
C26 C25 P2 117.9(4) . . ?
C30 C25 P2 124.2(4) . . ?
C25 C26 C27 121.0(6) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C28 C27 C26 120.8(6) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C29 C28 C27 119.3(5) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C28 C29 C30 120.0(6) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C25 C30 C29 121.1(5) . . ?
C25 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
C32 C31 C36 118.0(4) . . ?
C32 C31 P2 123.6(3) . . ?
C36 C31 P2 118.4(3) . . ?
C31 C32 C33 120.9(5) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C34 C33 C32 120.4(5) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 119.5(5) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C34 C35 C36 120.3(5) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C31 120.8(4) . . ?
C35 C36 H36 119.6 . . ?
C31 C36 H36 119.6 . . ?
N1 C37 N2 118.0(4) . . ?
N1 C37 S1 122.1(4) . . ?
N2 C37 S1 119.9(3) . . ?
O1 C38 N2 122.3(5) . . ?
O1 C38 C39 124.3(5) . . ?
N2 C38 C39 113.3(5) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
P2 Cu1 P1 125.40(5) . . ?
P2 Cu1 S1 98.33(5) . . ?
P1 Cu1 S1 108.51(5) . . ?
P2 Cu1 I1 105.34(3) . . ?
P1 Cu1 I1 107.53(4) . . ?
S1 Cu1 I1 111.25(4) . . ?
C37 N1 H1A 120.0 . . ?
C37 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C37 N2 C38 128.1(4) . . ?
C37 N2 H2A 116.0 . . ?
C38 N2 H2A 116.0 . . ?
C7 P1 C13 104.3(2) . . ?
C7 P1 C1 101.5(2) . . ?
C13 P1 C1 103.4(2) . . ?
C7 P1 Cu1 114.70(16) . . ?
C13 P1 Cu1 114.50(17) . . ?
C1 P1 Cu1 116.78(14) . . ?
C19B P2 C25 105.2(3) . . ?
C19B P2 C31 101.0(3) . . ?
C25 P2 C31 102.95(19) . . ?
C25 P2 C19A 105.2(3) . . ?
C31 P2 C19A 102.0(3) . . ?
C19B P2 Cu1 116.1(3) . . ?
C25 P2 Cu1 110.00(14) . . ?
C31 P2 Cu1 119.96(15) . . ?
C19A P2 Cu1 115.2(2) . . ?
C37 S1 Cu1 108.05(18) . . ?
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
C6 C1 C2 C3 -1.8(8) . . . . ?
P1 C1 C2 C3 -179.5(5) . . . . ?
C1 C2 C3 C4 -0.3(10) . . . . ?
C2 C3 C4 C5 1.4(11) . . . . ?
C3 C4 C5 C6 -0.3(11) . . . . ?
C2 C1 C6 C5 2.9(9) . . . . ?
P1 C1 C6 C5 -179.3(5) . . . . ?
C4 C5 C6 C1 -1.9(11) . . . . ?
C12 C7 C8 C9 0.5(7) . . . . ?
P1 C7 C8 C9 178.8(4) . . . . ?
C7 C8 C9 C10 -0.5(8) . . . . ?
C8 C9 C10 C11 0.1(9) . . . . ?
C9 C10 C11 C12 0.4(9) . . . . ?
C10 C11 C12 C7 -0.5(9) . . . . ?
C8 C7 C12 C11 0.0(7) . . . . ?
P1 C7 C12 C11 -178.2(4) . . . . ?
C18 C13 C14 C15 -3.6(9) . . . . ?
P1 C13 C14 C15 -179.1(5) . . . . ?
C13 C14 C15 C16 1.5(12) . . . . ?
C14 C15 C16 C17 -0.1(14) . . . . ?
C15 C16 C17 C18 0.9(12) . . . . ?
C14 C13 C18 C17 4.5(8) . . . . ?
P1 C13 C18 C17 -179.8(4) . . . . ?
C16 C17 C18 C13 -3.1(10) . . . . ?
C24A C19A C20A C21A 0.0 . . . . ?
P2 C19A C20A C21A 179.9(5) . . . . ?
C19A C20A C21A C22A 0.0 . . . . ?
C20A C21A C22A C23A 0.0 . . . . ?
C21A C22A C23A C24A 0.0 . . . . ?
C22A C23A C24A C19A 0.0 . . . . ?
C20A C19A C24A C23A 0.0 . . . . ?
P2 C19A C24A C23A -179.9(5) . . . . ?
C24B C19B C20B C21B 0.0 . . . . ?
P2 C19B C20B C21B -176.1(7) . . . . ?
C19B C20B C21B C22B 0.0 . . . . ?
C20B C21B C22B C23B 0.0 . . . . ?
C21B C22B C23B C24B 0.0 . . . . ?
C22B C23B C24B C19B 0.0 . . . . ?
C20B C19B C24B C23B 0.0 . . . . ?
P2 C19B C24B C23B 176.4(6) . . . . ?
C30 C25 C26 C27 2.4(7) . . . . ?
P2 C25 C26 C27 -176.6(4) . . . . ?
C25 C26 C27 C28 -1.4(9) . . . . ?
C26 C27 C28 C29 -0.2(9) . . . . ?
C27 C28 C29 C30 0.7(8) . . . . ?
C26 C25 C30 C29 -1.9(7) . . . . ?
P2 C25 C30 C29 177.1(4) . . . . ?
C28 C29 C30 C25 0.3(8) . . . . ?
C36 C31 C32 C33 0.1(7) . . . . ?
P2 C31 C32 C33 179.9(4) . . . . ?
C31 C32 C33 C34 0.5(9) . . . . ?
C32 C33 C34 C35 -1.3(9) . . . . ?
C33 C34 C35 C36 1.4(8) . . . . ?
C34 C35 C36 C31 -0.8(8) . . . . ?
C32 C31 C36 C35 0.0(7) . . . . ?
P2 C31 C36 C35 -179.8(4) . . . . ?
N1 C37 N2 C38 1.1(8) . . . . ?
S1 C37 N2 C38 -178.7(4) . . . . ?
O1 C38 N2 C37 0.2(9) . . . . ?
C39 C38 N2 C37 179.8(5) . . . . ?
C8 C7 P1 C13 113.3(4) . . . . ?
C12 C7 P1 C13 -68.5(4) . . . . ?
C8 C7 P1 C1 -139.6(4) . . . . ?
C12 C7 P1 C1 38.7(4) . . . . ?
C8 C7 P1 Cu1 -12.8(4) . . . . ?
C12 C7 P1 Cu1 165.5(3) . . . . ?
C18 C13 P1 C7 -176.8(4) . . . . ?
C14 C13 P1 C7 -1.3(5) . . . . ?
C18 C13 P1 C1 77.5(5) . . . . ?
C14 C13 P1 C1 -107.0(5) . . . . ?
C18 C13 P1 Cu1 -50.6(4) . . . . ?
C14 C13 P1 Cu1 124.8(4) . . . . ?
C6 C1 P1 C7 52.7(4) . . . . ?
C2 C1 P1 C7 -129.6(4) . . . . ?
C6 C1 P1 C13 160.6(4) . . . . ?
C2 C1 P1 C13 -21.8(5) . . . . ?
C6 C1 P1 Cu1 -72.8(4) . . . . ?
C2 C1 P1 Cu1 104.9(4) . . . . ?
C20B C19B P2 C25 -114.5(7) . . . . ?
C24B C19B P2 C25 69.2(5) . . . . ?
C20B C19B P2 C31 -7.7(7) . . . . ?
C24B C19B P2 C31 176.0(5) . . . . ?
C20B C19B P2 Cu1 123.7(6) . . . . ?
C24B C19B P2 Cu1 -52.6(6) . . . . ?
C26 C25 P2 C19B -167.7(4) . . . . ?
C30 C25 P2 C19B 13.4(5) . . . . ?
C26 C25 P2 C31 87.0(4) . . . . ?
C30 C25 P2 C31 -92.0(4) . . . . ?
C26 C25 P2 C19A -166.6(4) . . . . ?
C30 C25 P2 C19A 14.5(5) . . . . ?
C26 C25 P2 Cu1 -42.0(4) . . . . ?
C30 C25 P2 Cu1 139.1(4) . . . . ?
C32 C31 P2 C19B -103.9(5) . . . . ?
C36 C31 P2 C19B 75.8(5) . . . . ?
C32 C31 P2 C25 4.6(4) . . . . ?
C36 C31 P2 C25 -175.6(4) . . . . ?
C32 C31 P2 C19A -104.3(4) . . . . ?
C36 C31 P2 C19A 75.5(4) . . . . ?
C32 C31 P2 Cu1 127.1(4) . . . . ?
C36 C31 P2 Cu1 -53.1(4) . . . . ?
C20A C19A P2 C25 -85.2(5) . . . . ?
C24A C19A P2 C25 94.7(5) . . . . ?
C20A C19A P2 C31 21.9(5) . . . . ?
C24A C19A P2 C31 -158.2(5) . . . . ?
C20A C19A P2 Cu1 153.5(4) . . . . ?
C24A C19A P2 Cu1 -26.6(5) . . . . ?
N1 C37 S1 Cu1 -153.2(4) . . . . ?
N2 C37 S1 Cu1 26.6(4) . . . . ?
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
C18 H18 S1 0.93 2.85 3.629(6) 141.7 .
C24A H24A S1 0.93 2.94 3.756(6) 146.8 .
C24B H24B S1 0.93 2.79 3.614(6) 148.3 .
N1 H1A O1 0.86 2.01 2.661(6) 132.1 .
N1 H1B I1 0.86 2.80 3.630(4) 163.1 2
N2 H2A I1 0.86 2.78 3.635(4) 177.4 .
_refine_diff_density_max 0.822
_refine_diff_density_min -0.614
_refine_diff_density_rms 0.080
_shelx_res_file
;
shelx.res created by SHELXL-2014/7
TITL IS411NEWQAU_0m in P2(1)/n COLORLESS PLATE
CELL 0.71073 14.1491 13.2914 20.5626 90.000 100.843 90.000
ZERR 4.00 0.0027 0.0020 0.0048 0.000 0.012 0.000
LATT 1
SYMM -x+1/2, y+1/2, -z+1/2
SFAC C H N O P S Cu I
UNIT 156 144 8 4 8 4 4 4
L.S. 20
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.37 0.18 0.14
CONF
HTAB
OMIT 0 0 2
OMIT-1 0 1
OMIT 0 1 1
OMIT 1 0 1
TEMP 23.000
EADP C19A C20A C21A C22A C23A C24A C19B C20B C21B C22B C23B C24B
HTAB C18 S1
HTAB C24A S1
HTAB C24B S1
HTAB N1 O1
EQIV $1 -x+1/2, y+1/2, -z+1/2
HTAB N1 I1_$1
HTAB N2 I1
WGHT 0.039500
FVAR 0.27781 0.54200
C1 1 0.162634 0.279507 0.015319 11.00000 0.05584 0.05789 =
0.04846 -0.00022 0.00741 -0.00292
C2 1 0.091006 0.346393 0.021557 11.00000 0.06864 0.08313 =
0.08962 -0.01433 -0.00613 0.01084
AFIX 43
H2 2 0.106994 0.406816 0.043711 11.00000 -1.20000
AFIX 0
C3 1 -0.005632 0.325605 -0.004720 11.00000 0.05776 0.12054 =
0.12582 -0.01998 0.00450 0.01241
AFIX 43
H3 2 -0.052924 0.371985 0.000351 11.00000 -1.20000
AFIX 0
C4 1 -0.030322 0.239538 -0.037039 11.00000 0.05605 0.13008 =
0.11382 -0.01200 0.00207 -0.02368
AFIX 43
H4 2 -0.094322 0.226210 -0.055353 11.00000 -1.20000
AFIX 0
C5 1 0.039870 0.171517 -0.042741 11.00000 0.07656 0.09597 =
0.15675 -0.04528 0.00129 -0.02307
AFIX 43
H5 2 0.023177 0.111310 -0.064996 11.00000 -1.20000
AFIX 0
C6 1 0.135863 0.190560 -0.015898 11.00000 0.06277 0.07383 =
0.11511 -0.02399 0.00458 -0.01226
AFIX 43
H6 2 0.182260 0.142254 -0.019242 11.00000 -1.20000
AFIX 0
C7 1 0.344095 0.272256 -0.023985 11.00000 0.05207 0.06086 =
0.05369 0.00349 0.00452 -0.01409
C8 1 0.428070 0.218995 -0.016634 11.00000 0.07164 0.08257 =
0.05538 0.00768 0.00893 0.00314
AFIX 43
H8 2 0.457535 0.198382 0.025541 11.00000 -1.20000
AFIX 0
C9 1 0.471000 0.194557 -0.070279 11.00000 0.08143 0.09561 =
0.09327 -0.00403 0.04039 -0.00155
AFIX 43
H9 2 0.528457 0.158721 -0.063922 11.00000 -1.20000
AFIX 0
C10 1 0.427749 0.223801 -0.131808 11.00000 0.09496 0.12488 =
0.06694 -0.01166 0.03035 -0.03379
AFIX 43
H10 2 0.455460 0.207954 -0.168094 11.00000 -1.20000
AFIX 0
C11 1 0.343837 0.276316 -0.140540 11.00000 0.08616 0.16655 =
0.05171 0.02050 0.00640 -0.02592
AFIX 43
H11 2 0.314663 0.295611 -0.183062 11.00000 -1.20000
AFIX 0
C12 1 0.300659 0.301828 -0.087534 11.00000 0.06847 0.12144 =
0.05119 0.01421 0.01090 -0.00826
AFIX 43
H12 2 0.243485 0.338185 -0.094385 11.00000 -1.20000
AFIX 0
C13 1 0.301186 0.436016 0.058057 11.00000 0.06124 0.04887 =
0.06455 -0.00098 -0.00615 -0.00290
C14 1 0.343274 0.497075 0.016849 11.00000 0.10397 0.06734 =
0.12025 0.01082 0.01496 -0.02067
AFIX 43
H14 2 0.367387 0.468924 -0.018094 11.00000 -1.20000
AFIX 0
C15 1 0.349528 0.600529 0.027669 11.00000 0.19568 0.06238 =
0.15927 0.00914 0.02392 -0.04547
AFIX 43
H15 2 0.376437 0.641532 -0.000666 11.00000 -1.20000
AFIX 0
C16 1 0.316184 0.641787 0.079842 11.00000 0.15965 0.05111 =
0.18101 -0.01414 -0.00484 -0.01893
AFIX 43
H16 2 0.320853 0.710934 0.086601 11.00000 -1.20000
AFIX 0
C17 1 0.276318 0.584023 0.122119 11.00000 0.11245 0.06091 =
0.15009 -0.03174 0.00906 -0.00614
AFIX 43
H17 2 0.252995 0.612831 0.157184 11.00000 -1.20000
AFIX 0
C18 1 0.271326 0.479895 0.111418 11.00000 0.10419 0.05410 =
0.10123 -0.00329 0.00213 -0.00010
AFIX 43
H18 2 0.247128 0.439189 0.141237 11.00000 -1.20000
AFIX 66
PART 1
C19A 1 0.549336 0.106271 0.256681 21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
C20A 1 0.640667 0.063628 0.268718 21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H20A 2 0.684887 0.080972 0.242398 21.00000 -1.20000
AFIX 65
C21A 1 0.665906 -0.004937 0.320093 21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H21A 2 0.727013 -0.033468 0.328146 21.00000 -1.20000
AFIX 65
C22A 1 0.599815 -0.030860 0.359431 21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H22A 2 0.616702 -0.076734 0.393804 21.00000 -1.20000
AFIX 65
C23A 1 0.508483 0.011783 0.347394 21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H23A 2 0.464264 -0.005562 0.373714 21.00000 -1.20000
AFIX 65
C24A 1 0.483243 0.080348 0.296020 21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H24A 2 0.422136 0.108878 0.287966 21.00000 -1.20000
AFIX 66
PART 2
C19B 1 0.549893 0.110475 0.252887 -21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
C20B 1 0.615879 0.033001 0.252883 -21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H20B 2 0.649199 0.027105 0.218158 -21.00000 -1.20000
AFIX 65
C21B 1 0.632066 -0.035660 0.304779 -21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H21B 2 0.676215 -0.087495 0.304776 -21.00000 -1.20000
AFIX 65
C22B 1 0.582265 -0.026848 0.356680 -21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H22B 2 0.593096 -0.072787 0.391402 -21.00000 -1.20000
AFIX 65
C23B 1 0.516279 0.050625 0.356685 -21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H23B 2 0.482959 0.056521 0.391410 -21.00000 -1.20000
AFIX 65
C24B 1 0.500091 0.119287 0.304789 -21.00000 0.07663 0.06232 =
0.06776 0.01437 0.00890 0.00416
AFIX 43
H24B 2 0.455942 0.171122 0.304792 -21.00000 -1.20000
AFIX 0
PART 0
C25 1 0.560448 0.319758 0.221839 11.00000 0.04830 0.04876 =
0.05450 -0.00407 0.00600 -0.00096
C26 1 0.529392 0.404829 0.186420 11.00000 0.07020 0.06107 =
0.10149 0.00080 -0.00986 -0.01379
AFIX 43
H26 2 0.484898 0.399213 0.147072 11.00000 -1.20000
AFIX 0
C27 1 0.563060 0.498261 0.208223 11.00000 0.08198 0.04884 =
0.15199 0.00939 0.01294 -0.00262
AFIX 43
H27 2 0.542153 0.554845 0.182974 11.00000 -1.20000
AFIX 0
C28 1 0.626922 0.508971 0.266592 11.00000 0.08309 0.06528 =
0.11537 -0.03652 0.03265 -0.02192
AFIX 43
H28 2 0.649595 0.572361 0.281010 11.00000 -1.20000
AFIX 0
C29 1 0.657048 0.425545 0.303490 11.00000 0.10484 0.08632 =
0.08118 -0.03039 0.01573 -0.01850
AFIX 43
H29 2 0.699909 0.431996 0.343522 11.00000 -1.20000
AFIX 0
C30 1 0.623732 0.331329 0.281258 11.00000 0.08099 0.06555 =
0.06191 -0.00953 -0.00417 0.00230
AFIX 43
H30 2 0.644328 0.274917 0.306775 11.00000 -1.20000
AFIX 0
C31 1 0.603916 0.167189 0.134284 11.00000 0.04863 0.05343 =
0.04871 0.00315 0.00355 0.00386
C32 1 0.684491 0.224358 0.130852 11.00000 0.06570 0.07018 =
0.07040 -0.00735 0.01479 -0.00257
AFIX 43
H32 2 0.696496 0.282484 0.156240 11.00000 -1.20000
AFIX 0
C33 1 0.747530 0.196261 0.090147 11.00000 0.05610 0.09552 =
0.10046 -0.01036 0.02801 -0.01819
AFIX 43
H33 2 0.801661 0.235266 0.088688 11.00000 -1.20000
AFIX 0
C34 1 0.730643 0.111506 0.052092 11.00000 0.07312 0.09588 =
0.06919 -0.00824 0.02254 0.01054
AFIX 43
H34 2 0.772375 0.093486 0.024110 11.00000 -1.20000
AFIX 0
C35 1 0.651665 0.053178 0.055464 11.00000 0.07355 0.07061 =
0.06992 -0.01732 0.01141 0.00402
AFIX 43
H35 2 0.640678 -0.005360 0.030405 11.00000 -1.20000
AFIX 0
C36 1 0.588377 0.080983 0.095905 11.00000 0.06196 0.06391 =
0.06217 -0.01029 0.01447 -0.00147
AFIX 43
H36 2 0.534676 0.041310 0.097370 11.00000 -1.20000
AFIX 0
C37 1 0.181743 0.269939 0.223005 11.00000 0.07056 0.05449 =
0.06138 -0.00005 0.02495 -0.00173
C38 1 0.039691 0.172416 0.167895 11.00000 0.07854 0.08452 =
0.09151 -0.01415 0.04084 -0.02337
C39 1 0.017142 0.081979 0.124306 11.00000 0.08666 0.11860 =
0.15686 -0.05696 0.05100 -0.04737
AFIX 137
H39A 2 0.043283 0.022982 0.148019 11.00000 -1.50000
H39B 2 0.045045 0.090009 0.085526 11.00000 -1.50000
H39C 2 -0.051358 0.074970 0.111431 11.00000 -1.50000
AFIX 0
CU1 7 0.356684 0.209104 0.142021 11.00000 0.05085 0.05356 =
0.04660 -0.00017 0.00439 -0.00123
I1 8 0.297173 0.018281 0.122629 11.00000 0.09235 0.04680 =
0.06811 -0.00439 0.02406 -0.00551
N1 3 0.128044 0.331788 0.249025 11.00000 0.07451 0.08343 =
0.12030 -0.04434 0.04061 -0.00740
AFIX 93
H1A 2 0.066642 0.323788 0.241798 11.00000 -1.20000
H1B 2 0.153946 0.380676 0.273454 11.00000 -1.20000
AFIX 0
N2 3 0.137331 0.193121 0.184410 11.00000 0.06228 0.06893 =
0.07727 -0.02299 0.02932 -0.01174
AFIX 43
H2A 2 0.174662 0.152756 0.168460 11.00000 -1.20000
AFIX 0
O1 4 -0.020104 0.223613 0.187034 11.00000 0.07209 0.10276 =
0.16703 -0.03749 0.04657 -0.01407
P1 5 0.291216 0.299084 0.048493 11.00000 0.05510 0.04535 =
0.05057 0.00272 0.00157 -0.00443
P2 5 0.517219 0.198959 0.186914 11.00000 0.04879 0.05020 =
0.04581 -0.00223 0.00413 0.00103
S1 6 0.302249 0.282097 0.235245 11.00000 0.06373 0.08066 =
0.06367 -0.02316 0.01188 0.00008
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM IS411NEWQAU_0m in P2(1)/n COLORLESS PLATE
REM R1 = 0.0511 for 4816 Fo > 4sig(Fo) and 0.1130 for all 8949 data
REM 390 parameters refined using 0 restraints
END
WGHT 0.0395 0.0000
REM Instructions for potential hydrogen bonds
HTAB C18 S1
HTAB C24A S1
HTAB C24B S1
HTAB N1 O1
HTAB N1 I1_$1
HTAB N2 I1
REM Highest difference peak 0.822, deepest hole -0.614, 1-sigma level 0.080
Q1 1 0.6376 -0.0055 0.3418 11.00000 0.05 0.55
Q2 1 0.2791 0.0265 0.1638 11.00000 0.05 0.42
Q3 1 0.5584 0.0265 0.3644 11.00000 0.05 0.41
Q4 1 0.2586 -0.0392 0.1209 11.00000 0.05 0.40
Q5 1 0.5797 -0.0803 0.3304 11.00000 0.05 0.37
Q6 1 0.6344 0.0367 0.2824 11.00000 0.05 0.35
Q7 1 0.5827 0.2124 -0.0869 11.00000 0.05 0.34
Q8 1 0.3445 -0.0065 0.1319 11.00000 0.05 0.33
Q9 1 0.4609 0.1539 -0.1923 11.00000 0.05 0.33
Q10 1 0.5715 0.1875 0.1752 11.00000 0.05 0.32
Q11 1 0.2018 -0.0098 0.1207 11.00000 0.05 0.31
Q12 1 -0.0412 0.1614 0.0123 11.00000 0.05 0.31
Q13 1 0.3976 0.0403 0.1297 11.00000 0.05 0.30
Q14 1 0.0285 0.1802 0.2267 11.00000 0.05 0.29
Q15 1 0.3399 0.5978 0.1202 11.00000 0.05 0.29
Q16 1 0.0985 0.4187 0.3349 11.00000 0.05 0.29
Q17 1 0.2666 0.2348 0.2347 11.00000 0.05 0.29
Q18 1 -0.0453 0.2362 0.1851 11.00000 0.05 0.28
Q19 1 0.0797 0.0574 0.1042 11.00000 0.05 0.28
Q20 1 0.2648 -0.0588 0.0869 11.00000 0.05 0.28
;
_shelx_res_checksum 71564