# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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
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data_crystal2_cu_a
_audit_block_doi 10.5517/ccdc.csd.cc2145n1
_database_code_depnum_ccdc_archive 'CCDC 1880852'
_audit_update_record
;
2018-11-23 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;
_audit_creation_date 2016-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C18 H24 Cl2 Cu N2, 1(B F4), C6 H16 N'
_chemical_formula_sum 'C24 H40 B Cl2 Cu F4 N3'
_chemical_formula_weight 591.84
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
F F 0.0171 0.0103 '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'
_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 triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.4731(5)
_cell_length_b 13.2115(10)
_cell_length_c 14.9811(11)
_cell_angle_alpha 86.824(4)
_cell_angle_beta 81.552(4)
_cell_angle_gamma 81.251(4)
_cell_volume 1445.20(18)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 8117
_cell_measurement_temperature 221.99
_cell_measurement_theta_max 26.116
_cell_measurement_theta_min 2.751
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.984
_exptl_absorpt_correction_T_max 0.7455
_exptl_absorpt_correction_T_min 0.6772
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1297 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.9084.
The \l/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'bluish green'
_exptl_crystal_colour_modifier bluish
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 1.360
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 618
_exptl_crystal_size_max 0.226
_exptl_crystal_size_mid 0.044
_exptl_crystal_size_min 0.022
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0595
_diffrn_reflns_av_unetI/netI 0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 30697
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 25.000
_diffrn_reflns_theta_max 27.062
_diffrn_reflns_theta_min 2.751
_diffrn_ambient_temperature 221.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4822
_reflns_number_total 6317
_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 v8.34A (Bruker, 2013)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.862
_refine_diff_density_min -0.438
_refine_diff_density_rms 0.057
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 433
_refine_ls_number_reflns 6317
_refine_ls_number_restraints 149
_refine_ls_R_factor_all 0.0619
_refine_ls_R_factor_gt 0.0424
_refine_ls_restrained_S_all 1.065
_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^)+(0.0569P)^2^+0.6322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1096
_refine_ls_wR_factor_ref 0.1222
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H,H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C2T-C1T \\sim C2T'-C1T
with sigma of 0.02
C4T'-C3T \\sim C4T-C3T
with sigma of 0.02
C6T-C5T \\sim C6T'-C5T
with sigma of 0.02
F4A-F3A \\sim F4A-F1A \\sim F3A-F1A \\sim F3A-F2A \\sim F1A-F2A
with sigma of 0.04
B1-F4A \\sim B1-F3A \\sim B1-F1A \\sim B1-F2A
with sigma of 0.02
F1-F2 \\sim F1-F5 \\sim F1-F0AA \\sim F2-F5 \\sim F5-F0AA
with sigma of 0.04
B11-F1 \\sim B11-F2 \\sim B11-F5 \\sim B11-F0AA
with sigma of 0.02
B2-F2AA \\sim B2-F4 \\sim B2-F4A \\sim B2-F1AA
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(B2) = Uanis(B1) = Uanis(B11)
4. Rigid body (RIGU) restrains
C5T, C6T'
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C5T, C6T
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C1T, C2T
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C2T', C1T
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C3T, C4T
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C3T, C4T'
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
B1, F3AA, F2A, F3A, F1A, B2, F4A, F2AA, F1AA, F4, B11, F1, F5, F2, F0AA
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
Fixed Sof: B1(0.33333) H1TC(0.5) H1TD(0.5) H1TA(0.5) H1TB(0.5) C2T(0.5)
H2TA(0.5) H2TB(0.5) H2TC(0.5) H3TA(0.5) H3TB(0.5) H3TC(0.5) H3TD(0.5) C4T(0.5)
H4TA(0.5) H4TB(0.5) H4TC(0.5) H5TC(0.5) H5TD(0.5) H5TA(0.5) H5TB(0.5) C6T(0.5)
H6TA(0.5) H6TB(0.5) H6TC(0.5) C2T'(0.5) H2TD(0.5) H2TE(0.5) H2TF(0.5)
C4T'(0.5) H4TD(0.5) H4TE(0.5) H4TF(0.5) C6T'(0.5) H6TD(0.5) H6TE(0.5)
H6TF(0.5) F4A(0.33333) F3A(0.33333) F1A(0.33333) F2A(0.33333) F1(0.33333)
F2(0.33333) F5(0.33333) F0AA(0.33333) B11(0.33333) B2(0.33333) F1AA(0.33333)
F2AA(0.33333) F4(0.33333) F3AA(0.33333)
6.a Ternary CH refined with riding coordinates:
N1T(H1T)
6.b Secondary CH2 refined with riding coordinates:
C1T(H1TC,H1TD), C1T(H1TA,H1TB), C3T(H3TA,H3TB), C3T(H3TC,H3TD), C5T(H5TC,
H5TD), C5T(H5TA,H5TB)
6.c Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C4(H4), C7(H7), C9(H9), C10(H10)
6.d Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C2T(H2TA,H2TB,H2TC), C4T(H4TA,
H4TB,H4TC), C6T(H6TA,H6TB,H6TC), C2T'(H2TD,H2TE,H2TF), C4T'(H4TD,H4TE,H4TF),
C6T'(H6TD,H6TE,H6TF)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_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
Cu1 Cu 0.17734(4) 0.62444(2) 0.58402(2) 0.03973(12) Uani 1 1 d . . . . .
Cl1 Cl -0.03209(11) 0.65737(6) 0.70395(6) 0.0647(2) Uani 1 1 d . . . . .
Cl2 Cl 0.28134(11) 0.77348(5) 0.58336(6) 0.0600(2) Uani 1 1 d . . . . .
N1 N 0.1591(3) 0.47335(16) 0.58903(14) 0.0372(5) Uani 1 1 d . . . . .
N2 N 0.2986(3) 0.58770(15) 0.45942(14) 0.0368(4) Uani 1 1 d . . . . .
C1 C 0.0862(4) 0.4185(2) 0.66015(17) 0.0441(6) Uani 1 1 d . . . . .
H1 H 0.0290 0.4531 0.7122 0.053 Uiso 1 1 calc R . . . .
C2 C 0.0923(4) 0.3146(2) 0.65952(18) 0.0444(6) Uani 1 1 d . . . . .
H2 H 0.0402 0.2797 0.7109 0.053 Uiso 1 1 calc R . . . .
C3 C 0.1743(3) 0.25993(19) 0.58403(17) 0.0395(6) Uani 1 1 d . . . . .
C4 C 0.2460(3) 0.31794(19) 0.51025(17) 0.0387(5) Uani 1 1 d . . . . .
H4 H 0.3006 0.2852 0.4568 0.046 Uiso 1 1 calc R . . . .
C5 C 0.2376(3) 0.42243(18) 0.51491(16) 0.0341(5) Uani 1 1 d . . . . .
C6 C 0.3126(3) 0.48826(18) 0.43936(16) 0.0348(5) Uani 1 1 d . . . . .
C7 C 0.3853(3) 0.45258(19) 0.35539(16) 0.0384(5) Uani 1 1 d . . . . .
H7 H 0.3971 0.3822 0.3450 0.046 Uiso 1 1 calc R . . . .
C8 C 0.4422(3) 0.5202(2) 0.28508(17) 0.0402(6) Uani 1 1 d . . . . .
C9 C 0.4269(4) 0.6224(2) 0.30732(19) 0.0458(6) Uani 1 1 d . . . . .
H9 H 0.4640 0.6711 0.2630 0.055 Uiso 1 1 calc R . . . .
C10 C 0.3583(4) 0.6527(2) 0.39326(18) 0.0442(6) Uani 1 1 d . . . . .
H10 H 0.3526 0.7219 0.4065 0.053 Uiso 1 1 calc R . . . .
C11 C 0.1927(4) 0.1433(2) 0.58370(19) 0.0482(7) Uani 1 1 d . . . . .
C12 C 0.3443(6) 0.0997(3) 0.6395(3) 0.0871(12) Uani 1 1 d . . . . .
H12A H 0.4584 0.1219 0.6123 0.131 Uiso 1 1 calc GR . . . .
H12B H 0.3580 0.0254 0.6412 0.131 Uiso 1 1 calc GR . . . .
H12C H 0.3125 0.1240 0.7005 0.131 Uiso 1 1 calc GR . . . .
C13 C 0.0123(5) 0.1067(3) 0.6233(3) 0.0743(10) Uani 1 1 d . . . . .
H13A H -0.0231 0.1295 0.6847 0.111 Uiso 1 1 calc GR . . . .
H13B H 0.0273 0.0325 0.6235 0.111 Uiso 1 1 calc GR . . . .
H13C H -0.0819 0.1349 0.5870 0.111 Uiso 1 1 calc GR . . . .
C14 C 0.2442(6) 0.1024(2) 0.4883(2) 0.0722(10) Uani 1 1 d . . . . .
H14A H 0.1534 0.1330 0.4510 0.108 Uiso 1 1 calc GR . . . .
H14B H 0.2490 0.0285 0.4910 0.108 Uiso 1 1 calc GR . . . .
H14C H 0.3630 0.1197 0.4626 0.108 Uiso 1 1 calc GR . . . .
C15 C 0.5027(4) 0.4851(2) 0.18868(18) 0.0499(7) Uani 1 1 d . . . . .
C16 C 0.5526(5) 0.3692(3) 0.1851(2) 0.0716(10) Uani 1 1 d . . . . .
H16A H 0.6490 0.3465 0.2216 0.107 Uiso 1 1 calc GR . . . .
H16B H 0.5945 0.3501 0.1231 0.107 Uiso 1 1 calc GR . . . .
H16C H 0.4459 0.3371 0.2083 0.107 Uiso 1 1 calc GR . . . .
C17 C 0.3417(5) 0.5192(3) 0.1361(2) 0.0749(10) Uani 1 1 d . . . . .
H17A H 0.2366 0.4884 0.1642 0.112 Uiso 1 1 calc GR . . . .
H17B H 0.3749 0.4976 0.0743 0.112 Uiso 1 1 calc GR . . . .
H17C H 0.3115 0.5932 0.1365 0.112 Uiso 1 1 calc GR . . . .
C18 C 0.6687(5) 0.5353(3) 0.1452(2) 0.0711(10) Uani 1 1 d . . . . .
H18A H 0.6372 0.6093 0.1463 0.107 Uiso 1 1 calc GR . . . .
H18B H 0.7031 0.5146 0.0832 0.107 Uiso 1 1 calc GR . . . .
H18C H 0.7704 0.5138 0.1787 0.107 Uiso 1 1 calc GR . . . .
B1 B 0.344(3) 0.8292(12) 0.0954(11) 0.0844(16) Uani 0.3333 1 d D U P A 1
N1T N 0.1480(5) 0.1194(3) 0.1109(2) 0.0892(10) Uani 1 1 d . . . . .
H1T H 0.1843 0.0454 0.1000 0.107 Uiso 1 1 calc R . . . .
C1T C 0.2963(6) 0.1497(4) 0.1494(3) 0.0896(12) Uani 1 1 d D U . . .
H1TC H 0.2645 0.2221 0.1643 0.107 Uiso 0.5 1 calc R . P B 2
H1TD H 0.4050 0.1437 0.1035 0.107 Uiso 0.5 1 calc R . P B 2
H1TA H 0.2677 0.2230 0.1613 0.107 Uiso 0.5 1 calc R . P C 1
H1TB H 0.4069 0.1399 0.1048 0.107 Uiso 0.5 1 calc R . P C 1
C2T C 0.335(4) 0.0934(18) 0.2337(11) 0.132(10) Uani 0.5 1 d D U P D 1
H2TA H 0.3959 0.1345 0.2682 0.198 Uiso 0.5 1 calc GR . P D 1
H2TB H 0.4143 0.0293 0.2194 0.198 Uiso 0.5 1 calc GR . P D 1
H2TC H 0.2218 0.0792 0.2690 0.198 Uiso 0.5 1 calc GR . P D 1
C3T C -0.0294(7) 0.1269(4) 0.1710(4) 0.1134(16) Uani 1 1 d D U . . .
H3TA H -0.0969 0.1963 0.1675 0.136 Uiso 0.5 1 calc R . P E 1
H3TB H -0.0100 0.1104 0.2338 0.136 Uiso 0.5 1 calc R . P E 1
H3TC H -0.0028 0.0949 0.2291 0.136 Uiso 0.5 1 calc R . P F 2
H3TD H -0.0688 0.1999 0.1815 0.136 Uiso 0.5 1 calc R . P F 2
C4T C -0.186(2) 0.0871(15) 0.151(2) 0.110(5) Uani 0.5 1 d D U P G 2
H4TA H -0.2239 0.1204 0.0957 0.164 Uiso 0.5 1 calc GR . P G 2
H4TB H -0.2853 0.1000 0.2001 0.164 Uiso 0.5 1 calc GR . P G 2
H4TC H -0.1556 0.0139 0.1424 0.164 Uiso 0.5 1 calc GR . P G 2
C5T C 0.1301(8) 0.1688(5) 0.0201(4) 0.1184(17) Uani 1 1 d D U . . .
H5TC H 0.0415 0.1353 -0.0052 0.142 Uiso 0.5 1 calc R . P H 2
H5TD H 0.2483 0.1506 -0.0176 0.142 Uiso 0.5 1 calc R . P H 2
H5TA H 0.0291 0.1460 -0.0044 0.142 Uiso 0.5 1 calc R . P I 1
H5TB H 0.2430 0.1501 -0.0215 0.142 Uiso 0.5 1 calc R . P I 1
C6T C 0.094(7) 0.2833(10) 0.031(2) 0.141(12) Uani 0.5 1 d D U P J 1
H6TA H 0.0378 0.3159 -0.0198 0.212 Uiso 0.5 1 calc GR . P J 1
H6TB H 0.2083 0.3086 0.0331 0.212 Uiso 0.5 1 calc GR . P J 1
H6TC H 0.0121 0.2989 0.0866 0.212 Uiso 0.5 1 calc GR . P J 1
C2T' C 0.344(3) 0.0896(18) 0.2318(12) 0.106(7) Uani 0.5 1 d D U P D 2
H2TD H 0.3298 0.0186 0.2261 0.159 Uiso 0.5 1 calc GR . P D 2
H2TE H 0.2633 0.1173 0.2843 0.159 Uiso 0.5 1 calc GR . P D 2
H2TF H 0.4696 0.0938 0.2387 0.159 Uiso 0.5 1 calc GR . P D 2
C4T' C -0.132(2) 0.0515(16) 0.139(2) 0.122(6) Uani 0.5 1 d D U P G 1
H4TD H -0.1584 0.0719 0.0781 0.183 Uiso 0.5 1 calc GR . P G 1
H4TE H -0.2458 0.0494 0.1787 0.183 Uiso 0.5 1 calc GR . P G 1
H4TF H -0.0590 -0.0158 0.1377 0.183 Uiso 0.5 1 calc GR . P G 1
C6T' C 0.076(6) 0.2818(10) 0.006(2) 0.132(9) Uani 0.5 1 d D U P J 2
H6TD H 0.0973 0.2998 -0.0579 0.197 Uiso 0.5 1 calc GR . P J 2
H6TE H 0.1484 0.3184 0.0382 0.197 Uiso 0.5 1 calc GR . P J 2
H6TF H -0.0526 0.3003 0.0287 0.197 Uiso 0.5 1 calc GR . P J 2
F4A F 0.387(3) 0.7556(15) 0.0324(13) 0.081(5) Uani 0.3333 1 d D U P K 3
F3A F 0.489(3) 0.8297(18) 0.1392(17) 0.128(6) Uani 0.3333 1 d D U P A 1
F1A F 0.326(2) 0.9184(13) 0.0454(11) 0.100(5) Uani 0.3333 1 d D U P A 1
F2A F 0.184(3) 0.8168(11) 0.1454(14) 0.117(5) Uani 0.3333 1 d D U P A 1
F1 F 0.264(3) 0.9180(10) 0.0723(10) 0.122(5) Uani 0.3333 1 d D U P L 2
F2 F 0.339(3) 0.7722(14) 0.0200(12) 0.099(5) Uani 0.3333 1 d D U P L 2
F5 F 0.194(2) 0.7791(10) 0.1551(12) 0.110(4) Uani 0.3333 1 d D U P L 2
F0AA F 0.485(3) 0.8042(17) 0.1439(16) 0.102(5) Uani 0.3333 1 d D U P L 2
B11 B 0.331(3) 0.8202(13) 0.1011(11) 0.0844(16) Uani 0.3333 1 d D U P L 2
B2 B 0.352(2) 0.8370(11) 0.0922(10) 0.0844(16) Uani 0.3333 1 d D U P K 3
F1AA F 0.1744(17) 0.8726(12) 0.1320(10) 0.133(4) Uani 0.3333 1 d D U P K 3
F2AA F 0.417(2) 0.8237(18) 0.1752(9) 0.138(5) Uani 0.3333 1 d D U P K 3
F4 F 0.4143(19) 0.9262(11) 0.0522(12) 0.113(5) Uani 0.3333 1 d D U P K 3
F3AA F 0.431(3) 0.7529(16) 0.0466(14) 0.111(5) Uani 0.3333 1 d . U P A 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 0.03999(18) 0.04031(18) 0.0388(2) -0.00955(13) -0.00209(13) -0.00592(13)
Cl1 0.0608(4) 0.0665(5) 0.0641(5) -0.0305(4) 0.0175(4) -0.0161(4)
Cl2 0.0700(5) 0.0446(4) 0.0661(5) -0.0146(3) 0.0009(4) -0.0156(3)
N1 0.0370(11) 0.0433(11) 0.0309(11) -0.0049(9) -0.0012(8) -0.0069(9)
N2 0.0381(11) 0.0363(11) 0.0366(11) -0.0013(9) -0.0062(9) -0.0060(8)
C1 0.0468(14) 0.0569(16) 0.0281(13) -0.0047(11) 0.0010(11) -0.0109(12)
C2 0.0500(15) 0.0506(15) 0.0322(14) 0.0043(11) 0.0004(11) -0.0138(12)
C3 0.0391(13) 0.0427(14) 0.0364(14) 0.0018(11) -0.0054(10) -0.0062(10)
C4 0.0430(13) 0.0391(13) 0.0325(13) -0.0034(10) -0.0002(10) -0.0056(10)
C5 0.0324(11) 0.0412(13) 0.0283(12) -0.0002(10) -0.0038(9) -0.0052(10)
C6 0.0332(12) 0.0384(12) 0.0326(13) 0.0015(10) -0.0053(10) -0.0047(9)
C7 0.0426(13) 0.0398(13) 0.0323(13) -0.0022(10) -0.0013(10) -0.0078(10)
C8 0.0400(13) 0.0483(14) 0.0335(13) 0.0016(11) -0.0061(10) -0.0108(11)
C9 0.0499(15) 0.0474(15) 0.0402(15) 0.0111(12) -0.0048(12) -0.0139(12)
C10 0.0498(15) 0.0362(13) 0.0462(16) 0.0023(11) -0.0042(12) -0.0089(11)
C11 0.0542(16) 0.0407(14) 0.0475(17) 0.0045(12) -0.0013(13) -0.0082(12)
C12 0.098(3) 0.057(2) 0.109(3) 0.013(2) -0.042(3) 0.0012(19)
C13 0.076(2) 0.0546(19) 0.089(3) -0.0006(18) 0.012(2) -0.0232(17)
C14 0.103(3) 0.0431(16) 0.066(2) -0.0090(15) 0.0109(19) -0.0144(17)
C15 0.0557(16) 0.0668(18) 0.0290(14) -0.0013(12) 0.0007(12) -0.0205(14)
C16 0.094(3) 0.074(2) 0.0437(18) -0.0173(16) 0.0117(17) -0.0170(19)
C17 0.075(2) 0.116(3) 0.0386(18) -0.0009(18) -0.0132(16) -0.025(2)
C18 0.070(2) 0.101(3) 0.0444(18) -0.0085(17) 0.0115(15) -0.036(2)
B1 0.112(3) 0.069(3) 0.061(3) 0.004(2) -0.002(2) 0.009(3)
N1T 0.093(2) 0.100(3) 0.075(2) 0.0020(19) -0.0080(19) -0.023(2)
C1T 0.077(3) 0.103(3) 0.085(3) -0.021(2) -0.001(2) -0.006(2)
C2T 0.18(2) 0.111(13) 0.080(8) -0.016(7) -0.003(8) 0.055(11)
C3T 0.102(3) 0.131(4) 0.101(4) -0.011(3) 0.008(3) -0.017(3)
C4T 0.071(7) 0.125(13) 0.127(12) 0.018(10) 0.001(8) -0.018(8)
C5T 0.117(4) 0.145(4) 0.096(4) 0.020(3) -0.014(3) -0.035(3)
C6T 0.22(3) 0.131(8) 0.069(11) 0.038(6) -0.017(14) -0.038(8)
C2T' 0.092(11) 0.138(15) 0.097(10) 0.004(9) -0.042(9) -0.024(10)
C4T' 0.088(11) 0.143(13) 0.138(14) 0.007(11) -0.024(13) -0.025(10)
C6T' 0.138(15) 0.145(8) 0.12(3) 0.050(7) -0.041(16) -0.046(7)
F4A 0.101(12) 0.077(6) 0.061(6) -0.002(5) -0.037(6) 0.022(6)
F3A 0.134(8) 0.142(14) 0.106(11) -0.012(9) -0.025(8) -0.003(8)
F1A 0.136(12) 0.086(6) 0.060(7) 0.010(5) 0.011(7) 0.015(6)
F2A 0.129(6) 0.073(9) 0.119(9) 0.030(8) 0.032(6) 0.023(7)
F1 0.220(15) 0.054(4) 0.077(9) 0.006(5) -0.032(9) 0.031(6)
F2 0.132(12) 0.084(7) 0.076(6) -0.014(5) -0.029(5) 0.025(6)
F5 0.131(7) 0.084(9) 0.094(7) 0.016(6) 0.018(5) 0.004(7)
F0AA 0.127(7) 0.098(8) 0.079(8) 0.045(7) -0.022(6) -0.019(6)
B11 0.112(3) 0.069(3) 0.061(3) 0.004(2) -0.002(2) 0.009(3)
B2 0.112(3) 0.069(3) 0.061(3) 0.004(2) -0.002(2) 0.009(3)
F1AA 0.127(6) 0.137(10) 0.118(9) -0.015(8) 0.018(5) 0.009(6)
F2AA 0.198(12) 0.136(10) 0.088(7) 0.026(7) -0.049(7) -0.033(10)
F4 0.138(10) 0.073(5) 0.113(8) 0.005(4) 0.008(7) 0.009(6)
F3AA 0.117(11) 0.092(6) 0.112(11) -0.011(7) 0.009(7) 0.005(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
Cu1 Cl1 2.2181(8) . ?
Cu1 Cl2 2.2232(8) . ?
Cu1 N1 2.018(2) . ?
Cu1 N2 2.003(2) . ?
N1 C1 1.350(3) . ?
N1 C5 1.342(3) . ?
N2 C6 1.349(3) . ?
N2 C10 1.346(3) . ?
C1 H1 0.9400 . ?
C1 C2 1.366(4) . ?
C2 H2 0.9400 . ?
C2 C3 1.389(4) . ?
C3 C4 1.398(3) . ?
C3 C11 1.526(4) . ?
C4 H4 0.9400 . ?
C4 C5 1.378(3) . ?
C5 C6 1.485(3) . ?
C6 C7 1.374(3) . ?
C7 H7 0.9400 . ?
C7 C8 1.402(4) . ?
C8 C9 1.393(4) . ?
C8 C15 1.524(4) . ?
C9 H9 0.9400 . ?
C9 C10 1.372(4) . ?
C10 H10 0.9400 . ?
C11 C12 1.530(5) . ?
C11 C13 1.528(4) . ?
C11 C14 1.531(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 C16 1.522(5) . ?
C15 C17 1.532(4) . ?
C15 C18 1.539(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
B1 F3A 1.349(14) . ?
B1 F1A 1.361(14) . ?
B1 F2A 1.343(14) . ?
B1 F3AA 1.31(2) . ?
N1T H1T 0.9900 . ?
N1T C1T 1.438(5) . ?
N1T C3T 1.482(6) . ?
N1T C5T 1.491(6) . ?
C1T H1TC 0.9800 . ?
C1T H1TD 0.9800 . ?
C1T H1TA 0.9800 . ?
C1T H1TB 0.9800 . ?
C1T C2T 1.475(12) . ?
C1T C2T' 1.489(11) . ?
C2T H2TA 0.9700 . ?
C2T H2TB 0.9700 . ?
C2T H2TC 0.9700 . ?
C3T H3TA 0.9800 . ?
C3T H3TB 0.9800 . ?
C3T H3TC 0.9800 . ?
C3T H3TD 0.9800 . ?
C3T C4T 1.433(12) . ?
C3T C4T' 1.487(12) . ?
C4T H4TA 0.9700 . ?
C4T H4TB 0.9700 . ?
C4T H4TC 0.9700 . ?
C5T H5TC 0.9800 . ?
C5T H5TD 0.9800 . ?
C5T H5TA 0.9800 . ?
C5T H5TB 0.9800 . ?
C5T C6T 1.508(14) . ?
C5T C6T' 1.497(14) . ?
C6T H6TA 0.9700 . ?
C6T H6TB 0.9700 . ?
C6T H6TC 0.9700 . ?
C2T' H2TD 0.9700 . ?
C2T' H2TE 0.9700 . ?
C2T' H2TF 0.9700 . ?
C4T' H4TD 0.9700 . ?
C4T' H4TE 0.9700 . ?
C4T' H4TF 0.9700 . ?
C6T' H6TD 0.9700 . ?
C6T' H6TE 0.9700 . ?
C6T' H6TF 0.9700 . ?
F4A B2 1.407(14) . ?
F1 B11 1.382(14) . ?
F2 B11 1.391(14) . ?
F5 B11 1.373(14) . ?
F0AA B11 1.379(13) . ?
B2 F1AA 1.394(13) . ?
B2 F2AA 1.393(14) . ?
B2 F4 1.404(13) . ?
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
Cl1 Cu1 Cl2 94.55(3) . . ?
N1 Cu1 Cl1 93.91(6) . . ?
N1 Cu1 Cl2 163.25(6) . . ?
N2 Cu1 Cl1 162.33(6) . . ?
N2 Cu1 Cl2 95.63(6) . . ?
N2 Cu1 N1 80.14(8) . . ?
C1 N1 Cu1 126.86(17) . . ?
C5 N1 Cu1 115.47(16) . . ?
C5 N1 C1 117.6(2) . . ?
C6 N2 Cu1 115.88(16) . . ?
C10 N2 Cu1 126.60(17) . . ?
C10 N2 C6 117.4(2) . . ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.7(2) . . ?
C2 C1 H1 118.7 . . ?
C1 C2 H2 119.5 . . ?
C1 C2 C3 120.9(2) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 C4 115.8(2) . . ?
C2 C3 C11 121.8(2) . . ?
C4 C3 C11 122.3(2) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.8(2) . . ?
C5 C4 H4 119.6 . . ?
N1 C5 C4 122.2(2) . . ?
N1 C5 C6 114.3(2) . . ?
C4 C5 C6 123.5(2) . . ?
N2 C6 C5 114.1(2) . . ?
N2 C6 C7 122.4(2) . . ?
C7 C6 C5 123.5(2) . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C15 121.8(2) . . ?
C9 C8 C7 115.9(2) . . ?
C9 C8 C15 122.1(2) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.6(2) . . ?
C10 C9 H9 119.7 . . ?
N2 C10 C9 122.9(2) . . ?
N2 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
C3 C11 C12 107.6(3) . . ?
C3 C11 C13 110.7(2) . . ?
C3 C11 C14 112.2(2) . . ?
C12 C11 C14 108.5(3) . . ?
C13 C11 C12 110.7(3) . . ?
C13 C11 C14 107.1(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C15 C17 107.1(2) . . ?
C8 C15 C18 110.2(2) . . ?
C16 C15 C8 111.9(2) . . ?
C16 C15 C17 109.0(3) . . ?
C16 C15 C18 109.0(3) . . ?
C17 C15 C18 109.6(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
F3A B1 F1A 106.5(15) . . ?
F2A B1 F3A 117.6(16) . . ?
F2A B1 F1A 110.3(13) . . ?
F3AA B1 F3A 91.0(18) . . ?
F3AA B1 F1A 111.4(18) . . ?
F3AA B1 F2A 118.2(18) . . ?
C1T N1T H1T 105.2 . . ?
C1T N1T C3T 115.5(4) . . ?
C1T N1T C5T 112.2(4) . . ?
C3T N1T H1T 105.2 . . ?
C3T N1T C5T 112.5(4) . . ?
C5T N1T H1T 105.2 . . ?
N1T C1T H1TC 108.5 . . ?
N1T C1T H1TD 108.5 . . ?
N1T C1T H1TA 108.6 . . ?
N1T C1T H1TB 108.6 . . ?
N1T C1T C2T 114.5(12) . . ?
N1T C1T C2T' 115.1(9) . . ?
H1TC C1T H1TD 107.5 . . ?
H1TA C1T H1TB 107.6 . . ?
C2T C1T H1TA 108.6 . . ?
C2T C1T H1TB 108.6 . . ?
C2T' C1T H1TC 108.5 . . ?
C2T' C1T H1TD 108.5 . . ?
C1T C2T H2TA 109.5 . . ?
C1T C2T H2TB 109.5 . . ?
C1T C2T H2TC 109.5 . . ?
H2TA C2T H2TB 109.5 . . ?
H2TA C2T H2TC 109.5 . . ?
H2TB C2T H2TC 109.5 . . ?
N1T C3T H3TA 110.5 . . ?
N1T C3T H3TB 110.5 . . ?
N1T C3T H3TC 106.3 . . ?
N1T C3T H3TD 106.3 . . ?
N1T C3T C4T' 106.1(11) . . ?
H3TA C3T H3TB 108.7 . . ?
H3TC C3T H3TD 106.4 . . ?
C4T C3T N1T 124.2(11) . . ?
C4T C3T H3TC 106.3 . . ?
C4T C3T H3TD 106.3 . . ?
C4T' C3T H3TA 110.5 . . ?
C4T' C3T H3TB 110.5 . . ?
C3T C4T H4TA 109.5 . . ?
C3T C4T H4TB 109.5 . . ?
C3T C4T H4TC 109.5 . . ?
H4TA C4T H4TB 109.5 . . ?
H4TA C4T H4TC 109.5 . . ?
H4TB C4T H4TC 109.5 . . ?
N1T C5T H5TC 106.6 . . ?
N1T C5T H5TD 106.6 . . ?
N1T C5T H5TA 110.2 . . ?
N1T C5T H5TB 110.2 . . ?
N1T C5T C6T 107.8(14) . . ?
N1T C5T C6T' 122.8(14) . . ?
H5TC C5T H5TD 106.6 . . ?
H5TA C5T H5TB 108.5 . . ?
C6T C5T H5TA 110.2 . . ?
C6T C5T H5TB 110.2 . . ?
C6T' C5T H5TC 106.6 . . ?
C6T' C5T H5TD 106.6 . . ?
C5T C6T H6TA 109.5 . . ?
C5T C6T H6TB 109.5 . . ?
C5T C6T H6TC 109.5 . . ?
H6TA C6T H6TB 109.5 . . ?
H6TA C6T H6TC 109.5 . . ?
H6TB C6T H6TC 109.5 . . ?
C1T C2T' H2TD 109.5 . . ?
C1T C2T' H2TE 109.5 . . ?
C1T C2T' H2TF 109.5 . . ?
H2TD C2T' H2TE 109.5 . . ?
H2TD C2T' H2TF 109.5 . . ?
H2TE C2T' H2TF 109.5 . . ?
C3T C4T' H4TD 109.5 . . ?
C3T C4T' H4TE 109.5 . . ?
C3T C4T' H4TF 109.5 . . ?
H4TD C4T' H4TE 109.5 . . ?
H4TD C4T' H4TF 109.5 . . ?
H4TE C4T' H4TF 109.5 . . ?
C5T C6T' H6TD 109.5 . . ?
C5T C6T' H6TE 109.5 . . ?
C5T C6T' H6TF 109.5 . . ?
H6TD C6T' H6TE 109.5 . . ?
H6TD C6T' H6TF 109.5 . . ?
H6TE C6T' H6TF 109.5 . . ?
F1 B11 F2 97.5(12) . . ?
F5 B11 F1 109.0(13) . . ?
F5 B11 F2 102.2(15) . . ?
F5 B11 F0AA 108.4(13) . . ?
F0AA B11 F1 120.1(15) . . ?
F0AA B11 F2 118.0(18) . . ?
F1AA B2 F4A 121.1(17) . . ?
F1AA B2 F4 103.1(13) . . ?
F2AA B2 F4A 119.5(16) . . ?
F2AA B2 F1AA 92.6(13) . . ?
F2AA B2 F4 105.5(16) . . ?
F4 B2 F4A 112.1(17) . . ?
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 N1 C1 C2 -174.9(2) . . . . ?
Cu1 N1 C5 C4 176.03(19) . . . . ?
Cu1 N1 C5 C6 -4.3(3) . . . . ?
Cu1 N2 C6 C5 -1.1(3) . . . . ?
Cu1 N2 C6 C7 177.15(19) . . . . ?
Cu1 N2 C10 C9 -174.7(2) . . . . ?
N1 C1 C2 C3 -0.4(4) . . . . ?
N1 C5 C6 N2 3.5(3) . . . . ?
N1 C5 C6 C7 -174.7(2) . . . . ?
N2 C6 C7 C8 -2.6(4) . . . . ?
C1 N1 C5 C4 -0.4(4) . . . . ?
C1 N1 C5 C6 179.3(2) . . . . ?
C1 C2 C3 C4 -0.8(4) . . . . ?
C1 C2 C3 C11 176.3(3) . . . . ?
C2 C3 C4 C5 1.4(4) . . . . ?
C2 C3 C11 C12 -74.4(3) . . . . ?
C2 C3 C11 C13 46.7(4) . . . . ?
C2 C3 C11 C14 166.3(3) . . . . ?
C3 C4 C5 N1 -0.9(4) . . . . ?
C3 C4 C5 C6 179.4(2) . . . . ?
C4 C3 C11 C12 102.6(3) . . . . ?
C4 C3 C11 C13 -136.4(3) . . . . ?
C4 C3 C11 C14 -16.8(4) . . . . ?
C4 C5 C6 N2 -176.8(2) . . . . ?
C4 C5 C6 C7 5.0(4) . . . . ?
C5 N1 C1 C2 1.0(4) . . . . ?
C5 C6 C7 C8 175.5(2) . . . . ?
C6 N2 C10 C9 1.7(4) . . . . ?
C6 C7 C8 C9 2.6(4) . . . . ?
C6 C7 C8 C15 -172.8(2) . . . . ?
C7 C8 C9 C10 -0.6(4) . . . . ?
C7 C8 C15 C16 -18.6(4) . . . . ?
C7 C8 C15 C17 100.7(3) . . . . ?
C7 C8 C15 C18 -140.1(3) . . . . ?
C8 C9 C10 N2 -1.6(4) . . . . ?
C9 C8 C15 C16 166.3(3) . . . . ?
C9 C8 C15 C17 -74.4(3) . . . . ?
C9 C8 C15 C18 44.8(4) . . . . ?
C10 N2 C6 C5 -177.9(2) . . . . ?
C10 N2 C6 C7 0.4(4) . . . . ?
C11 C3 C4 C5 -175.7(2) . . . . ?
C15 C8 C9 C10 174.8(3) . . . . ?
C1T N1T C3T C4T -170.8(13) . . . . ?
C1T N1T C3T C4T' -154.6(13) . . . . ?
C1T N1T C5T C6T -60(2) . . . . ?
C1T N1T C5T C6T' -66(2) . . . . ?
C3T N1T C1T C2T 56.8(11) . . . . ?
C3T N1T C1T C2T' 59.9(13) . . . . ?
C3T N1T C5T C6T 72(2) . . . . ?
C3T N1T C5T C6T' 66(2) . . . . ?
C5T N1T C1T C2T -172.6(11) . . . . ?
C5T N1T C1T C2T' -169.4(12) . . . . ?
C5T N1T C3T C4T 58.7(14) . . . . ?
C5T N1T C3T C4T' 74.8(13) . . . . ?
_shelx_res_file
;
crystal2_cu_a.res created by SHELXL-2014/7
TITL crystal2_Cu_a.res in P-1
REM Old TITL crystal2_Cu in P-1
REM SHELXT solution in P-1
REM R1 0.204, Rweak 0.020, Alpha 0.056, Orientation as input
REM Formula found by SHELXT: C30 N2 O2 Cu
CELL 0.71073 7.4731 13.2115 14.9811 86.824 81.552 81.251
ZERR 2 0.0005 0.001 0.0011 0.004 0.004 0.004
LATT 1
SFAC C H B Cl Cu F N
UNIT 48 80 2 4 2 8 6
SADI C2T C1T C2T' C1T
SADI C4T' C3T C4T C3T
SADI C6T C5T C6T' C5T
SADI 0.04 F4A F3A F4A F1A F3A F1A F3A F2A F1A F2A
SADI B1 F4A B1 F3A B1 F1A B1 F2A
SADI 0.04 F1 F2 F1 F5 F1 F0AA F2 F5 F5 F0AA
SADI B11 F1 B11 F2 B11 F5 B11 F0AA
SADI B2 F2AA B2 F4 B2 F4A B2 F1AA
RIGU C5T C6T'
RIGU C5T C6T
RIGU C1T C2T
RIGU C2T' C1T
RIGU C3T C4T
RIGU C3T C4T'
RIGU B1 F3AA F2A F3A F1A B2 F4A F2AA F1AA F4 B11 F1 F5 F2 F0AA
EADP B2 B1 B11
L.S. 10
PLAN 30
TEMP -51.16
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 50.00
OMIT 0 0 1
OMIT 0 1 0
OMIT 0 -1 1
OMIT 1 0 0
OMIT 0 1 1
OMIT -1 1 0
OMIT 0 2 1
REM
REM
REM
WGHT 0.056900 0.632200
FVAR 0.55188
CU1 5 0.177340 0.624436 0.584024 11.00000 0.03999 0.04031 =
0.03878 -0.00955 -0.00209 -0.00592
CL1 4 -0.032085 0.657374 0.703949 11.00000 0.06084 0.06647 =
0.06408 -0.03050 0.01748 -0.01607
CL2 4 0.281345 0.773482 0.583365 11.00000 0.06997 0.04460 =
0.06609 -0.01461 0.00092 -0.01560
N1 7 0.159147 0.473351 0.589034 11.00000 0.03698 0.04327 =
0.03095 -0.00490 -0.00119 -0.00693
N2 7 0.298616 0.587701 0.459416 11.00000 0.03810 0.03626 =
0.03663 -0.00129 -0.00623 -0.00597
C1 1 0.086235 0.418461 0.660149 11.00000 0.04680 0.05693 =
0.02808 -0.00469 0.00100 -0.01090
AFIX 43
H1 2 0.028966 0.453100 0.712248 11.00000 -1.20000
AFIX 0
C2 1 0.092251 0.314629 0.659521 11.00000 0.04997 0.05064 =
0.03223 0.00430 0.00036 -0.01384
AFIX 43
H2 2 0.040170 0.279727 0.710891 11.00000 -1.20000
AFIX 0
C3 1 0.174252 0.259927 0.584033 11.00000 0.03905 0.04274 =
0.03639 0.00179 -0.00536 -0.00619
C4 1 0.245996 0.317938 0.510245 11.00000 0.04295 0.03910 =
0.03251 -0.00340 -0.00025 -0.00555
AFIX 43
H4 2 0.300649 0.285240 0.456776 11.00000 -1.20000
AFIX 0
C5 1 0.237606 0.422429 0.514906 11.00000 0.03242 0.04121 =
0.02829 -0.00020 -0.00383 -0.00520
C6 1 0.312569 0.488264 0.439362 11.00000 0.03321 0.03838 =
0.03258 0.00154 -0.00534 -0.00472
C7 1 0.385324 0.452581 0.355393 11.00000 0.04256 0.03982 =
0.03230 -0.00222 -0.00125 -0.00780
AFIX 43
H7 2 0.397109 0.382213 0.344965 11.00000 -1.20000
AFIX 0
C8 1 0.442184 0.520157 0.285080 11.00000 0.03996 0.04828 =
0.03354 0.00163 -0.00615 -0.01078
C9 1 0.426923 0.622400 0.307324 11.00000 0.04992 0.04738 =
0.04022 0.01114 -0.00484 -0.01387
AFIX 43
H9 2 0.464014 0.671082 0.263037 11.00000 -1.20000
AFIX 0
C10 1 0.358271 0.652680 0.393256 11.00000 0.04982 0.03622 =
0.04619 0.00234 -0.00423 -0.00892
AFIX 43
H10 2 0.352645 0.721902 0.406520 11.00000 -1.20000
AFIX 0
C11 1 0.192697 0.143291 0.583702 11.00000 0.05425 0.04070 =
0.04752 0.00449 -0.00135 -0.00820
C12 1 0.344302 0.099660 0.639538 11.00000 0.09805 0.05701 =
0.10876 0.01297 -0.04167 0.00123
AFIX 137
H12A 2 0.458434 0.121872 0.612276 11.00000 -1.50000
H12B 2 0.358028 0.025408 0.641189 11.00000 -1.50000
H12C 2 0.312538 0.124045 0.700539 11.00000 -1.50000
AFIX 0
C13 1 0.012267 0.106692 0.623341 11.00000 0.07606 0.05461 =
0.08901 -0.00062 0.01211 -0.02316
AFIX 137
H13A 2 -0.023109 0.129529 0.684698 11.00000 -1.50000
H13B 2 0.027292 0.032454 0.623501 11.00000 -1.50000
H13C 2 -0.081896 0.134866 0.586982 11.00000 -1.50000
AFIX 0
C14 1 0.244247 0.102381 0.488320 11.00000 0.10265 0.04305 =
0.06607 -0.00900 0.01092 -0.01442
AFIX 137
H14A 2 0.153391 0.132983 0.450955 11.00000 -1.50000
H14B 2 0.248973 0.028511 0.490983 11.00000 -1.50000
H14C 2 0.363046 0.119723 0.462577 11.00000 -1.50000
AFIX 0
C15 1 0.502741 0.485063 0.188678 11.00000 0.05566 0.06676 =
0.02897 -0.00130 0.00065 -0.02051
C16 1 0.552554 0.369178 0.185092 11.00000 0.09377 0.07404 =
0.04373 -0.01735 0.01169 -0.01698
AFIX 137
H16A 2 0.649037 0.346478 0.221602 11.00000 -1.50000
H16B 2 0.594505 0.350073 0.123098 11.00000 -1.50000
H16C 2 0.445875 0.337107 0.208290 11.00000 -1.50000
AFIX 0
C17 1 0.341675 0.519194 0.136077 11.00000 0.07492 0.11608 =
0.03862 -0.00086 -0.01317 -0.02544
AFIX 137
H17A 2 0.236590 0.488370 0.164174 11.00000 -1.50000
H17B 2 0.374943 0.497587 0.074263 11.00000 -1.50000
H17C 2 0.311518 0.593236 0.136490 11.00000 -1.50000
AFIX 0
C18 1 0.668677 0.535325 0.145212 11.00000 0.07038 0.10066 =
0.04437 -0.00850 0.01149 -0.03589
AFIX 137
H18A 2 0.637177 0.609276 0.146305 11.00000 -1.50000
H18B 2 0.703081 0.514551 0.083207 11.00000 -1.50000
H18C 2 0.770369 0.513830 0.178725 11.00000 -1.50000
AFIX 0
PART 1
B1 3 0.343923 0.829153 0.095411 10.33333 0.11202 0.06910 =
0.06136 0.00384 -0.00201 0.00852
PART 0
N1T 7 0.148041 0.119414 0.110937 11.00000 0.09295 0.10036 =
0.07525 0.00198 -0.00798 -0.02276
AFIX 13
H1T 2 0.184319 0.045429 0.099951 11.00000 -1.20000
AFIX 0
C1T 1 0.296331 0.149741 0.149377 11.00000 0.07708 0.10347 =
0.08490 -0.02126 -0.00132 -0.00588
PART 2
AFIX 23
H1TC 2 0.264493 0.222130 0.164346 10.50000 -1.20000
H1TD 2 0.404980 0.143724 0.103500 10.50000 -1.20000
AFIX 23
PART 0
PART 1
H1TA 2 0.267722 0.223034 0.161332 10.50000 -1.20000
H1TB 2 0.406920 0.139938 0.104813 10.50000 -1.20000
AFIX 0
C2T 1 0.335434 0.093370 0.233713 10.50000 0.17845 0.11055 =
0.07983 -0.01617 -0.00322 0.05451
AFIX 137
H2TA 2 0.395917 0.134464 0.268231 10.50000 -1.50000
H2TB 2 0.414319 0.029316 0.219387 10.50000 -1.50000
H2TC 2 0.221790 0.079246 0.269000 10.50000 -1.50000
AFIX 0
PART 0
C3T 1 -0.029359 0.126863 0.171005 11.00000 0.10237 0.13067 =
0.10143 -0.01118 0.00765 -0.01730
PART 1
AFIX 23
H3TA 2 -0.096891 0.196293 0.167530 10.50000 -1.20000
H3TB 2 -0.009950 0.110359 0.233768 10.50000 -1.20000
AFIX 23
PART 0
PART 2
H3TC 2 -0.002786 0.094914 0.229129 10.50000 -1.20000
H3TD 2 -0.068767 0.199946 0.181496 10.50000 -1.20000
AFIX 0
C4T 1 -0.186196 0.087064 0.150675 10.50000 0.07065 0.12488 =
0.12737 0.01824 0.00145 -0.01798
AFIX 137
H4TA 2 -0.223854 0.120444 0.095747 10.50000 -1.50000
H4TB 2 -0.285336 0.099953 0.200118 10.50000 -1.50000
H4TC 2 -0.155572 0.013853 0.142398 10.50000 -1.50000
AFIX 0
PART 0
C5T 1 0.130147 0.168814 0.020109 11.00000 0.11657 0.14503 =
0.09554 0.01988 -0.01397 -0.03492
PART 2
AFIX 23
H5TC 2 0.041541 0.135275 -0.005214 10.50000 -1.20000
H5TD 2 0.248272 0.150569 -0.017605 10.50000 -1.20000
AFIX 23
PART 0
PART 1
H5TA 2 0.029053 0.145975 -0.004445 10.50000 -1.20000
H5TB 2 0.242974 0.150109 -0.021538 10.50000 -1.20000
AFIX 0
C6T 1 0.093838 0.283256 0.030966 10.50000 0.22134 0.13089 =
0.06894 0.03784 -0.01699 -0.03753
AFIX 137
H6TA 2 0.037803 0.315862 -0.019766 10.50000 -1.50000
H6TB 2 0.208259 0.308638 0.033065 10.50000 -1.50000
H6TC 2 0.012104 0.298857 0.086579 10.50000 -1.50000
AFIX 0
PART 0
PART 2
C2T' 1 0.343915 0.089602 0.231800 10.50000 0.09228 0.13785 =
0.09733 0.00449 -0.04181 -0.02378
AFIX 137
H2TD 2 0.329842 0.018552 0.226126 10.50000 -1.50000
H2TE 2 0.263295 0.117265 0.284305 10.50000 -1.50000
H2TF 2 0.469609 0.093809 0.238666 10.50000 -1.50000
AFIX 0
PART 0
PART 1
C4T' 1 -0.132090 0.051546 0.138537 10.50000 0.08807 0.14347 =
0.13770 0.00689 -0.02413 -0.02502
AFIX 137
H4TD 2 -0.158387 0.071920 0.078068 10.50000 -1.50000
H4TE 2 -0.245847 0.049378 0.178711 10.50000 -1.50000
H4TF 2 -0.059041 -0.015784 0.137655 10.50000 -1.50000
AFIX 0
PART 0
PART 2
C6T' 1 0.076059 0.281779 0.006052 10.50000 0.13798 0.14483 =
0.12047 0.04980 -0.04050 -0.04585
AFIX 137
H6TD 2 0.097280 0.299790 -0.057888 10.50000 -1.50000
H6TE 2 0.148419 0.318412 0.038219 10.50000 -1.50000
H6TF 2 -0.052562 0.300319 0.028718 10.50000 -1.50000
AFIX 0
PART 0
PART 3
F4A 6 0.387040 0.755617 0.032357 10.33333 0.10101 0.07731 =
0.06128 -0.00244 -0.03698 0.02203
PART 0
PART 1
F3A 6 0.489176 0.829668 0.139192 10.33333 0.13412 0.14178 =
0.10648 -0.01155 -0.02498 -0.00268
F1A 6 0.326383 0.918378 0.045381 10.33333 0.13616 0.08600 =
0.06003 0.00961 0.01147 0.01462
F2A 6 0.183658 0.816769 0.145352 10.33333 0.12895 0.07307 =
0.11916 0.02959 0.03202 0.02267
PART 0
PART 2
F1 6 0.264148 0.917968 0.072338 10.33333 0.22000 0.05432 =
0.07682 0.00616 -0.03160 0.03082
F2 6 0.339180 0.772205 0.019999 10.33333 0.13169 0.08354 =
0.07553 -0.01362 -0.02928 0.02482
F5 6 0.193765 0.779133 0.155134 10.33333 0.13141 0.08442 =
0.09413 0.01585 0.01847 0.00355
F0AA 6 0.484984 0.804186 0.143922 10.33333 0.12700 0.09756 =
0.07906 0.04523 -0.02194 -0.01925
B11 3 0.331477 0.820244 0.101070 10.33333 0.11202 0.06910 =
0.06136 0.00384 -0.00201 0.00852
PART 0
PART 3
B2 3 0.351827 0.836990 0.092233 10.33333 0.11202 0.06910 =
0.06136 0.00384 -0.00201 0.00852
F1AA 6 0.174439 0.872641 0.131968 10.33333 0.12672 0.13740 =
0.11778 -0.01536 0.01762 0.00854
F2AA 6 0.416835 0.823653 0.175228 10.33333 0.19793 0.13563 =
0.08816 0.02645 -0.04948 -0.03308
F4 6 0.414286 0.926167 0.052249 10.33333 0.13789 0.07261 =
0.11284 0.00488 0.00797 0.00854
PART 0
PART 1
F3AA 6 0.431415 0.752934 0.046640 10.33333 0.11663 0.09208 =
0.11199 -0.01094 0.00931 0.00468
HKLF 4
REM crystal2_Cu_a.res in P-1
REM R1 = 0.0424 for 4822 Fo > 4sig(Fo) and 0.0619 for all 6317 data
REM 433 parameters refined using 149 restraints
END
WGHT 0.0569 0.6322
REM Highest difference peak 0.862, deepest hole -0.438, 1-sigma level 0.057
Q1 1 0.0846 0.1839 0.1413 11.00000 0.05 0.86
Q2 1 0.0026 0.2246 0.0570 11.00000 0.05 0.34
Q3 1 0.2979 0.4542 0.4768 11.00000 0.05 0.30
Q4 1 -0.0120 0.0977 0.1009 11.00000 0.05 0.27
Q5 1 0.4128 0.4823 0.3187 11.00000 0.05 0.27
Q6 1 0.1315 0.0802 0.2195 11.00000 0.05 0.25
Q7 1 0.0676 0.6415 0.7253 11.00000 0.05 0.23
Q8 1 0.1428 0.4569 0.6177 11.00000 0.05 0.21
Q9 1 0.0510 0.3487 0.0146 11.00000 0.05 0.21
Q10 1 0.2161 0.3720 0.5191 11.00000 0.05 0.20
Q11 1 0.5032 0.7574 0.1001 11.00000 0.05 0.20
Q12 1 0.1042 0.0200 0.2246 11.00000 0.05 0.20
Q13 1 0.2623 0.4855 0.4388 11.00000 0.05 0.20
Q14 1 0.2947 0.8662 0.2003 11.00000 0.05 0.20
Q15 1 0.2534 0.8839 0.1835 11.00000 0.05 0.19
Q16 1 0.2052 0.2849 0.5430 11.00000 0.05 0.19
Q17 1 0.1235 0.1220 0.5992 11.00000 0.05 0.19
Q18 1 0.3990 0.9002 0.1211 11.00000 0.05 0.19
Q19 1 0.2921 0.8004 0.1793 11.00000 0.05 0.18
Q20 1 0.4067 0.5670 0.3043 11.00000 0.05 0.18
Q21 1 0.5270 0.3067 0.2263 11.00000 0.05 0.18
Q22 1 0.3015 0.6210 0.4255 11.00000 0.05 0.18
Q23 1 0.5613 0.4913 0.1704 11.00000 0.05 0.17
Q24 1 0.4086 0.4616 0.4060 11.00000 0.05 0.17
Q25 1 0.2419 0.9231 0.0428 11.00000 0.05 0.17
Q26 1 0.3818 0.6788 0.2567 11.00000 0.05 0.17
Q27 1 0.0816 0.0899 0.6766 11.00000 0.05 0.17
Q28 1 -0.1193 -0.0394 0.2464 11.00000 0.05 0.17
Q29 1 0.2794 0.5344 0.5846 11.00000 0.05 0.17
Q30 1 0.7860 0.4774 0.1744 11.00000 0.05 0.16
;
_shelx_res_checksum 94992
_shelx_SHELXL_version_number 2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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_bishwnath_10sept216_a
_audit_block_doi 10.5517/ccdc.csd.cc2145p2
_database_code_depnum_ccdc_archive 'CCDC 1880853'
_audit_update_record
;
2019-01-24 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;
_audit_creation_date 2018-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C18 H24 Cu0.5 N2, B0.5 F2'
_chemical_formula_sum 'C18 H24 B0.50 Cu0.50 F2 N2'
_chemical_formula_weight 343.57
_chemical_absolute_configuration ?
_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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
_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 trigonal
_space_group_IT_number 154
_space_group_name_H-M_alt 'P 32 2 1'
_space_group_name_Hall 'P 32 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
_cell_length_a 11.2232(15)
_cell_length_b 11.2232(15)
_cell_length_c 27.924(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 3046.0(9)
_cell_formula_units_Z 6
_cell_measurement_reflns_used 6850
_cell_measurement_temperature 150.0
_cell_measurement_theta_max 23.224
_cell_measurement_theta_min 2.188
_shelx_estimated_absorpt_T_max 0.974
_shelx_estimated_absorpt_T_min 0.833
_exptl_absorpt_coefficient_mu 0.583
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6189
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1056 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.8301. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'dark red'
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.124
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1086
_exptl_crystal_size_max 0.326
_exptl_crystal_size_mid 0.135
_exptl_crystal_size_min 0.045
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0425
_diffrn_reflns_av_unetI/netI 0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 19079
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 24.987
_diffrn_reflns_theta_max 24.987
_diffrn_reflns_theta_min 2.188
_diffrn_ambient_temperature 150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.722
_reflns_Friedel_fraction_full 0.998
_reflns_Friedel_fraction_max 0.998
_reflns_number_gt 3228
_reflns_number_total 3579
_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 v8.34A (Bruker, 2013)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max 1.060
_refine_diff_density_min -1.147
_refine_diff_density_rms 0.134
_refine_ls_abs_structure_details
;
Flack x determined using 1209 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.036(8)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.097
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 218
_refine_ls_number_reflns 3579
_refine_ls_number_restraints 19
_refine_ls_R_factor_all 0.0857
_refine_ls_R_factor_gt 0.0787
_refine_ls_restrained_S_all 1.105
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1594P)^2^+2.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2163
_refine_ls_wR_factor_ref 0.2253
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
F6-B0AA = F1AA-B0AA = F4AA-B0AA = F2AA-B0AA = F1-B0AA = F2-B0AA = F3AA-B0AA
1.419 with sigma of 0.02
F4AA-F6
2.32 with sigma of 0.02
F6-F3AA
2.32 with sigma of 0.02
F3AA-F4AA
2.32 with sigma of 0.02
F2AA-F1AA
2.32 with sigma of 0.02
F1AA-F2
2.32 with sigma of 0.02
F2-F2AA
2.32 with sigma of 0.02
F1-F4AA
2.32 with sigma of 0.02
F1-F6
2.32 with sigma of 0.02
F1-F3AA
2.32 with sigma of 0.02
F1-F1AA
2.32 with sigma of 0.02
F1-F2AA
2.32 with sigma of 0.02
F1-F2
2.32 with sigma of 0.02
3. Others
Fixed Sof: F1(0.5) F2(0.25) B0AA(0.5) F1AA(0.25) F2AA(0.25) F3AA(0.25)
F4AA(0.25) F6(0.25)
Fixed Uiso: F2(0.04883) F1AA(0.04883) F2AA(0.04883) F3AA(0.04883)
F4AA(0.04883) F6(0.04883)
4.a Aromatic/amide H refined with riding coordinates:
C006(H006), C009(H009), C00A(H00A), C00B(H00B), C00C(H00C), C00D(H00D)
4.b Idealised Me refined as rotating group:
C00F(H00E,H00F,H00G), C00G(H00H,H00I,H00J), C00H(H00K,H00L,H00M), C00J(H00N,
H00O,H00P), C00K(H00Q,H00R,H00S), C00L(H00T,H00U,H00V)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_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
Cu01 Cu 0.50213(10) 0.000000 0.666667 0.0297(4) Uani 1 2 d S T P . .
N002 N 0.6369(6) 0.0971(6) 0.61362(18) 0.0269(13) Uani 1 1 d . . . . .
N003 N 0.4797(7) 0.1678(7) 0.6603(2) 0.0331(14) Uani 1 1 d . . . . .
C004 C 0.5495(7) 0.2504(7) 0.6233(2) 0.0258(14) Uani 1 1 d . . . . .
C005 C 0.6483(7) 0.2163(7) 0.6002(2) 0.0243(14) Uani 1 1 d . . . . .
C006 C 0.7451(7) 0.3019(7) 0.5664(2) 0.0323(16) Uani 1 1 d . . . . .
H006 H 0.750946 0.386692 0.558052 0.039 Uiso 1 1 calc R . . . .
C007 C 0.4324(10) 0.3801(8) 0.6307(3) 0.0399(17) Uani 1 1 d . . . . .
C008 C 0.8322(8) 0.2645(9) 0.5451(2) 0.0376(18) Uani 1 1 d . . . . .
C009 C 0.5291(8) 0.3568(7) 0.6083(2) 0.0320(16) Uani 1 1 d . . . . .
H009 H 0.581915 0.414123 0.582549 0.038 Uiso 1 1 calc R . . . .
C00A C 0.8206(8) 0.1390(8) 0.5589(3) 0.0423(18) Uani 1 1 d . . . . .
H00A H 0.878598 0.109052 0.545149 0.051 Uiso 1 1 calc R . . . .
C00B C 0.7237(8) 0.0595(8) 0.5929(3) 0.0360(16) Uani 1 1 d . . . . .
H00B H 0.716978 -0.025015 0.602312 0.043 Uiso 1 1 calc R . . . .
C00C C 0.3620(11) 0.2940(11) 0.6696(3) 0.056(3) Uani 1 1 d . . . . .
H00C H 0.297268 0.307493 0.687170 0.067 Uiso 1 1 calc R . . . .
C00D C 0.3866(11) 0.1919(11) 0.6820(3) 0.054(2) Uani 1 1 d . . . . .
H00D H 0.334795 0.133202 0.707616 0.064 Uiso 1 1 calc R . . . .
C00E C 0.9351(9) 0.3568(9) 0.5068(3) 0.046(2) Uani 1 1 d . . . . .
C00F C 1.0309(10) 0.4988(11) 0.5280(4) 0.065(3) Uani 1 1 d . . . . .
H00E H 0.976293 0.531666 0.544930 0.097 Uiso 1 1 calc GR . . . .
H00F H 1.083058 0.563150 0.502198 0.097 Uiso 1 1 calc GR . . . .
H00G H 1.094759 0.492836 0.550477 0.097 Uiso 1 1 calc GR . . . .
C00G C 0.8477(11) 0.3719(13) 0.4664(3) 0.070(3) Uani 1 1 d . . . . .
H00H H 0.773510 0.280540 0.456945 0.104 Uiso 1 1 calc GR . . . .
H00I H 0.906546 0.417729 0.438685 0.104 Uiso 1 1 calc GR . . . .
H00J H 0.808117 0.426830 0.478200 0.104 Uiso 1 1 calc GR . . . .
C00H C 0.2718(13) 0.4779(13) 0.6347(4) 0.069(3) Uani 1 1 d . . . . .
H00K H 0.197849 0.384626 0.627051 0.104 Uiso 1 1 calc GR . . . .
H00L H 0.251307 0.545131 0.620172 0.104 Uiso 1 1 calc GR . . . .
H00M H 0.278874 0.490362 0.669500 0.104 Uiso 1 1 calc GR . . . .
C00I C 0.4113(12) 0.4993(11) 0.6144(4) 0.056(3) Uani 1 1 d . . . . .
C00J C 0.4096(15) 0.5062(14) 0.5604(4) 0.073(3) Uani 1 1 d . . . . .
H00N H 0.497725 0.521948 0.547669 0.109 Uiso 1 1 calc GR . . . .
H00O H 0.395066 0.581860 0.550614 0.109 Uiso 1 1 calc GR . . . .
H00P H 0.334924 0.419236 0.547790 0.109 Uiso 1 1 calc GR . . . .
C00K C 1.0197(12) 0.2943(14) 0.4863(5) 0.077(3) Uani 1 1 d . . . . .
H00Q H 1.074670 0.285824 0.511985 0.115 Uiso 1 1 calc GR . . . .
H00R H 1.080966 0.354321 0.461094 0.115 Uiso 1 1 calc GR . . . .
H00S H 0.957240 0.203149 0.472984 0.115 Uiso 1 1 calc GR . . . .
C00L C 0.5300(14) 0.6322(10) 0.6342(4) 0.073(3) Uani 1 1 d . . . . .
H00T H 0.526312 0.629928 0.669305 0.109 Uiso 1 1 calc GR . . . .
H00U H 0.522526 0.710618 0.622602 0.109 Uiso 1 1 calc GR . . . .
H00V H 0.617429 0.641571 0.623557 0.109 Uiso 1 1 calc GR . . . .
F1 F 0.7624(14) 0.8062(14) 0.5483(5) 0.087(4) Uiso 0.5 1 d D . . A .
F2 F 0.8063(18) 0.6344(16) 0.5667(6) 0.049 Uiso 0.25 1 d D . . A 2
B0AA B 0.8494(18) 0.7534(18) 0.5393(6) 0.074(7) Uiso 0.5 1 d D . . . .
F1AA F 0.9884(15) 0.8425(19) 0.5506(6) 0.049 Uiso 0.25 1 d D . . A 2
F2AA F 0.8417(18) 0.716(2) 0.4897(5) 0.049 Uiso 0.25 1 d D . . A 2
F3AA F 0.7728(18) 0.6073(14) 0.5325(7) 0.049 Uiso 0.25 1 d D . . A 1
F4AA F 0.903(2) 0.8081(19) 0.4916(5) 0.049 Uiso 0.25 1 d D . . A 1
F6 F 0.9550(18) 0.786(2) 0.5704(6) 0.049 Uiso 0.25 1 d D . . A 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
Cu01 0.0327(5) 0.0278(7) 0.0271(6) 0.0094(5) 0.0047(2) 0.0139(3)
N002 0.034(3) 0.025(3) 0.021(3) 0.000(2) 0.001(2) 0.015(2)
N003 0.040(3) 0.038(4) 0.027(3) 0.004(3) 0.002(3) 0.024(3)
C004 0.025(3) 0.024(3) 0.023(3) -0.001(3) -0.004(3) 0.008(3)
C005 0.024(3) 0.021(3) 0.020(3) -0.002(2) -0.003(2) 0.005(3)
C006 0.029(4) 0.027(4) 0.030(3) 0.004(3) 0.001(3) 0.006(3)
C007 0.059(5) 0.038(4) 0.036(4) -0.001(3) 0.000(4) 0.034(4)
C008 0.031(4) 0.043(4) 0.025(3) 0.013(3) 0.004(3) 0.008(3)
C009 0.045(4) 0.026(3) 0.024(3) 0.001(3) -0.004(3) 0.017(3)
C00A 0.037(4) 0.053(5) 0.040(4) 0.000(3) 0.011(3) 0.025(4)
C00B 0.032(4) 0.034(4) 0.044(4) 0.007(3) 0.004(3) 0.017(3)
C00C 0.065(6) 0.074(7) 0.055(5) 0.016(5) 0.021(5) 0.055(5)
C00D 0.066(6) 0.069(6) 0.045(5) 0.024(4) 0.027(4) 0.048(5)
C00E 0.032(4) 0.053(5) 0.037(4) 0.012(3) 0.016(4) 0.009(4)
C00F 0.043(5) 0.060(6) 0.055(5) 0.014(5) 0.006(4) -0.001(5)
C00G 0.051(6) 0.091(8) 0.031(4) 0.024(5) 0.004(4) 0.009(6)
C00H 0.093(8) 0.084(8) 0.070(6) 0.010(6) 0.015(6) 0.073(7)
C00I 0.078(7) 0.050(5) 0.062(5) 0.009(4) 0.001(5) 0.049(5)
C00J 0.112(10) 0.089(8) 0.058(6) 0.018(6) 0.007(6) 0.080(8)
C00K 0.052(6) 0.085(8) 0.077(7) 0.020(6) 0.036(6) 0.022(6)
C00L 0.091(9) 0.035(5) 0.090(8) 0.002(5) 0.002(7) 0.029(5)
_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
Cu01 N002 2.005(6) 5_556 ?
Cu01 N002 2.005(6) . ?
Cu01 N003 2.028(7) 5_556 ?
Cu01 N003 2.028(7) . ?
N002 C005 1.332(9) . ?
N002 C00B 1.369(10) . ?
N003 C004 1.347(9) . ?
N003 C00D 1.346(11) . ?
C004 C005 1.489(10) . ?
C004 C009 1.388(10) . ?
C005 C006 1.397(9) . ?
C006 H006 0.9500 . ?
C006 C008 1.377(12) . ?
C007 C009 1.387(12) . ?
C007 C00C 1.404(12) . ?
C007 C00I 1.540(11) . ?
C008 C00A 1.402(12) . ?
C008 C00E 1.534(10) . ?
C009 H009 0.9500 . ?
C00A H00A 0.9500 . ?
C00A C00B 1.382(11) . ?
C00B H00B 0.9500 . ?
C00C H00C 0.9500 . ?
C00C C00D 1.351(13) . ?
C00D H00D 0.9500 . ?
C00E C00F 1.528(14) . ?
C00E C00G 1.559(14) . ?
C00E C00K 1.544(15) . ?
C00F H00E 0.9800 . ?
C00F H00F 0.9800 . ?
C00F H00G 0.9800 . ?
C00G H00H 0.9800 . ?
C00G H00I 0.9800 . ?
C00G H00J 0.9800 . ?
C00H H00K 0.9800 . ?
C00H H00L 0.9800 . ?
C00H H00M 0.9800 . ?
C00H C00I 1.566(15) . ?
C00I C00J 1.511(14) . ?
C00I C00L 1.523(16) . ?
C00J H00N 0.9800 . ?
C00J H00O 0.9800 . ?
C00J H00P 0.9800 . ?
C00K H00Q 0.9800 . ?
C00K H00R 0.9800 . ?
C00K H00S 0.9800 . ?
C00L H00T 0.9800 . ?
C00L H00U 0.9800 . ?
C00L H00V 0.9800 . ?
F1 B0AA 1.395(18) . ?
F1 F2AA 1.33(2) 4_556 ?
F1 F4AA 1.46(2) 4_556 ?
F2 B0AA 1.398(18) . ?
B0AA F1AA 1.404(19) . ?
B0AA F2AA 1.439(18) . ?
B0AA F3AA 1.433(19) . ?
B0AA F4AA 1.466(18) . ?
B0AA F6 1.363(18) . ?
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
N002 Cu01 N002 122.3(3) 5_556 . ?
N002 Cu01 N003 136.6(2) . 5_556 ?
N002 Cu01 N003 80.8(2) . . ?
N002 Cu01 N003 80.8(2) 5_556 5_556 ?
N002 Cu01 N003 136.6(2) 5_556 . ?
N003 Cu01 N003 107.9(4) 5_556 . ?
C005 N002 Cu01 114.9(5) . . ?
C005 N002 C00B 117.7(6) . . ?
C00B N002 Cu01 127.2(5) . . ?
C004 N003 Cu01 114.0(5) . . ?
C00D N003 Cu01 128.1(6) . . ?
C00D N003 C004 116.6(7) . . ?
N003 C004 C005 114.0(6) . . ?
N003 C004 C009 122.3(7) . . ?
C009 C004 C005 123.7(6) . . ?
N002 C005 C004 115.2(6) . . ?
N002 C005 C006 122.1(7) . . ?
C006 C005 C004 122.6(6) . . ?
C005 C006 H006 119.7 . . ?
C008 C006 C005 120.6(7) . . ?
C008 C006 H006 119.7 . . ?
C009 C007 C00C 116.2(7) . . ?
C009 C007 C00I 120.4(8) . . ?
C00C C007 C00I 123.3(9) . . ?
C006 C008 C00A 117.6(6) . . ?
C006 C008 C00E 120.3(8) . . ?
C00A C008 C00E 122.0(8) . . ?
C004 C009 H009 119.7 . . ?
C007 C009 C004 120.5(7) . . ?
C007 C009 H009 119.7 . . ?
C008 C00A H00A 120.5 . . ?
C00B C00A C008 119.0(7) . . ?
C00B C00A H00A 120.5 . . ?
N002 C00B C00A 122.9(7) . . ?
N002 C00B H00B 118.6 . . ?
C00A C00B H00B 118.6 . . ?
C007 C00C H00C 120.0 . . ?
C00D C00C C007 119.9(8) . . ?
C00D C00C H00C 120.0 . . ?
N003 C00D C00C 124.3(8) . . ?
N003 C00D H00D 117.8 . . ?
C00C C00D H00D 117.8 . . ?
C008 C00E C00G 106.0(7) . . ?
C008 C00E C00K 112.2(8) . . ?
C00F C00E C008 109.5(7) . . ?
C00F C00E C00G 108.6(9) . . ?
C00F C00E C00K 110.2(9) . . ?
C00K C00E C00G 110.2(9) . . ?
C00E C00F H00E 109.5 . . ?
C00E C00F H00F 109.5 . . ?
C00E C00F H00G 109.5 . . ?
H00E C00F H00F 109.5 . . ?
H00E C00F H00G 109.5 . . ?
H00F C00F H00G 109.5 . . ?
C00E C00G H00H 109.5 . . ?
C00E C00G H00I 109.5 . . ?
C00E C00G H00J 109.5 . . ?
H00H C00G H00I 109.5 . . ?
H00H C00G H00J 109.5 . . ?
H00I C00G H00J 109.5 . . ?
H00K C00H H00L 109.5 . . ?
H00K C00H H00M 109.5 . . ?
H00L C00H H00M 109.5 . . ?
C00I C00H H00K 109.5 . . ?
C00I C00H H00L 109.5 . . ?
C00I C00H H00M 109.5 . . ?
C007 C00I C00H 109.6(9) . . ?
C00J C00I C007 110.6(8) . . ?
C00J C00I C00H 109.4(9) . . ?
C00J C00I C00L 109.9(10) . . ?
C00L C00I C007 107.7(8) . . ?
C00L C00I C00H 109.7(9) . . ?
C00I C00J H00N 109.5 . . ?
C00I C00J H00O 109.5 . . ?
C00I C00J H00P 109.5 . . ?
H00N C00J H00O 109.5 . . ?
H00N C00J H00P 109.5 . . ?
H00O C00J H00P 109.5 . . ?
C00E C00K H00Q 109.5 . . ?
C00E C00K H00R 109.5 . . ?
C00E C00K H00S 109.5 . . ?
H00Q C00K H00R 109.5 . . ?
H00Q C00K H00S 109.5 . . ?
H00R C00K H00S 109.5 . . ?
C00I C00L H00T 109.5 . . ?
C00I C00L H00U 109.5 . . ?
C00I C00L H00V 109.5 . . ?
H00T C00L H00U 109.5 . . ?
H00T C00L H00V 109.5 . . ?
H00U C00L H00V 109.5 . . ?
B0AA F1 F4AA 96.9(13) . 4_556 ?
F2AA F1 B0AA 116.7(13) 4_556 . ?
F2AA F1 F4AA 38.0(10) 4_556 4_556 ?
F1 B0AA F2 109.1(14) . . ?
F1 B0AA F1AA 114.9(15) . . ?
F1 B0AA F2AA 110.3(14) . . ?
F1 B0AA F3AA 111.3(14) . . ?
F1 B0AA F4AA 102.3(13) . . ?
F2 B0AA F1AA 106.8(15) . . ?
F2 B0AA F2AA 107.7(15) . . ?
F1AA B0AA F2AA 107.9(15) . . ?
F3AA B0AA F4AA 104.1(14) . . ?
F6 B0AA F1 118.1(15) . . ?
F6 B0AA F3AA 109.5(15) . . ?
F6 B0AA F4AA 110.3(15) . . ?
F1 F2AA B0AA 129.6(16) 4_556 . ?
F1 F4AA B0AA 118.0(15) 4_556 . ?
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
Cu01 N002 C005 C004 -5.9(7) . . . . ?
Cu01 N002 C005 C006 174.9(5) . . . . ?
Cu01 N002 C00B C00A -174.9(6) . . . . ?
Cu01 N003 C004 C005 -10.7(7) . . . . ?
Cu01 N003 C004 C009 169.0(5) . . . . ?
Cu01 N003 C00D C00C -167.6(8) . . . . ?
N002 C005 C006 C008 0.7(10) . . . . ?
N003 C004 C005 N002 11.1(8) . . . . ?
N003 C004 C005 C006 -169.8(6) . . . . ?
N003 C004 C009 C007 -1.5(11) . . . . ?
C004 N003 C00D C00C -1.6(15) . . . . ?
C004 C005 C006 C008 -178.3(6) . . . . ?
C005 N002 C00B C00A -0.4(11) . . . . ?
C005 C004 C009 C007 178.2(7) . . . . ?
C005 C006 C008 C00A -0.6(11) . . . . ?
C005 C006 C008 C00E 178.0(7) . . . . ?
C006 C008 C00A C00B 0.0(11) . . . . ?
C006 C008 C00E C00F 59.1(11) . . . . ?
C006 C008 C00E C00G -57.9(10) . . . . ?
C006 C008 C00E C00K -178.2(8) . . . . ?
C007 C00C C00D N003 2.4(18) . . . . ?
C008 C00A C00B N002 0.5(12) . . . . ?
C009 C004 C005 N002 -168.6(6) . . . . ?
C009 C004 C005 C006 10.6(10) . . . . ?
C009 C007 C00C C00D -2.6(15) . . . . ?
C009 C007 C00I C00H 164.0(9) . . . . ?
C009 C007 C00I C00J 43.4(13) . . . . ?
C009 C007 C00I C00L -76.7(11) . . . . ?
C00A C008 C00E C00F -122.4(9) . . . . ?
C00A C008 C00E C00G 120.6(10) . . . . ?
C00A C008 C00E C00K 0.4(12) . . . . ?
C00B N002 C005 C004 178.9(6) . . . . ?
C00B N002 C005 C006 -0.2(10) . . . . ?
C00C C007 C009 C004 2.1(12) . . . . ?
C00C C007 C00I C00H -19.0(13) . . . . ?
C00C C007 C00I C00J -139.7(11) . . . . ?
C00C C007 C00I C00L 100.2(12) . . . . ?
C00D N003 C004 C005 -178.6(7) . . . . ?
C00D N003 C004 C009 1.0(11) . . . . ?
C00E C008 C00A C00B -178.6(7) . . . . ?
C00I C007 C009 C004 179.3(8) . . . . ?
C00I C007 C00C C00D -179.6(10) . . . . ?
F1 B0AA F2AA F1 25(2) . . . 4_556 ?
F1 B0AA F4AA F1 -64.5(18) . . . 4_556 ?
F2 B0AA F2AA F1 143.5(19) . . . 4_556 ?
F1AA B0AA F2AA F1 -102(2) . . . 4_556 ?
F2AA F1 B0AA F2 -133.0(16) 4_556 . . . ?
F2AA F1 B0AA F1AA 107.2(18) 4_556 . . . ?
F2AA F1 B0AA F2AA -14.9(18) 4_556 . . . ?
F3AA B0AA F4AA F1 51.5(19) . . . 4_556 ?
F4AA F1 B0AA F3AA -122.3(14) 4_556 . . . ?
F4AA F1 B0AA F4AA -11.6(13) 4_556 . . . ?
F4AA F1 B0AA F6 109.7(16) 4_556 . . . ?
F6 B0AA F4AA F1 168.9(16) . . . 4_556 ?
_shelx_res_file
;
TITL Bishwnath_10Sept216_a.res in P3(2)21
bishwnath_10sept216_a.res
created by SHELXL-2016/6 at 10:09:16 on 18-Oct-2018
REM Old TITL Bishwnath_10Sept216 in P3(2)21
REM SHELXT solution in P3(2)21
REM R1 0.128, Rweak 0.042, Alpha 0.017, Orientation as input
REM Flack x = 0.049 ( 0.009 ) from Parsons' quotients
REM Formula found by SHELXT: C44 N4 Cu
CELL 0.71073 11.2232 11.2232 27.9237 90 90 120
ZERR 6 0.0015 0.0015 0.0037 0 0 0
LATT -1
SYMM -Y,+X-Y,0.667+Z
SYMM +Y-X,-X,0.333+Z
SYMM +Y,+X,-Z
SYMM -Y+X,-Y,0.333-Z
SYMM -X,-X+Y,0.667-Z
SFAC C H B Cu F N
UNIT 108 144 3 3 12 12
DFIX 1.419 F6 B0AA F1AA B0AA F4AA B0AA F2AA B0AA F1 B0AA F2 B0AA F3AA B0AA
DFIX 2.32 F4AA F6
DFIX 2.32 F6 F3AA
DFIX 2.32 F3AA F4AA
DFIX 2.32 F2AA F1AA
DFIX 2.32 F1AA F2
DFIX 2.32 F2 F2AA
DFIX 2.32 F1 F4AA
DFIX 2.32 F1 F6
DFIX 2.32 F1 F3AA
DFIX 2.32 F1 F1AA
DFIX 2.32 F1 F2AA
DFIX 2.32 F1 F2
L.S. 15
PLAN 20
SIZE 0.045 0.135 0.326
TEMP -123.15
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
OMIT -3 50
OMIT 0 1 0
OMIT 1 1 0
OMIT 0 2 2
OMIT -1 1 2
OMIT 1 2 2
OMIT -2 2 2
OMIT 1 2 0
OMIT -3 3 3
OMIT -4 4 5
OMIT -4 4 2
OMIT 0 1 6
REM
REM
REM
WGHT 0.159400 2.600000
FVAR 0.52858
CU01 4 0.502133 0.000000 0.666667 10.50000 0.03270 0.02780 =
0.02705 0.00937 0.00468 0.01390
N002 6 0.636886 0.097131 0.613621 11.00000 0.03444 0.02483 =
0.02126 -0.00047 0.00090 0.01479
N003 6 0.479724 0.167793 0.660329 11.00000 0.03972 0.03838 =
0.02673 0.00397 0.00199 0.02362
C004 1 0.549475 0.250366 0.623315 11.00000 0.02495 0.02354 =
0.02297 -0.00128 -0.00364 0.00761
C005 1 0.648346 0.216312 0.600231 11.00000 0.02408 0.02098 =
0.01971 -0.00181 -0.00346 0.00526
C006 1 0.745129 0.301893 0.566420 11.00000 0.02929 0.02698 =
0.02993 0.00392 0.00087 0.00612
AFIX 43
H006 2 0.750946 0.386692 0.558052 11.00000 -1.20000
AFIX 0
C007 1 0.432372 0.380132 0.630740 11.00000 0.05873 0.03790 =
0.03589 -0.00086 -0.00044 0.03382
C008 1 0.832213 0.264464 0.545099 11.00000 0.03125 0.04251 =
0.02504 0.01316 0.00411 0.00789
C009 1 0.529135 0.356800 0.608343 11.00000 0.04459 0.02614 =
0.02413 0.00058 -0.00366 0.01679
AFIX 43
H009 2 0.581915 0.414123 0.582549 11.00000 -1.20000
AFIX 0
C00A 1 0.820637 0.138970 0.558934 11.00000 0.03708 0.05257 =
0.04011 0.00002 0.01145 0.02463
AFIX 43
H00A 2 0.878598 0.109052 0.545149 11.00000 -1.20000
AFIX 0
C00B 1 0.723687 0.059482 0.592911 11.00000 0.03164 0.03401 =
0.04351 0.00696 0.00376 0.01723
AFIX 43
H00B 2 0.716978 -0.025015 0.602312 11.00000 -1.20000
AFIX 0
C00C 1 0.362046 0.293983 0.669600 11.00000 0.06480 0.07392 =
0.05465 0.01610 0.02051 0.05462
AFIX 43
H00C 2 0.297268 0.307493 0.687170 11.00000 -1.20000
AFIX 0
C00D 1 0.386635 0.191894 0.681957 11.00000 0.06599 0.06893 =
0.04539 0.02436 0.02716 0.04825
AFIX 43
H00D 2 0.334795 0.133202 0.707616 11.00000 -1.20000
AFIX 0
C00E 1 0.935133 0.356777 0.506813 11.00000 0.03217 0.05321 =
0.03747 0.01193 0.01610 0.00947
C00F 1 1.030893 0.498840 0.528004 11.00000 0.04261 0.06048 =
0.05543 0.01384 0.00640 -0.00073
AFIX 137
H00E 2 0.976293 0.531666 0.544930 11.00000 -1.50000
H00F 2 1.083058 0.563150 0.502198 11.00000 -1.50000
H00G 2 1.094759 0.492836 0.550477 11.00000 -1.50000
AFIX 0
C00G 1 0.847709 0.371870 0.466409 11.00000 0.05078 0.09114 =
0.03126 0.02370 0.00354 0.00888
AFIX 137
H00H 2 0.773510 0.280540 0.456945 11.00000 -1.50000
H00I 2 0.906546 0.417729 0.438685 11.00000 -1.50000
H00J 2 0.808117 0.426830 0.478200 11.00000 -1.50000
AFIX 0
C00H 1 0.271775 0.477855 0.634677 11.00000 0.09257 0.08376 =
0.06964 0.00973 0.01466 0.07282
AFIX 137
H00K 2 0.197849 0.384626 0.627051 11.00000 -1.50000
H00L 2 0.251307 0.545131 0.620172 11.00000 -1.50000
H00M 2 0.278874 0.490362 0.669500 11.00000 -1.50000
AFIX 0
C00I 1 0.411274 0.499339 0.614397 11.00000 0.07829 0.04974 =
0.06172 0.00905 0.00117 0.04889
C00J 1 0.409600 0.506198 0.560370 11.00000 0.11150 0.08900 =
0.05764 0.01786 0.00672 0.08028
AFIX 137
H00N 2 0.497725 0.521948 0.547669 11.00000 -1.50000
H00O 2 0.395066 0.581860 0.550614 11.00000 -1.50000
H00P 2 0.334924 0.419236 0.547790 11.00000 -1.50000
AFIX 0
C00K 1 1.019732 0.294310 0.486349 11.00000 0.05242 0.08462 =
0.07655 0.01990 0.03553 0.02205
AFIX 137
H00Q 2 1.074670 0.285824 0.511985 11.00000 -1.50000
H00R 2 1.080966 0.354321 0.461094 11.00000 -1.50000
H00S 2 0.957240 0.203149 0.472984 11.00000 -1.50000
AFIX 0
C00L 1 0.529959 0.632201 0.634232 11.00000 0.09120 0.03485 =
0.08967 0.00249 0.00199 0.02908
AFIX 137
H00T 2 0.526312 0.629928 0.669305 11.00000 -1.50000
H00U 2 0.522526 0.710618 0.622602 11.00000 -1.50000
H00V 2 0.617429 0.641571 0.623557 11.00000 -1.50000
AFIX 0
F1 5 0.762387 0.806190 0.548283 10.50000 0.08738
PART 2
F2 5 0.806338 0.634426 0.566710 10.25000 10.04883
PART 0
B0AA 3 0.849405 0.753371 0.539330 10.50000 0.07394
PART 2
F1AA 5 0.988399 0.842495 0.550589 10.25000 10.04883
F2AA 5 0.841712 0.715586 0.489710 10.25000 10.04883
PART 0
PART 1
F3AA 5 0.772840 0.607255 0.532502 10.25000 10.04883
F4AA 5 0.903080 0.808129 0.491555 10.25000 10.04883
F6 5 0.954979 0.785841 0.570428 10.25000 10.04883
HKLF 4
REM Bishwnath_10Sept216_a.res in P3(2)21
REM R1 = 0.0787 for 3228 Fo > 4sig(Fo) and 0.0857 for all 3579 data
REM 218 parameters refined using 19 restraints
END
WGHT 0.1600 2.5683
REM Highest difference peak 1.060, deepest hole -1.147, 1-sigma level 0.134
Q1 1 0.8776 0.7032 0.5549 11.00000 0.05 1.06
Q2 1 0.7578 0.6304 0.5488 11.00000 0.05 0.91
Q3 1 0.9905 0.0264 0.6582 11.00000 0.05 0.83
Q4 1 0.8366 0.6772 0.5858 11.00000 0.05 0.76
Q5 1 1.0406 1.0562 0.6204 11.00000 0.05 0.75
Q6 1 0.8996 0.8390 0.5958 11.00000 0.05 0.61
Q7 1 0.7047 0.6030 0.5218 11.00000 0.05 0.50
Q8 1 0.9358 0.8331 0.5220 11.00000 0.05 0.48
Q9 1 0.7096 0.3291 0.4411 11.00000 0.05 0.44
Q10 1 0.4245 0.4414 0.6241 11.00000 0.05 0.43
Q11 1 0.9645 0.7663 0.5422 11.00000 0.05 0.41
Q12 1 0.3549 0.6257 0.5090 11.00000 0.05 0.38
Q13 1 0.7225 0.7847 0.5283 11.00000 0.05 0.34
Q14 1 0.7941 0.7271 0.5189 11.00000 0.05 0.34
Q15 1 0.3623 0.6255 0.5481 11.00000 0.05 0.33
Q16 1 0.5100 0.0491 0.6182 11.00000 0.05 0.32
Q17 1 0.6723 0.2830 0.5158 11.00000 0.05 0.31
Q18 1 0.0588 0.4803 0.6181 11.00000 0.05 0.31
Q19 1 0.7435 0.7435 0.5000 10.50000 0.05 0.30
Q20 1 0.4033 0.3299 0.6483 11.00000 0.05 0.30
;
_shelx_res_checksum 39884
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT601_bishwnath_10sept216_a
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 111 Ang**3
RESPONSE: The peaks of ~ 1 eA-3 are not included which may be partially
occupied / disordered solvent.
;
_vrf_PLAT987_bishwnath_10sept216_a
;
PROBLEM: The Flack x is >> 0 - Do a BASF/TWIN Refinement Please Check
RESPONSE: TWIN refinement does not make any difference to the Flack x.
;
# end Validation Reply Form
#######################################################################
#
# 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_bishwanath_27sept16_cu_0m_a
_audit_block_doi 10.5517/ccdc.csd.cc2145q3
_database_code_depnum_ccdc_archive 'CCDC 1880854'
_audit_update_record
;
2019-01-24 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;
_audit_creation_date 2018-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36.33 H48 Cu N4 O, 4(F2 P0.33)'
_chemical_formula_sum 'C36.33 H48 Cu F8 N4 O P1.33'
_chemical_formula_weight 813.62
_chemical_absolute_configuration ?
_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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
_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 trigonal
_space_group_IT_number 146
_space_group_name_H-M_alt 'R 3'
_space_group_name_Hall 'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
_cell_length_a 19.4230(19)
_cell_length_b 19.4230(19)
_cell_length_c 29.434(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 9616(2)
_cell_formula_units_Z 9
_cell_measurement_reflns_used 2663
_cell_measurement_temperature 149.99
_cell_measurement_theta_max 18.041
_cell_measurement_theta_min 2.518
_shelx_estimated_absorpt_T_max 0.978
_shelx_estimated_absorpt_T_min 0.932
_exptl_absorpt_coefficient_mu 0.627
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6255
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1278 before and 0.0776 after correction. The Ratio of minimum to maximum transmission is 0.8389. The \l/2 correction factor is 0.00150.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'bluish green'
_exptl_crystal_colour_modifier bluish
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 1.264
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 3807
_exptl_crystal_size_max 0.114
_exptl_crystal_size_mid 0.107
_exptl_crystal_size_min 0.036
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1113
_diffrn_reflns_av_unetI/netI 0.1420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_number 23382
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full 24.998
_diffrn_reflns_theta_max 24.998
_diffrn_reflns_theta_min 2.789
_diffrn_ambient_temperature 149.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.844
_reflns_Friedel_fraction_full 0.843
_reflns_Friedel_fraction_max 0.843
_reflns_number_gt 3786
_reflns_number_total 6937
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
The diffraction from this crystal falls off within two sigma
level after 38 degrees of two theta, could be attributed to
the lattice that contains disordered anions, terminal groups etc.
_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 v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.687
_refine_diff_density_min -1.068
_refine_diff_density_rms 0.081
_refine_ls_abs_structure_details
;
Flack x determined using 1164 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.033(18)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 488
_refine_ls_number_reflns 6937
_refine_ls_number_restraints 330
_refine_ls_R_factor_all 0.1592
_refine_ls_R_factor_gt 0.0812
_refine_ls_restrained_S_all 1.090
_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^)+(0.1356P)^2^+3.2895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2111
_refine_ls_wR_factor_ref 0.2586
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C27-CAD
2.52 with sigma of 0.02
C1AA-C1
1.54 with sigma of 0.02
C3BA-C24
2.52 with sigma of 0.02
C24-C12
2.52 with sigma of 0.02
C12-C3BA
2.52 with sigma of 0.02
C8AA-C00J
1.54 with sigma of 0.02
P2-F4 = P2-F5
1.64 with sigma of 0.02
P2-F3AA
1.64 with sigma of 0.02
P2-F17 = P2-F4AA = P2-F13
1.64 with sigma of 0.02
F17-F4AA
2.32 with sigma of 0.02
F3AA-F4AA
2.32 with sigma of 0.02
F13-F3AA
2.32 with sigma of 0.02
C17-C6 = C9-C30
2.52 with sigma of 0.02
C1-C27 = C7AA-C2AA
2.52 with sigma of 0.02
C27-CAD = C2AA-C4
2.52 with sigma of 0.02
CAD-C1 = C4-C7AA
2.52 with sigma of 0.02
C1BA-C0CA = C4BA-C18 = C5AA-C16
2.52 with sigma of 0.02
P1-F0AA
1.64 with sigma of 0.02
P1-F2AA
1.64 with sigma of 0.02
P1-F12
1.64 with sigma of 0.02
C32-C5 = C3BA-C24
2.52 with sigma of 0.02
C32-C21 = C6BA-C24
2.52 with sigma of 0.02
C3BA-C2 = C5-C2 = C24-C2 = C2-C12 = C21-C2
1.54 with sigma of 0.02
C21-C5
2.52 with sigma of 0.02
C21-C5 = C6BA-C3BA
2.52 with sigma of 0.02
C19-C1BA = C0AA-C4BA = C4AA-C5AA
2.52 with sigma of 0.02
C0CA-C19 = C18-C0AA = C16-C4AA
2.52 with sigma of 0.02
C30-C28 = C13-C6
2.52 with sigma of 0.02
C9-C28 = C17-C13
2.52 with sigma of 0.02
F2AB-F8A
2.32 with sigma of 0.02
F6AA-P2
1.64 with sigma of 0.02
P2-F13 = P2-F8AA = P2-F5 = P2-F31 = P2-F17 = P2-F3AA = P2-F3BA = P2-F7AA = P2-
F4
1.64 with sigma of 0.02
P2-F6AA
1.64 with sigma of 0.02
F4AA-F31
2.32 with sigma of 0.02
F31-F4
2.32 with sigma of 0.02
F13-F8AA
2.32 with sigma of 0.02
F4-F8AA
2.32 with sigma of 0.02
F7AA-F2
2.32 with sigma of 0.02
CAD-C1AA \\sim C27-C1AA
with sigma of 0.02
F4AA-F13 \\sim F4AA-F3AA \\sim F4AA-F17 \\sim F13-F3AA
with sigma of 0.04
P2-F4AA \\sim P2-F13 \\sim P2-F3AA \\sim P2-F17
with sigma of 0.02
C2AA-C1AA \\sim C27-C1AA \\sim C7AA-C1AA \\sim C1AA-C1 \\sim C4-C1AA \\sim
CAD-C1AA
with sigma of 0.02
P1-F2AA \\sim P1-F12
with sigma of 0.02
P1-F20 \\sim P1-F0AA \\sim P1-F2AA \\sim P1-F8 \\sim P1-F18
with sigma of 0.02
F0AA-F18 \\sim F8-F20
with sigma of 0.02
P1-F2AA \\sim P1-F2AB
with sigma of 0.02
P1-F0AA \\sim P1-F0AB
with sigma of 0.02
P1-F20 \\sim P1-F20A
with sigma of 0.02
P1-F8 \\sim P1-F8A
with sigma of 0.02
P1-F0AB \\sim P1-F20 \\sim P1-F20A \\sim P1-F8 \\sim P1-F8A \\sim P1-F2AA
\\sim P1-F2AB \\sim P1-F0AA
with sigma of 0.02
C21-C2 \\sim C6BA-C2 \\sim C5-C2 \\sim C3BA-C2 \\sim C24-C2 \\sim C32-C2
with sigma of 0.02
C5AA-C00J \\sim C0CA-C00J \\sim C18-C00J \\sim C16-C00J \\sim C19-C00J \\sim
C0AA-C00J \\sim C4AA-
C00J \\sim C1BA-C00J \\sim C4BA-C00J
with sigma of 0.02
C26-C13 \\sim C9-C26 \\sim C26-C17 \\sim C30-C26 \\sim C6-C26 \\sim C28-C26
with sigma of 0.02
F2-F7AA \\sim F2-F3BA \\sim F2-F6AA \\sim F2-F5 \\sim F17-F7AA \\sim F17-F3BA
\\sim F17-F5 \\sim F7AA-
F3BA \\sim F3BA-F6AA \\sim F6AA-F5
with sigma of 0.04
P2-F2 \\sim P2-F17 \\sim P2-F7AA \\sim P2-F3BA \\sim P2-F6AA \\sim P2-F5
with sigma of 0.02
3. Rigid bond restraints
F0AA, F2AA
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
F8, F2AA, F0AA, F20
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C21, CAD, C4, C1, C7AA, C27, C2AA
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C6BA) = Uanis(C2)
Uanis(C4) = Uanis(C1AA)
Uanis(C2AA) = Uanis(C1AA)
Uanis(C7AA) = Uanis(C1AA)
Uanis(C2) = Uanis(C21)
Uanis(C16) = Uanis(C19) = Uanis(C0AA) = Uanis(C1BA) = Uanis(C4BA) = Uanis(C5AA)
= Uanis(C0CA) = Uanis(C18) = Uanis(C4AA) = Uanis(C00J)
Uanis(C32) = Uanis(C2)
Uanis(C6) = Uanis(C26)
Uiso(F17) = Uiso(F31)
Uanis(C2AA) = Uanis(C27)
Uanis(Cu1) = Uanis(O00E)
Uanis(C2) = Uanis(C5)
Uiso(F6AA) = Uiso(F2)
Uiso(F31) = Uiso(F4AA)
5. Rigid body (RIGU) restrains
C3BA, C2
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C21, C2
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C9A, C2AA, CAD, C4, C1, C7AA, C27
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C9, C17, C30, C6, C28, C13, C26
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
Cu1, O00E
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
O00E, C00V
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
Cu1, O00E, C00V
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
C6, C30, C17, C9, C13, C28
with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
Fixed Sof: P1(0.33333) F4(0.5) F5(0.5) CAD(0.5) HADA(0.5) HADB(0.5) HADC(0.5)
C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C3BA(0.5) H3BA(0.5) H3BB(0.5) H3BC(0.5)
C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C1(0.5) H1C(0.5) H1D(0.5) H1E(0.5)
F12(0.33333) F3AA(0.5) F4AA(0.5) F13(0.5) F17(0.5) C28(0.5) H28A(0.5)
H28B(0.5) H28C(0.5) C4(0.5) H4C(0.5) H4D(0.5) H4E(0.5) C2AA(0.5) H2AA(0.5)
H2AB(0.5) H2AC(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C1BA(0.33333)
H1BA(0.33333) H1BB(0.33333) H1BC(0.33333) C5AA(0.33333) H5AA(0.33333)
H5AB(0.33333) H5AC(0.33333) C4BA(0.33333) H4BA(0.33333) H4BB(0.33333)
H4BC(0.33333) C7AA(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) F6AA(0.5) F7AA(0.5)
C6BA(0.5) H6BA(0.5) H6BB(0.5) H6BC(0.5) C0CA(0.33333) H0CA(0.33333)
H0CB(0.33333) H0CC(0.33333) F3BA(0.5) F8AA(0.5) F31(0.5) C17(0.5) H17A(0.5)
H17B(0.5) H17C(0.5) C4AA(0.33333) H4AA(0.33333) H4AB(0.33333) H4AC(0.33333)
C18(0.33333) H18A(0.33333) H18B(0.33333) H18C(0.33333) C30(0.5) H30A(0.5)
H30B(0.5) H30C(0.5) C9(0.5) H9C(0.5) H9D(0.5) H9E(0.5) C6(0.5) H6A(0.5)
H6B(0.5) H6C(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C0AA(0.33333)
H0AA(0.33333) H0AB(0.33333) H0AC(0.33333) C16(0.33333) H16A(0.33333)
H16B(0.33333) H16C(0.33333) C19(0.33333) H19A(0.33333) H19B(0.33333)
H19C(0.33333) F2AA(0.16667) F0AA(0.16667) F20(0.16667) F8(0.16667)
F18(0.33333) F20A(0.16666) F0AB(0.16666) F2AB(0.16666) F8A(0.16666) F2(0.5)
Fixed Uiso: F2AA(0.1) F0AA(0.1) F20(0.1) F8(0.1) F20A(0.1) F0AB(0.1)
F2AB(0.1) F8A(0.1)
7.a Riding coordinates:
CAD(HADA,HADB,HADC), C5(H5A,H5B,H5C), C24(H24A,H24B,H24C), C21(H21A,H21B,
H21C), C3BA(H3BA,H3BB,H3BC), C27(H27A,H27B,H27C), C1(H1C,H1D,H1E), C28(H28A,
H28B,H28C), C4(H4C,H4D,H4E), C2AA(H2AA,H2AB,H2AC), C32(H32A,H32B,H32C),
C1BA(H1BA,H1BB,H1BC), C5AA(H5AA,H5AB,H5AC), C4BA(H4BA,H4BB,H4BC), C7AA(H7AA,
H7AB,H7AC), C6BA(H6BA,H6BB,H6BC), C0CA(H0CA,H0CB,H0CC), C17(H17A,H17B,H17C),
C4AA(H4AA,H4AB,H4AC), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C9(H9C,H9D,
H9E), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C0AA(H0AA,H0AB,H0AC), C16(H16A,
H16B,H16C), C19(H19A,H19B,H19C)
7.b Free rotating group:
P2(F4,F5)
7.c Aromatic/amide H refined with riding coordinates:
C1A(H1A), C2A(H2A), C4A(H4A), C7A(H7A), C9A(H9A), C10A(H10A), C1B(H1B),
C2B(H2B), C4B(H4B), C7B(H7B), C9B(H9B), C10B(H10B)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_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
Cu1 Cu 0.52836(8) 0.33309(10) 0.50036(6) 0.0639(5) Uani 1 1 d . U . A 1
N1A N 0.4168(6) 0.2283(7) 0.5075(3) 0.066(3) Uani 1 1 d . . . . .
N2A N 0.5195(7) 0.3263(7) 0.5677(5) 0.068(4) Uani 1 1 d . . . . .
C1A C 0.3698(10) 0.1761(11) 0.4765(5) 0.087(5) Uani 1 1 d . . . . .
H1A H 0.386433 0.185039 0.445625 0.105 Uiso 1 1 calc R . . . .
C2A C 0.2995(11) 0.1107(11) 0.4868(5) 0.089(5) Uani 1 1 d . . . . .
H2A H 0.267986 0.077289 0.462662 0.107 Uiso 1 1 calc R . . . .
C4A C 0.3251(9) 0.1448(9) 0.5635(4) 0.074(4) Uani 1 1 d . . . . .
H4A H 0.311343 0.134747 0.594751 0.089 Uiso 1 1 calc R . . . .
C5A C 0.3940(8) 0.2096(8) 0.5523(4) 0.058(3) Uani 1 1 d . . . . .
C6A C 0.4514(8) 0.2687(8) 0.5855(4) 0.061(3) Uani 1 1 d . . . . .
C7A C 0.4371(8) 0.2613(8) 0.6313(4) 0.063(3) Uani 1 1 d . . . . .
H7A H 0.388799 0.218097 0.642334 0.06(3) Uiso 1 1 calc R . . . .
C8A C 0.4900(9) 0.3141(8) 0.6613(4) 0.070(4) Uani 1 1 d . . . . .
C9A C 0.5622(9) 0.3756(10) 0.6430(4) 0.077(4) Uani 1 1 d . U . . .
H9A H 0.601807 0.414222 0.662335 0.092 Uiso 1 1 calc R . . . .
C10A C 0.5743(9) 0.3786(9) 0.5969(5) 0.077(4) Uani 1 1 d . . . . .
H10A H 0.623447 0.419246 0.585024 0.092 Uiso 1 1 calc R . . . .
C1AA C 0.4725(9) 0.3110(8) 0.7120(4) 0.101(5) Uani 1 1 d D . . . .
N1B N 0.5265(5) 0.3399(6) 0.4327(4) 0.054(3) Uani 1 1 d . . . . .
N2B N 0.5215(6) 0.4375(7) 0.4925(3) 0.068(3) Uani 1 1 d . . . . .
C1B C 0.5303(9) 0.2905(9) 0.4039(4) 0.073(4) Uani 1 1 d . . . . .
H1B H 0.540813 0.251031 0.415549 0.08(4) Uiso 1 1 calc R . . . .
C2B C 0.5199(9) 0.2923(9) 0.3577(4) 0.078(4) Uani 1 1 d . . . . .
H2B H 0.520503 0.252947 0.338860 0.093 Uiso 1 1 calc R . . . .
C4B C 0.5083(8) 0.4062(8) 0.3697(4) 0.067(3) Uani 1 1 d . . . . .
H4B H 0.502499 0.448934 0.358538 0.080 Uiso 1 1 calc R . . . .
C5B C 0.5160(7) 0.3990(8) 0.4153(3) 0.059(3) Uani 1 1 d . . . . .
C6B C 0.5171(8) 0.4553(8) 0.4495(4) 0.064(3) Uani 1 1 d . . . . .
C7B C 0.5135(8) 0.5234(8) 0.4379(4) 0.067(3) Uani 1 1 d . . . . .
H7B H 0.510874 0.534484 0.406696 0.081 Uiso 1 1 calc R . . . .
C8B C 0.5138(8) 0.5743(9) 0.4699(5) 0.076(4) Uani 1 1 d . . . . .
C9B C 0.5228(9) 0.5573(10) 0.5136(5) 0.085(4) Uani 1 1 d . . . . .
H9B H 0.527379 0.592892 0.537119 0.102 Uiso 1 1 calc R . . . .
C10B C 0.5254(9) 0.4895(10) 0.5246(4) 0.083(4) Uani 1 1 d . . . . .
H10B H 0.530033 0.478967 0.555651 0.13(6) Uiso 1 1 calc R . . . .
O00E O 0.5986(5) 0.2723(5) 0.4997(3) 0.0639(5) Uani 1 1 d . U . . .
C00J C 0.1951(10) 0.0200(10) 0.5441(5) 0.119(6) Uani 1 1 d D . . . .
C00V C 0.666667 0.333333 0.5016(7) 0.061(5) Uani 1 3 d S TU P A .
C26 C 0.5090(13) 0.6484(11) 0.4569(5) 0.117(6) Uani 1 1 d D U . . .
C2 C 0.4933(9) 0.3558(7) 0.2879(4) 0.098(4) Uani 1 1 d D U . . .
P1 P 0.1826(8) 0.1818(8) 0.6680(5) 0.103(4) Uiso 0.3333 1 d D . . . .
P2 P 0.3346(4) 0.0547(3) 0.3335(2) 0.1203(17) Uiso 1 1 d D . . . .
F4 F 0.3655(13) 0.0604(11) 0.2809(3) 0.140(8) Uiso 0.5 1 d DG . . B 2
F5 F 0.2927(13) -0.0427(4) 0.3316(6) 0.139(8) Uiso 0.5 1 d DG . . B 1
CAD C 0.434(2) 0.2280(13) 0.7350(15) 0.15(2) Uani 0.5 1 d D U . C 1
HADA H 0.383182 0.192798 0.720381 0.228 Uiso 0.5 1 d R . . C 1
HADB H 0.426242 0.231458 0.767541 0.228 Uiso 0.5 1 d R . . C 1
HADC H 0.470112 0.206528 0.730531 0.228 Uiso 0.5 1 d R . . C 1
C5 C 0.505(2) 0.4372(12) 0.2744(11) 0.098(4) Uani 0.5 1 d D . . D 1
H5A H 0.466887 0.447177 0.290540 0.147 Uiso 0.5 1 d R . . D 1
H5B H 0.498297 0.439517 0.241600 0.147 Uiso 0.5 1 d R . . D 1
H5C H 0.559317 0.477617 0.282990 0.147 Uiso 0.5 1 d R . . D 1
C12 C 0.5089(9) 0.3503(8) 0.3388(4) 0.071(4) Uani 1 1 d D . . . .
C24 C 0.4036(10) 0.3253(16) 0.2817(9) 0.093(11) Uani 0.5 1 d D . . D 2
H24A H 0.389292 0.362291 0.295540 0.140 Uiso 0.5 1 d R . . D 2
H24B H 0.373132 0.273031 0.296100 0.140 Uiso 0.5 1 d R . . D 2
H24C H 0.391232 0.320421 0.249140 0.140 Uiso 0.5 1 d R . . D 2
C21 C 0.5532(15) 0.3388(17) 0.2643(10) 0.098(4) Uani 0.5 1 d D U . D 1
H21A H 0.532139 0.317896 0.234072 0.147 Uiso 0.5 1 d R . . D 1
H21B H 0.560069 0.299306 0.281382 0.147 Uiso 0.5 1 d R . . D 1
H21C H 0.604659 0.387786 0.261392 0.147 Uiso 0.5 1 d R . . D 1
C3BA C 0.5429(16) 0.4411(10) 0.2711(9) 0.088(10) Uani 0.5 1 d D U . D 2
H3BA H 0.525419 0.443163 0.240215 0.132 Uiso 0.5 1 d R . . D 2
H3BB H 0.599169 0.456103 0.270715 0.132 Uiso 0.5 1 d R . . D 2
H3BC H 0.535829 0.478023 0.290575 0.132 Uiso 0.5 1 d R . . D 2
C27 C 0.5453(14) 0.3686(15) 0.7424(9) 0.101(5) Uani 0.5 1 d D U . C 1
H27A H 0.592740 0.366112 0.733592 0.152 Uiso 0.5 1 d R . . C 1
H27B H 0.533360 0.353902 0.774502 0.152 Uiso 0.5 1 d R . . C 1
H27C H 0.555120 0.422732 0.737912 0.152 Uiso 0.5 1 d R . . C 1
C1 C 0.4117(17) 0.341(2) 0.7149(9) 0.112(13) Uani 0.5 1 d D U . C 1
H1C H 0.425840 0.385090 0.693655 0.168 Uiso 0.5 1 d R . . C 1
H1D H 0.413070 0.359670 0.746035 0.168 Uiso 0.5 1 d R . . C 1
H1E H 0.358180 0.297530 0.707995 0.168 Uiso 0.5 1 d R . . C 1
F12 F 0.1395(16) 0.2342(15) 0.6691(9) 0.102(8) Uiso 0.3333 1 d D . . G .
C8AA C 0.2713(8) 0.0903(8) 0.5306(4) 0.076(4) Uani 1 1 d D . . . .
F3AA F 0.3144(16) 0.1230(15) 0.3191(10) 0.172(10) Uiso 0.5 1 d D . . B 2
F4AA F 0.2995(19) 0.0386(19) 0.3835(6) 0.204(8) Uiso 0.5 1 d D . . B 2
F13 F 0.4200(13) 0.1225(15) 0.3542(13) 0.248(18) Uiso 0.5 1 d D . . B 2
F17 F 0.2731(16) 0.0464(18) 0.2943(9) 0.204(8) Uiso 0.5 1 d D . . B 1
C28 C 0.4206(17) 0.620(2) 0.446(2) 0.19(2) Uani 0.5 1 d D U . E 1
H28A H 0.381846 0.577832 0.425713 0.292 Uiso 0.5 1 d R . . E 1
H28B H 0.415906 0.667322 0.442783 0.292 Uiso 0.5 1 d R . . E 1
H28C H 0.410216 0.600982 0.477263 0.292 Uiso 0.5 1 d R . . E 1
C4 C 0.4029(18) 0.2281(13) 0.7256(11) 0.101(5) Uani 0.5 1 d D U . C 2
H4C H 0.353512 0.222210 0.713013 0.152 Uiso 0.5 1 d R . . C 2
H4D H 0.398912 0.223990 0.758763 0.152 Uiso 0.5 1 d R . . C 2
H4E H 0.411732 0.186160 0.713473 0.152 Uiso 0.5 1 d R . . C 2
C2AA C 0.5468(15) 0.3278(18) 0.7405(10) 0.101(5) Uani 0.5 1 d D U . C 2
H2AA H 0.564626 0.289312 0.735753 0.152 Uiso 0.5 1 d R . . C 2
H2AB H 0.530825 0.325892 0.772323 0.152 Uiso 0.5 1 d R . . C 2
H2AC H 0.590166 0.381372 0.733413 0.152 Uiso 0.5 1 d R . . C 2
C32 C 0.4076(13) 0.2915(16) 0.2788(11) 0.098(4) Uani 0.5 1 d D . . D 1
H32A H 0.403243 0.239092 0.279896 0.147 Uiso 0.5 1 d R . . D 1
H32B H 0.389813 0.299262 0.249096 0.147 Uiso 0.5 1 d R . . D 1
H32C H 0.374213 0.295042 0.302666 0.147 Uiso 0.5 1 d R . . D 1
C1BA C 0.207(3) -0.053(2) 0.5517(18) 0.119(6) Uani 0.3333 1 d D . . F 1
H1BA H 0.201378 -0.082684 0.523691 0.178 Uiso 0.3333 1 d R . . F 1
H1BB H 0.164408 -0.087014 0.572901 0.178 Uiso 0.3333 1 d R . . F 1
H1BC H 0.258598 -0.036774 0.565601 0.178 Uiso 0.3333 1 d R . . F 1
C5AA C 0.151(3) -0.041(2) 0.5052(12) 0.119(6) Uani 0.3333 1 d D . . F 3
H5AA H 0.152001 -0.090195 0.512002 0.178 Uiso 0.3333 1 d R . . F 3
H5AB H 0.182641 -0.016505 0.477882 0.178 Uiso 0.3333 1 d R . . F 3
H5AC H 0.096151 -0.053895 0.500152 0.178 Uiso 0.3333 1 d R . . F 3
C4BA C 0.196(3) -0.054(2) 0.5233(16) 0.119(6) Uani 0.3333 1 d D . . F 2
H4BA H 0.241443 -0.055762 0.536716 0.178 Uiso 0.3333 1 d R . . F 2
H4BB H 0.202533 -0.048762 0.490266 0.178 Uiso 0.3333 1 d R . . F 2
H4BC H 0.146893 -0.103252 0.530716 0.178 Uiso 0.3333 1 d R . . F 2
C7AA C 0.450(2) 0.3751(17) 0.7250(11) 0.101(5) Uani 0.5 1 d D U . C 2
H7AA H 0.497127 0.428453 0.722901 0.152 Uiso 0.5 1 d R . . C 2
H7AB H 0.429407 0.365753 0.756031 0.152 Uiso 0.5 1 d R . . C 2
H7AC H 0.409527 0.370803 0.703781 0.152 Uiso 0.5 1 d R . . C 2
F6AA F 0.2603(14) 0.0305(17) 0.3678(10) 0.192(10) Uiso 0.5 1 d D . . B 1
F7AA F 0.4049(12) 0.1109(15) 0.2989(7) 0.159(9) Uiso 0.5 1 d D . . B 1
C6BA C 0.5142(18) 0.3015(15) 0.2601(10) 0.098(4) Uani 0.5 1 d D . . D 2
H6BA H 0.502191 0.299928 0.227612 0.147 Uiso 0.5 1 d R . . D 2
H6BB H 0.482731 0.248128 0.273022 0.147 Uiso 0.5 1 d R . . D 2
H6BC H 0.570861 0.320018 0.264042 0.147 Uiso 0.5 1 d R . . D 2
C0CA C 0.128(3) -0.007(3) 0.5075(14) 0.119(6) Uani 0.3333 1 d D . . F 1
H0CA H 0.106625 0.029023 0.508146 0.178 Uiso 0.3333 1 d R . . F 1
H0CB H 0.085075 -0.061707 0.512776 0.178 Uiso 0.3333 1 d R . . F 1
H0CC H 0.152295 -0.003877 0.477796 0.178 Uiso 0.3333 1 d R . . F 1
F3BA F 0.3454(16) 0.1406(11) 0.3498(9) 0.167(10) Uiso 0.5 1 d D . . B 1
F8AA F 0.3757(16) -0.0044(13) 0.3379(8) 0.148(9) Uiso 0.5 1 d D . . B 2
F31 F 0.2455(12) 0.006(2) 0.3128(9) 0.204(8) Uiso 0.5 1 d D . . B 2
C17 C 0.5904(18) 0.726(2) 0.4614(18) 0.178(19) Uani 0.5 1 d D U . E 2
H17A H 0.588278 0.774100 0.453291 0.267 Uiso 0.5 1 d R . . E 2
H17B H 0.602859 0.705280 0.434251 0.267 Uiso 0.5 1 d R . . E 2
H17C H 0.631798 0.739650 0.484351 0.267 Uiso 0.5 1 d R . . E 2
C4AA C 0.205(3) -0.025(3) 0.5844(14) 0.119(6) Uani 0.3333 1 d D . . F 3
H4AA H 0.233317 -0.052962 0.575617 0.178 Uiso 0.3333 1 d R . . F 3
H4AB H 0.152307 -0.063492 0.596147 0.178 Uiso 0.3333 1 d R . . F 3
H4AC H 0.235247 0.014048 0.608137 0.178 Uiso 0.3333 1 d R . . F 3
C18 C 0.131(3) 0.031(3) 0.5188(16) 0.119(6) Uani 0.3333 1 d D . . F 2
H18A H 0.127411 0.075640 0.531404 0.178 Uiso 0.3333 1 d R . . F 2
H18B H 0.079481 -0.018160 0.522344 0.178 Uiso 0.3333 1 d R . . F 2
H18C H 0.144561 0.040160 0.486484 0.178 Uiso 0.3333 1 d R . . F 2
C30 C 0.535(4) 0.709(3) 0.4963(13) 0.22(3) Uani 0.5 1 d D U . E 1
H30A H 0.546615 0.759241 0.481672 0.331 Uiso 0.5 1 d R . . E 1
H30B H 0.581525 0.702221 0.493792 0.331 Uiso 0.5 1 d R . . E 1
H30C H 0.522705 0.710791 0.528432 0.331 Uiso 0.5 1 d R . . E 1
C9 C 0.561(3) 0.691(2) 0.4159(14) 0.16(2) Uani 0.5 1 d D U . E 1
H9C H 0.616473 0.712228 0.405806 0.239 Uiso 0.5 1 d R . . E 1
H9D H 0.545533 0.731068 0.411036 0.239 Uiso 0.5 1 d R . . E 1
H9E H 0.526423 0.643128 0.398326 0.239 Uiso 0.5 1 d R . . E 1
C6 C 0.449(2) 0.655(2) 0.4883(12) 0.117(6) Uani 0.5 1 d D U . E 2
H6A H 0.498900 0.700532 0.498938 0.176 Uiso 0.5 1 d R . . E 2
H6B H 0.428360 0.613713 0.512108 0.176 Uiso 0.5 1 d R . . E 2
H6C H 0.410380 0.671043 0.481548 0.176 Uiso 0.5 1 d R . . E 2
C13 C 0.480(3) 0.640(3) 0.4075(9) 0.18(2) Uani 0.5 1 d D U . E 2
H13A H 0.489151 0.613849 0.381752 0.274 Uiso 0.5 1 d R . . E 2
H13B H 0.477231 0.686449 0.396682 0.274 Uiso 0.5 1 d R . . E 2
H13C H 0.428981 0.602539 0.421992 0.274 Uiso 0.5 1 d R . . E 2
C0AA C 0.170(3) 0.000(3) 0.5948(8) 0.119(6) Uani 0.3333 1 d D . . F 2
H0AA H 0.185121 0.049860 0.610194 0.178 Uiso 0.3333 1 d R . . F 2
H0AB H 0.200411 -0.023730 0.607704 0.178 Uiso 0.3333 1 d R . . F 2
H0AC H 0.113211 -0.037250 0.598904 0.178 Uiso 0.3333 1 d R . . F 2
C16 C 0.140(3) 0.053(3) 0.5601(16) 0.119(6) Uani 0.3333 1 d D . . F 3
H16A H 0.110576 0.029035 0.588348 0.178 Uiso 0.3333 1 d R . . F 3
H16B H 0.101596 0.040435 0.535238 0.178 Uiso 0.3333 1 d R . . F 3
H16C H 0.171896 0.110505 0.563758 0.178 Uiso 0.3333 1 d R . . F 3
C19 C 0.162(3) 0.034(3) 0.5896(11) 0.119(6) Uani 0.3333 1 d D . . F 1
H19A H 0.113159 -0.014264 0.599505 0.178 Uiso 0.3333 1 d R . . F 1
H19B H 0.149649 0.076026 0.583295 0.178 Uiso 0.3333 1 d R . . F 1
H19C H 0.201749 0.050866 0.613775 0.178 Uiso 0.3333 1 d R . . F 1
F2AA F 0.101(2) 0.098(2) 0.675(2) 0.100 Uiso 0.1667 1 d D U . G 1
F0AA F 0.170(4) 0.172(4) 0.6135(8) 0.100 Uiso 0.1667 1 d D U . G 1
F20 F 0.262(2) 0.268(2) 0.6583(17) 0.100 Uiso 0.1667 1 d D U . G 1
F8 F 0.204(3) 0.200(3) 0.7217(9) 0.100 Uiso 0.1667 1 d D U . G 1
F18 F 0.2368(19) 0.142(2) 0.6652(10) 0.134(11) Uiso 0.3333 1 d D . . G .
F20A F 0.245(3) 0.255(3) 0.6996(16) 0.100 Uiso 0.1667 1 d D . . G 2
F0AB F 0.223(3) 0.223(3) 0.6199(12) 0.100 Uiso 0.1667 1 d D . . G 2
F2AB F 0.107(2) 0.111(3) 0.6436(14) 0.100 Uiso 0.1667 1 d D . . G 2
F8A F 0.144(3) 0.149(3) 0.7176(9) 0.100 Uiso 0.1667 1 d D . . G 2
F2 F 0.3947(15) 0.0690(18) 0.3716(7) 0.192(10) Uiso 0.5 1 d D . . B 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 0.0714(10) 0.0830(11) 0.0405(7) 0.0027(7) 0.0020(7) 0.0411(9)
N1A 0.062(6) 0.094(8) 0.049(6) -0.011(6) -0.003(5) 0.045(6)
N2A 0.066(8) 0.076(8) 0.058(9) 0.003(6) 0.007(6) 0.032(6)
C1A 0.074(10) 0.116(13) 0.049(8) -0.009(8) -0.009(7) 0.031(10)
C2A 0.105(13) 0.128(14) 0.060(9) -0.030(9) -0.031(8) 0.078(12)
C4A 0.078(10) 0.090(10) 0.050(7) 0.002(7) -0.009(7) 0.039(9)
C5A 0.078(9) 0.067(8) 0.035(6) -0.006(5) -0.005(6) 0.040(7)
C6A 0.070(8) 0.070(8) 0.046(7) -0.006(6) -0.014(6) 0.037(7)
C7A 0.074(9) 0.076(9) 0.033(6) 0.002(6) 0.003(6) 0.034(8)
C8A 0.078(10) 0.054(8) 0.051(8) 0.002(6) -0.010(7) 0.013(7)
C9A 0.087(10) 0.100(11) 0.048(8) -0.021(8) -0.025(7) 0.051(9)
C10A 0.072(9) 0.076(10) 0.065(10) 0.003(7) -0.008(7) 0.025(8)
C1AA 0.144(12) 0.095(9) 0.042(6) -0.015(6) -0.014(6) 0.042(8)
N1B 0.059(7) 0.058(6) 0.044(7) 0.006(5) 0.002(4) 0.028(5)
N2B 0.075(7) 0.097(8) 0.044(6) 0.001(5) 0.006(5) 0.052(7)
C1B 0.096(11) 0.077(9) 0.048(8) -0.001(7) 0.009(7) 0.046(8)
C2B 0.113(12) 0.062(8) 0.054(9) 0.006(7) 0.023(7) 0.040(9)
C4B 0.079(9) 0.068(8) 0.052(7) 0.005(6) -0.008(6) 0.035(7)
C5B 0.061(8) 0.086(9) 0.032(6) -0.006(6) 0.001(5) 0.038(7)
C6B 0.071(8) 0.082(9) 0.042(7) -0.003(6) 0.002(6) 0.042(7)
C7B 0.093(10) 0.075(9) 0.042(7) 0.003(6) 0.012(6) 0.047(8)
C8B 0.071(9) 0.089(10) 0.062(8) 0.000(7) 0.016(7) 0.036(8)
C9B 0.097(11) 0.092(11) 0.065(10) -0.016(8) 0.025(8) 0.047(9)
C10B 0.110(12) 0.113(13) 0.044(8) -0.007(8) 0.010(7) 0.070(11)
O00E 0.0714(10) 0.0830(11) 0.0405(7) 0.0027(7) 0.0020(7) 0.0411(9)
C00J 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
C00V 0.062(6) 0.062(6) 0.059(12) 0.000 0.000 0.031(3)
C26 0.173(16) 0.104(11) 0.101(9) 0.009(9) 0.047(11) 0.089(12)
C2 0.147(13) 0.082(7) 0.046(6) -0.007(5) -0.007(6) 0.043(8)
CAD 0.15(4) 0.07(2) 0.16(4) 0.03(2) -0.08(3) 0.00(2)
C5 0.147(13) 0.082(7) 0.046(6) -0.007(5) -0.007(6) 0.043(8)
C12 0.098(11) 0.068(9) 0.037(7) 0.004(6) 0.000(7) 0.034(9)
C24 0.15(3) 0.07(2) 0.061(17) -0.008(16) -0.015(18) 0.05(2)
C21 0.147(13) 0.082(7) 0.046(6) -0.007(5) -0.007(6) 0.043(8)
C3BA 0.12(3) 0.099(16) 0.051(15) 0.023(14) 0.038(18) 0.063(18)
C27 0.144(12) 0.095(9) 0.042(6) -0.015(6) -0.014(6) 0.042(8)
C1 0.12(3) 0.16(4) 0.042(16) -0.044(19) -0.011(17) 0.05(3)
C8AA 0.085(10) 0.080(9) 0.063(8) -0.016(7) -0.041(7) 0.041(8)
C28 0.17(2) 0.08(3) 0.37(8) 0.00(3) 0.03(3) 0.10(3)
C4 0.144(12) 0.095(9) 0.042(6) -0.015(6) -0.014(6) 0.042(8)
C2AA 0.144(12) 0.095(9) 0.042(6) -0.015(6) -0.014(6) 0.042(8)
C32 0.147(13) 0.082(7) 0.046(6) -0.007(5) -0.007(6) 0.043(8)
C1BA 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
C5AA 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
C4BA 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
C7AA 0.144(12) 0.095(9) 0.042(6) -0.015(6) -0.014(6) 0.042(8)
C6BA 0.147(13) 0.082(7) 0.046(6) -0.007(5) -0.007(6) 0.043(8)
C0CA 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
C17 0.19(3) 0.11(3) 0.22(5) 0.02(3) 0.10(3) 0.066(19)
C4AA 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
C18 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
C30 0.43(8) 0.18(4) 0.19(3) -0.08(3) -0.05(4) 0.25(5)
C9 0.24(5) 0.08(3) 0.19(4) 0.07(2) 0.12(4) 0.10(3)
C6 0.173(16) 0.104(11) 0.101(9) 0.009(9) 0.047(11) 0.089(12)
C13 0.39(7) 0.15(4) 0.097(16) 0.01(2) 0.02(3) 0.20(5)
C0AA 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
C16 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
C19 0.101(9) 0.093(9) 0.119(10) 0.024(9) -0.048(8) 0.016(8)
_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
Cu1 N1A 2.115(11) . ?
Cu1 N2A 1.987(14) . ?
Cu1 N1B 1.996(12) . ?
Cu1 N2B 2.111(11) . ?
Cu1 O00E 2.206(9) . ?
N1A C1A 1.331(17) . ?
N1A C5A 1.380(14) . ?
N2A C6A 1.341(17) . ?
N2A C10A 1.350(19) . ?
C1A C2A 1.36(2) . ?
C2A C8AA 1.38(2) . ?
C4A C5A 1.341(18) . ?
C4A C8AA 1.429(18) . ?
C5A C6A 1.495(16) . ?
C6A C7A 1.370(16) . ?
C7A C8A 1.353(17) . ?
C8A C9A 1.42(2) . ?
C8A C1AA 1.526(19) . ?
C9A C10A 1.373(18) . ?
C1AA CAD 1.554(18) . ?
C1AA C27 1.573(17) . ?
C1AA C1 1.559(16) . ?
C1AA C4 1.549(18) . ?
C1AA C2AA 1.557(18) . ?
C1AA C7AA 1.553(18) . ?
N1B C1B 1.310(17) . ?
N1B C5B 1.363(16) . ?
N2B C6B 1.327(15) . ?
N2B C10B 1.358(17) . ?
C1B C2B 1.377(18) . ?
C2B C12 1.37(2) . ?
C4B C5B 1.367(16) . ?
C4B C12 1.420(19) . ?
C5B C6B 1.478(17) . ?
C6B C7B 1.400(17) . ?
C7B C8B 1.366(18) . ?
C8B C9B 1.36(2) . ?
C8B C26 1.54(2) . ?
C9B C10B 1.38(2) . ?
O00E C00V 1.260(9) . ?
C00J C8AA 1.481(18) . ?
C00J C1BA 1.563(19) . ?
C00J C5AA 1.561(19) . ?
C00J C4BA 1.573(19) . ?
C00J C0CA 1.563(19) . ?
C00J C4AA 1.545(19) . ?
C00J C18 1.553(19) . ?
C00J C0AA 1.56(2) . ?
C00J C16 1.57(2) . ?
C00J C19 1.57(2) . ?
C26 C28 1.55(2) . ?
C26 C17 1.553(19) . ?
C26 C30 1.548(19) . ?
C26 C9 1.530(19) . ?
C26 C6 1.532(19) . ?
C26 C13 1.542(19) . ?
C2 C5 1.532(15) . ?
C2 C12 1.540(15) . ?
C2 C24 1.546(14) . ?
C2 C21 1.525(15) . ?
C2 C3BA 1.524(14) . ?
C2 C32 1.524(18) . ?
C2 C6BA 1.541(17) . ?
P1 F12 1.609(16) . ?
P1 F2AA 1.620(18) . ?
P1 F0AA 1.620(18) . ?
P1 F20 1.64(2) . ?
P1 F8 1.62(2) . ?
P1 F18 1.59(2) . ?
P1 F20A 1.62(2) . ?
P1 F0AB 1.62(2) . ?
P1 F2AB 1.60(2) . ?
P1 F8A 1.62(2) . ?
P2 F4 1.6449 . ?
P2 F5 1.6448 . ?
P2 F3AA 1.617(13) . ?
P2 F4AA 1.585(15) . ?
P2 F13 1.634(14) . ?
P2 F17 1.611(14) . ?
P2 F6AA 1.627(13) . ?
P2 F7AA 1.613(14) . ?
P2 F3BA 1.647(15) . ?
P2 F8AA 1.698(19) . ?
P2 F31 1.62(2) . ?
P2 F2 1.539(17) . ?
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
N1A Cu1 O00E 95.5(4) . . ?
N2A Cu1 N1A 79.8(4) . . ?
N2A Cu1 N2B 97.4(4) . . ?
N2A Cu1 O00E 91.7(4) . . ?
N1B Cu1 N1A 96.9(4) . . ?
N1B Cu1 N2A 174.1(4) . . ?
N1B Cu1 N2B 79.4(4) . . ?
N1B Cu1 O00E 93.6(4) . . ?
N2B Cu1 N1A 114.1(4) . . ?
N2B Cu1 O00E 150.0(4) . . ?
C1A N1A Cu1 130.3(9) . . ?
C1A N1A C5A 116.6(12) . . ?
C5A N1A Cu1 112.9(8) . . ?
C6A N2A Cu1 117.5(10) . . ?
C6A N2A C10A 117.1(14) . . ?
C10A N2A Cu1 125.2(10) . . ?
N1A C1A C2A 123.1(13) . . ?
C1A C2A C8AA 123.2(14) . . ?
C5A C4A C8AA 123.0(12) . . ?
N1A C5A C6A 113.8(11) . . ?
C4A C5A N1A 121.4(11) . . ?
C4A C5A C6A 124.8(11) . . ?
N2A C6A C5A 115.5(12) . . ?
N2A C6A C7A 122.4(12) . . ?
C7A C6A C5A 121.9(12) . . ?
C8A C7A C6A 121.7(13) . . ?
C7A C8A C9A 116.5(12) . . ?
C7A C8A C1AA 122.6(13) . . ?
C9A C8A C1AA 120.8(11) . . ?
C10A C9A C8A 119.2(12) . . ?
N2A C10A C9A 122.9(14) . . ?
C8A C1AA CAD 117(2) . . ?
C8A C1AA C27 115.2(16) . . ?
C8A C1AA C1 103.5(15) . . ?
C8A C1AA C4 110.8(15) . . ?
C8A C1AA C2AA 110.8(16) . . ?
C8A C1AA C7AA 110.7(16) . . ?
CAD C1AA C27 106.4(14) . . ?
C1 C1AA CAD 108.0(18) . . ?
C1 C1AA C27 106.4(14) . . ?
C4 C1AA C2AA 108.3(15) . . ?
C4 C1AA C7AA 108.8(17) . . ?
C7AA C1AA C2AA 107.3(14) . . ?
C1B N1B Cu1 126.1(9) . . ?
C1B N1B C5B 117.4(12) . . ?
C5B N1B Cu1 116.5(8) . . ?
C6B N2B Cu1 113.4(8) . . ?
C6B N2B C10B 117.3(12) . . ?
C10B N2B Cu1 129.2(9) . . ?
N1B C1B C2B 123.9(14) . . ?
C12 C2B C1B 120.7(13) . . ?
C5B C4B C12 120.5(12) . . ?
N1B C5B C4B 121.8(11) . . ?
N1B C5B C6B 114.5(10) . . ?
C4B C5B C6B 123.6(12) . . ?
N2B C6B C5B 115.8(11) . . ?
N2B C6B C7B 121.2(11) . . ?
C7B C6B C5B 123.0(10) . . ?
C8B C7B C6B 122.1(11) . . ?
C7B C8B C9B 115.5(14) . . ?
C7B C8B C26 121.8(12) . . ?
C9B C8B C26 122.6(14) . . ?
C10B C9B C8B 121.6(13) . . ?
N2B C10B C9B 122.0(13) . . ?
C00V O00E Cu1 97.8(5) . . ?
C8AA C00J C1BA 110(2) . . ?
C8AA C00J C5AA 115(2) . . ?
C8AA C00J C4BA 106(2) . . ?
C8AA C00J C0CA 114(2) . . ?
C8AA C00J C4AA 112(2) . . ?
C8AA C00J C18 104(2) . . ?
C8AA C00J C0AA 122(2) . . ?
C8AA C00J C16 106(2) . . ?
C8AA C00J C19 112(2) . . ?
C1BA C00J C19 106.9(18) . . ?
C5AA C00J C16 107.7(19) . . ?
C0CA C00J C1BA 105.5(18) . . ?
C0CA C00J C19 108(2) . . ?
C4AA C00J C5AA 107.9(19) . . ?
C4AA C00J C16 107.7(19) . . ?
C18 C00J C4BA 108.4(18) . . ?
C18 C00J C0AA 109.0(19) . . ?
C0AA C00J C4BA 106.5(18) . . ?
O00E C00V O00E 119.80(17) . 3_665 ?
O00E C00V O00E 119.80(17) 2_655 . ?
O00E C00V O00E 119.80(17) 2_655 3_665 ?
C8B C26 C28 106.8(19) . . ?
C8B C26 C17 112(2) . . ?
C8B C26 C30 112(2) . . ?
C30 C26 C28 108.4(18) . . ?
C9 C26 C8B 111.6(17) . . ?
C9 C26 C28 110.1(19) . . ?
C9 C26 C30 107.7(19) . . ?
C6 C26 C8B 108.9(18) . . ?
C6 C26 C17 108.4(17) . . ?
C6 C26 C13 108.8(19) . . ?
C13 C26 C8B 109.1(19) . . ?
C13 C26 C17 109.1(19) . . ?
C12 C2 C5 112.9(16) . . ?
C12 C2 C24 108.2(13) . . ?
C21 C2 C5 111.5(13) . . ?
C21 C2 C12 103.4(15) . . ?
C3BA C2 C12 110.5(13) . . ?
C3BA C2 C24 110.9(13) . . ?
C3BA C2 C6BA 109.4(14) . . ?
C32 C2 C5 109.8(16) . . ?
C32 C2 C12 106.6(16) . . ?
C32 C2 C21 112.5(15) . . ?
C6BA C2 C12 110.0(15) . . ?
C6BA C2 C24 107.8(14) . . ?
F12 P1 F2AA 94(2) . . ?
F12 P1 F0AA 90(2) . . ?
F12 P1 F20 83(2) . . ?
F12 P1 F8 90(2) . . ?
F12 P1 F20A 81(2) . . ?
F12 P1 F0AB 89(2) . . ?
F12 P1 F8A 87(2) . . ?
F2AA P1 F0AA 90(3) . . ?
F2AA P1 F20 176(3) . . ?
F0AA P1 F20 87(3) . . ?
F8 P1 F2AA 96(3) . . ?
F8 P1 F0AA 174(3) . . ?
F8 P1 F20 87(2) . . ?
F18 P1 F12 171.7(17) . . ?
F18 P1 F2AA 94(3) . . ?
F18 P1 F0AA 89.2(19) . . ?
F18 P1 F20 89(3) . . ?
F18 P1 F8 90(2) . . ?
F18 P1 F20A 94(2) . . ?
F18 P1 F0AB 85(2) . . ?
F18 P1 F2AB 96(2) . . ?
F18 P1 F8A 98(2) . . ?
F20A P1 F0AB 96(3) . . ?
F2AB P1 F12 90(2) . . ?
F2AB P1 F20A 168(3) . . ?
F2AB P1 F0AB 92(3) . . ?
F2AB P1 F8A 91.3(17) . . ?
F8A P1 F20A 80(3) . . ?
F8A P1 F0AB 175(3) . . ?
F4 P2 F8AA 80.7(9) . . ?
F3AA P2 F4 85.9(12) . . ?
F3AA P2 F8AA 164.4(13) . . ?
F4AA P2 F4 173.5(14) . . ?
F4AA P2 F3AA 98.5(12) . . ?
F4AA P2 F13 88.6(17) . . ?
F4AA P2 F8AA 95.6(14) . . ?
F13 P2 F4 96.2(16) . . ?
F13 P2 F3AA 90.0(11) . . ?
F13 P2 F8AA 83.5(11) . . ?
F17 P2 F5 86.8(12) . . ?
F17 P2 F6AA 84.8(17) . . ?
F17 P2 F7AA 87.1(13) . . ?
F17 P2 F3BA 91.3(13) . . ?
F6AA P2 F5 80.3(11) . . ?
F6AA P2 F7AA 156.3(13) . . ?
F6AA P2 F3BA 75.9(11) . . ?
F7AA P2 F5 121.5(11) . . ?
F7AA P2 F3BA 82.1(12) . . ?
F3BA P2 F5 156.2(11) . . ?
F31 P2 F4 86.0(11) . . ?
F31 P2 F3AA 76.0(19) . . ?
F31 P2 F4AA 90.3(12) . . ?
F31 P2 F13 165.7(18) . . ?
F31 P2 F8AA 110.8(17) . . ?
F2 P2 F5 97.3(12) . . ?
F2 P2 F17 175.7(15) . . ?
F2 P2 F6AA 94.8(14) . . ?
F2 P2 F7AA 91.7(11) . . ?
F2 P2 F3BA 84.5(13) . . ?
C2B C12 C4B 115.6(11) . . ?
C2B C12 C2 124.7(12) . . ?
C4B C12 C2 119.6(12) . . ?
C2A C8AA C4A 112.5(14) . . ?
C2A C8AA C00J 125.8(14) . . ?
C4A C8AA C00J 121.7(13) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_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 N1A C1A C2A 179.4(11) . . . . ?
Cu1 N1A C5A C4A -179.6(10) . . . . ?
Cu1 N1A C5A C6A 2.0(13) . . . . ?
Cu1 N2A C6A C5A 7.6(15) . . . . ?
Cu1 N2A C6A C7A -176.1(9) . . . . ?
Cu1 N2A C10A C9A 173.7(11) . . . . ?
Cu1 N1B C1B C2B 172.4(11) . . . . ?
Cu1 N1B C5B C4B -175.4(9) . . . . ?
Cu1 N1B C5B C6B 6.9(13) . . . . ?
Cu1 N2B C6B C5B 1.2(14) . . . . ?
Cu1 N2B C6B C7B -178.9(10) . . . . ?
Cu1 N2B C10B C9B 177.6(11) . . . . ?
Cu1 O00E C00V O00E -176.4(16) . . . 2_655 ?
Cu1 O00E C00V O00E -5(2) . . . 3_665 ?
N1A C1A C2A C8AA -3(3) . . . . ?
N1A C5A C6A N2A -6.2(16) . . . . ?
N1A C5A C6A C7A 177.5(11) . . . . ?
N2A C6A C7A C8A 3(2) . . . . ?
C1A N1A C5A C4A -4.6(19) . . . . ?
C1A N1A C5A C6A 177.0(12) . . . . ?
C1A C2A C8AA C4A -1(2) . . . . ?
C1A C2A C8AA C00J 179.8(16) . . . . ?
C4A C5A C6A N2A 175.5(13) . . . . ?
C4A C5A C6A C7A -1(2) . . . . ?
C5A N1A C1A C2A 5(2) . . . . ?
C5A C4A C8AA C2A 2(2) . . . . ?
C5A C4A C8AA C00J -179.0(15) . . . . ?
C5A C6A C7A C8A 178.7(13) . . . . ?
C6A N2A C10A C9A -1(2) . . . . ?
C6A C7A C8A C9A -2(2) . . . . ?
C6A C7A C8A C1AA 175.0(13) . . . . ?
C7A C8A C9A C10A 0(2) . . . . ?
C7A C8A C1AA CAD 45(2) . . . . ?
C7A C8A C1AA C27 171.0(16) . . . . ?
C7A C8A C1AA C1 -73.3(19) . . . . ?
C7A C8A C1AA C4 19(2) . . . . ?
C7A C8A C1AA C2AA 138.7(17) . . . . ?
C7A C8A C1AA C7AA -102.3(19) . . . . ?
C8A C9A C10A N2A 1(2) . . . . ?
C9A C8A C1AA CAD -137.6(19) . . . . ?
C9A C8A C1AA C27 -12(2) . . . . ?
C9A C8A C1AA C1 103.9(19) . . . . ?
C9A C8A C1AA C4 -164.3(19) . . . . ?
C9A C8A C1AA C2AA -44(2) . . . . ?
C9A C8A C1AA C7AA 75(2) . . . . ?
C10A N2A C6A C5A -177.0(11) . . . . ?
C10A N2A C6A C7A -0.8(19) . . . . ?
C1AA C8A C9A C10A -177.0(14) . . . . ?
N1B C1B C2B C12 3(2) . . . . ?
N1B C5B C6B N2B -5.3(16) . . . . ?
N1B C5B C6B C7B 174.8(12) . . . . ?
N2B C6B C7B C8B -1(2) . . . . ?
C1B N1B C5B C4B 1.1(18) . . . . ?
C1B N1B C5B C6B -176.6(11) . . . . ?
C1B C2B C12 C4B 0(2) . . . . ?
C1B C2B C12 C2 -177.3(14) . . . . ?
C4B C5B C6B N2B 177.1(12) . . . . ?
C4B C5B C6B C7B -3(2) . . . . ?
C5B N1B C1B C2B -4(2) . . . . ?
C5B C4B C12 C2B -2(2) . . . . ?
C5B C4B C12 C2 175.1(12) . . . . ?
C5B C6B C7B C8B 179.3(13) . . . . ?
C6B N2B C10B C9B 2(2) . . . . ?
C6B C7B C8B C9B 4(2) . . . . ?
C6B C7B C8B C26 -179.4(14) . . . . ?
C7B C8B C9B C10B -5(2) . . . . ?
C7B C8B C26 C28 78(3) . . . . ?
C7B C8B C26 C17 -104(2) . . . . ?
C7B C8B C26 C30 -163(3) . . . . ?
C7B C8B C26 C9 -42(3) . . . . ?
C7B C8B C26 C6 135(2) . . . . ?
C7B C8B C26 C13 17(3) . . . . ?
C8B C9B C10B N2B 2(2) . . . . ?
C9B C8B C26 C28 -105(3) . . . . ?
C9B C8B C26 C17 72(2) . . . . ?
C9B C8B C26 C30 13(3) . . . . ?
C9B C8B C26 C9 134(3) . . . . ?
C9B C8B C26 C6 -48(2) . . . . ?
C9B C8B C26 C13 -167(3) . . . . ?
C10B N2B C6B C5B 177.8(12) . . . . ?
C10B N2B C6B C7B -2.4(19) . . . . ?
C26 C8B C9B C10B 178.8(15) . . . . ?
C5 C2 C12 C2B -164.7(18) . . . . ?
C5 C2 C12 C4B 19(2) . . . . ?
C12 C4B C5B N1B 1.7(19) . . . . ?
C12 C4B C5B C6B 179.1(12) . . . . ?
C24 C2 C12 C2B 102.4(18) . . . . ?
C24 C2 C12 C4B -74.4(16) . . . . ?
C21 C2 C12 C2B -44.0(19) . . . . ?
C21 C2 C12 C4B 139.2(15) . . . . ?
C3BA C2 C12 C2B -136.1(17) . . . . ?
C3BA C2 C12 C4B 47.2(18) . . . . ?
C8AA C4A C5A N1A 1(2) . . . . ?
C8AA C4A C5A C6A 179.2(12) . . . . ?
C32 C2 C12 C2B 75(2) . . . . ?
C32 C2 C12 C4B -102.1(17) . . . . ?
C1BA C00J C8AA C2A 88(2) . . . . ?
C1BA C00J C8AA C4A -91(2) . . . . ?
C5AA C00J C8AA C2A 10(3) . . . . ?
C5AA C00J C8AA C4A -169(2) . . . . ?
C4BA C00J C8AA C2A 55(2) . . . . ?
C4BA C00J C8AA C4A -124(2) . . . . ?
C6BA C2 C12 C2B -15(2) . . . . ?
C6BA C2 C12 C4B 168.1(15) . . . . ?
C0CA C00J C8AA C2A -30(3) . . . . ?
C0CA C00J C8AA C4A 151(2) . . . . ?
C4AA C00J C8AA C2A 134(3) . . . . ?
C4AA C00J C8AA C4A -46(3) . . . . ?
C18 C00J C8AA C2A -59(3) . . . . ?
C18 C00J C8AA C4A 122(2) . . . . ?
C0AA C00J C8AA C2A 177(3) . . . . ?
C0AA C00J C8AA C4A -2(3) . . . . ?
C16 C00J C8AA C2A -109(2) . . . . ?
C16 C00J C8AA C4A 72(2) . . . . ?
C19 C00J C8AA C2A -153(2) . . . . ?
C19 C00J C8AA C4A 28(3) . . . . ?
_shelx_res_file
;
TITL Bishwanath_27Sept16_Cu_0m_a.res in R3
bishwanath_27sept16_cu_0m_a.res
created by SHELXL-2016/6 at 15:47:33 on 22-Oct-2018
REM Old TITL Bishwanath_27Sept16_Cu_0m in R3
REM SHELXT solution in R3
REM R1 0.229, Rweak 0.067, Alpha 0.012, Orientation as input
REM Flack x = 0.225 ( 0.016 ) from Parsons' quotients
REM Formula found by SHELXT: C100 N27 O6 Cu3
CELL 0.71073 19.423 19.423 29.4339 90 90 120
ZERR 9 0.0019 0.0019 0.0029 0 0 0
LATT -3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H Cu F N O P
UNIT 327 432 9 72 36 9 12
DFIX 2.52 C27 CAD
DFIX 1.54 C1AA C1
DFIX 2.52 C3BA C24
DFIX 2.52 C24 C12
DFIX 2.52 C12 C3BA
DFIX 1.54 C8AA C00J
DFIX 1.64 P2 F4 P2 F5
DFIX 1.64 P2 F3AA
DFIX 1.64 P2 F17 P2 F4AA P2 F13
DFIX 2.32 F17 F4AA
DFIX 2.32 F3AA F4AA
DFIX 2.32 F13 F3AA
DFIX 2.52 C17 C6 C9 C30
DFIX 2.52 C1 C27 C7AA C2AA
DFIX 2.52 C27 CAD C2AA C4
DFIX 2.52 CAD C1 C4 C7AA
DFIX 2.52 C1BA C0CA C4BA C18 C5AA C16
DFIX 1.64 P1 F0AA
DFIX 1.64 P1 F2AA
DFIX 1.64 P1 F12
DFIX 2.52 C32 C5 C3BA C24
DFIX 2.52 C32 C21 C6BA C24
DFIX 1.54 C3BA C2 C5 C2 C24 C2 C2 C12 C21 C2
DFIX 2.52 C21 C5
DFIX 2.52 C21 C5 C6BA C3BA
DFIX 2.52 C19 C1BA C0AA C4BA C4AA C5AA
DFIX 2.52 C0CA C19 C18 C0AA C16 C4AA
DFIX 2.52 C30 C28 C13 C6
DFIX 2.52 C9 C28 C17 C13
DFIX 2.32 F2AB F8A
DFIX 1.64 F6AA P2
DFIX 1.64 P2 F13 P2 F8AA P2 F5 P2 F31 P2 F17 P2 F3AA P2 F3BA P2 F7AA P2 F4
DFIX 1.64 P2 F6AA
DFIX 2.32 F4AA F31
DFIX 2.32 F31 F4
DFIX 2.32 F13 F8AA
DFIX 2.32 F4 F8AA
DFIX 2.32 F7AA F2
SADI CAD C1AA C27 C1AA
SADI 0.04 F4AA F13 F4AA F3AA F4AA F17 F13 F3AA
SADI P2 F4AA P2 F13 P2 F3AA P2 F17
SADI C2AA C1AA C27 C1AA C7AA C1AA C1AA C1 C4 C1AA CAD C1AA
SADI P1 F2AA P1 F12
SADI P1 F20 P1 F0AA P1 F2AA P1 F8 P1 F18
SADI F0AA F18 F8 F20
SADI P1 F2AA P1 F2AB
SADI P1 F0AA P1 F0AB
SADI P1 F20 P1 F20A
SADI P1 F8 P1 F8A
SADI P1 F0AB P1 F20 P1 F20A P1 F8 P1 F8A P1 F2AA P1 F2AB P1 F0AA
SADI C21 C2 C6BA C2 C5 C2 C3BA C2 C24 C2 C32 C2
SADI C5AA C00J C0CA C00J C18 C00J C16 C00J C19 C00J C0AA C00J C4AA C00J =
C1BA C00J C4BA C00J
SADI C26 C13 C9 C26 C26 C17 C30 C26 C6 C26 C28 C26
SADI 0.04 F2 F7AA F2 F3BA F2 F6AA F2 F5 F17 F7AA F17 F3BA F17 F5 F7AA F3BA =
F3BA F6AA F6AA F5
SADI P2 F2 P2 F17 P2 F7AA P2 F3BA P2 F6AA P2 F5
DELU F0AA F2AA
DELU F8 F2AA F0AA F20
DELU C21 CAD C4 C1 C7AA C27 C2AA
RIGU C3BA C2
RIGU C21 C2
RIGU C9A C2AA CAD C4 C1 C7AA C27
RIGU C9 C17 C30 C6 C28 C13 C26
RIGU Cu1 O00E
RIGU O00E C00V
RIGU Cu1 O00E C00V
RIGU 0.002 0.002 C6 C30 C17 C9 C13 C28
EADP C6BA C2
EADP C4 C1AA
EADP C2AA C1AA
EADP C7AA C1AA
EADP C2 C21
EADP C16 C19 C0AA C1BA C4BA C5AA C0CA C18 C4AA C00J
EADP C32 C2
EADP C6 C26
EADP F17 F31
EADP C2AA C27
EADP Cu1 O00E
EADP C2 C5
EADP F6AA F2
EADP F31 F4AA
L.S. 50
PLAN 32
SIZE 0.036 0.107 0.114
TEMP -123.16
BIND P2 F6AA
CONN 0 F6AA
LIST 6
MORE -1
CONF
fmap 2
acta 52
OMIT -3 50
OMIT 1 1 0
OMIT -1 1 1
OMIT 0 1 -1
OMIT -1 2 0
OMIT -1 1 -2
OMIT 0 1 2
OMIT 0 0 -3
OMIT -2 2 -1
OMIT 0 0 3
OMIT 0 2 1
REM
REM
REM
WGHT 0.135600 3.289500
FVAR 0.15056
PART 1
CU1 3 0.528361 0.333094 0.500364 11.00000 0.07141 0.08304 =
0.04046 0.00272 0.00204 0.04105
PART 0
N1A 5 0.416792 0.228322 0.507547 11.00000 0.06243 0.09357 =
0.04929 -0.01059 -0.00269 0.04496
N2A 5 0.519538 0.326324 0.567657 11.00000 0.06626 0.07621 =
0.05795 0.00261 0.00712 0.03187
C1A 1 0.369837 0.176078 0.476472 11.00000 0.07427 0.11633 =
0.04893 -0.00917 -0.00912 0.03133
AFIX 43
H1A 2 0.386433 0.185039 0.445625 11.00000 -1.20000
AFIX 0
C2A 1 0.299470 0.110709 0.486785 11.00000 0.10526 0.12789 =
0.05953 -0.03049 -0.03129 0.07777
AFIX 43
H2A 2 0.267986 0.077289 0.462662 11.00000 -1.20000
AFIX 0
C4A 1 0.325063 0.144844 0.563515 11.00000 0.07821 0.08959 =
0.05045 0.00250 -0.00868 0.03906
AFIX 43
H4A 2 0.311343 0.134747 0.594751 11.00000 -1.20000
AFIX 0
C5A 1 0.393969 0.209595 0.552307 11.00000 0.07784 0.06657 =
0.03526 -0.00586 -0.00546 0.04011
C6A 1 0.451415 0.268663 0.585495 11.00000 0.06954 0.06990 =
0.04599 -0.00592 -0.01367 0.03730
C7A 1 0.437087 0.261341 0.631318 11.00000 0.07363 0.07622 =
0.03337 0.00187 0.00274 0.03366
AFIX 43
H7A 2 0.388799 0.218097 0.642334 11.00000 0.05785
AFIX 0
C8A 1 0.489962 0.314133 0.661278 11.00000 0.07751 0.05446 =
0.05075 0.00217 -0.00964 0.01315
C9A 1 0.562232 0.375586 0.642956 11.00000 0.08745 0.09954 =
0.04841 -0.02084 -0.02478 0.05053
AFIX 43
H9A 2 0.601807 0.414222 0.662335 11.00000 -1.20000
AFIX 0
C10A 1 0.574320 0.378576 0.596879 11.00000 0.07241 0.07572 =
0.06506 0.00261 -0.00847 0.02467
AFIX 43
H10A 2 0.623447 0.419246 0.585024 11.00000 -1.20000
AFIX 0
C1AA 1 0.472459 0.311015 0.712000 11.00000 0.14366 0.09490 =
0.04150 -0.01474 -0.01440 0.04153
N1B 5 0.526540 0.339861 0.432749 11.00000 0.05888 0.05846 =
0.04421 0.00645 0.00164 0.02814
N2B 5 0.521487 0.437532 0.492489 11.00000 0.07514 0.09717 =
0.04397 0.00103 0.00639 0.05169
C1B 1 0.530307 0.290483 0.403913 11.00000 0.09577 0.07739 =
0.04809 -0.00069 0.00855 0.04595
AFIX 43
H1B 2 0.540813 0.251031 0.415549 11.00000 0.08079
AFIX 0
C2B 1 0.519942 0.292349 0.357727 11.00000 0.11278 0.06197 =
0.05414 0.00573 0.02259 0.04014
AFIX 43
H2B 2 0.520503 0.252947 0.338860 11.00000 -1.20000
AFIX 0
C4B 1 0.508296 0.406200 0.369674 11.00000 0.07865 0.06775 =
0.05155 0.00548 -0.00795 0.03451
AFIX 43
H4B 2 0.502499 0.448934 0.358538 11.00000 -1.20000
AFIX 0
C5B 1 0.516034 0.398975 0.415321 11.00000 0.06141 0.08576 =
0.03168 -0.00592 0.00140 0.03794
C6B 1 0.517083 0.455285 0.449455 11.00000 0.07099 0.08233 =
0.04210 -0.00328 0.00228 0.04181
C7B 1 0.513531 0.523368 0.437873 11.00000 0.09275 0.07472 =
0.04223 0.00273 0.01190 0.04744
AFIX 43
H7B 2 0.510874 0.534484 0.406696 11.00000 -1.20000
AFIX 0
C8B 1 0.513761 0.574330 0.469948 11.00000 0.07058 0.08892 =
0.06239 -0.00026 0.01607 0.03631
C9B 1 0.522769 0.557296 0.513621 11.00000 0.09744 0.09235 =
0.06506 -0.01576 0.02525 0.04704
AFIX 43
H9B 2 0.527379 0.592892 0.537119 11.00000 -1.20000
AFIX 0
C10B 1 0.525375 0.489541 0.524632 11.00000 0.11017 0.11344 =
0.04363 -0.00732 0.00976 0.06961
AFIX 43
H10B 2 0.530033 0.478967 0.555651 11.00000 0.13411
AFIX 0
O00E 6 0.598609 0.272330 0.499699 11.00000 0.07141 0.08304 =
0.04046 0.00272 0.00204 0.04105
C00J 1 0.195053 0.020023 0.544081 11.00000 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
C00V 1 0.666667 0.333333 0.501610 10.33333 0.06165 0.06165 =
0.05926 0.00000 0.00000 0.03082
C26 1 0.509032 0.648449 0.456946 11.00000 0.17316 0.10393 =
0.10078 0.00858 0.04709 0.08863
C2 1 0.493305 0.355759 0.287940 11.00000 0.14726 0.08246 =
0.04583 -0.00665 -0.00674 0.04304
P1 7 0.182597 0.181751 0.668036 10.33333 0.10282
AFIX 6
P2 7 0.334648 0.054685 0.333517 11.00000 0.12030
PART 2
F4 4 0.365460 0.060358 0.280869 10.50000 0.13976
PART 0
PART 1
F5 4 0.292669 -0.042728 0.331570 10.50000 0.13903
AFIX 0
CAD 1 0.434402 0.227958 0.734971 10.50000 0.14893 0.07480 =
0.16389 0.03219 -0.07927 0.00497
AFIX 3
HADA 2 0.383182 0.192798 0.720381 10.50000 -1.50000
HADB 2 0.426242 0.231458 0.767541 10.50000 -1.50000
HADC 2 0.470112 0.206528 0.730531 10.50000 -1.50000
AFIX 0
C5 1 0.505207 0.437187 0.274400 10.50000 0.14726 0.08246 =
0.04583 -0.00665 -0.00674 0.04304
AFIX 3
H5A 2 0.466887 0.447177 0.290540 10.50000 -1.50000
H5B 2 0.498297 0.439517 0.241600 10.50000 -1.50000
H5C 2 0.559317 0.477617 0.282990 10.50000 -1.50000
AFIX 0
PART 0
C12 1 0.508854 0.350343 0.338764 11.00000 0.09787 0.06824 =
0.03667 0.00429 -0.00002 0.03351
PART 2
C24 1 0.403552 0.325261 0.281670 10.50000 0.14680 0.06985 =
0.06074 -0.00841 -0.01520 0.05269
AFIX 3
H24A 2 0.389292 0.362291 0.295540 10.50000 -1.50000
H24B 2 0.373132 0.273031 0.296100 10.50000 -1.50000
H24C 2 0.391232 0.320421 0.249140 10.50000 -1.50000
AFIX 0
PART 0
PART 1
C21 1 0.553189 0.338806 0.264332 10.50000 0.14726 0.08246 =
0.04583 -0.00665 -0.00674 0.04304
AFIX 3
H21A 2 0.532139 0.317896 0.234072 10.50000 -1.50000
H21B 2 0.560069 0.299306 0.281382 10.50000 -1.50000
H21C 2 0.604659 0.387786 0.261392 10.50000 -1.50000
AFIX 0
PART 0
PART 2
C3BA 1 0.542909 0.441063 0.271145 10.50000 0.12455 0.09921 =
0.05052 0.02283 0.03844 0.06344
AFIX 3
H3BA 2 0.525419 0.443163 0.240215 10.50000 -1.50000
H3BB 2 0.599169 0.456103 0.270715 10.50000 -1.50000
H3BC 2 0.535829 0.478023 0.290575 10.50000 -1.50000
AFIX 0
PART 0
PART 1
C27 1 0.545340 0.368592 0.742432 10.50000 0.14366 0.09490 =
0.04150 -0.01474 -0.01440 0.04153
AFIX 3
H27A 2 0.592740 0.366112 0.733592 10.50000 -1.50000
H27B 2 0.533360 0.353902 0.774502 10.50000 -1.50000
H27C 2 0.555120 0.422732 0.737912 10.50000 -1.50000
AFIX 0
C1 1 0.411740 0.341160 0.714905 10.50000 0.11626 0.15583 =
0.04223 -0.04419 -0.01078 0.05229
AFIX 3
H1C 2 0.425840 0.385090 0.693655 10.50000 -1.50000
H1D 2 0.413070 0.359670 0.746035 10.50000 -1.50000
H1E 2 0.358180 0.297530 0.707995 10.50000 -1.50000
AFIX 0
PART 0
F12 4 0.139484 0.234155 0.669053 10.33333 0.10248
C8AA 1 0.271341 0.090348 0.530632 11.00000 0.08481 0.08038 =
0.06257 -0.01552 -0.04113 0.04060
PART 2
F3AA 4 0.314410 0.122988 0.319118 10.50000 0.17204
F4AA 4 0.299505 0.038620 0.383487 10.50000 0.20353
F13 4 0.419971 0.122546 0.354210 10.50000 0.24770
PART 0
PART 1
F17 4 0.273131 0.046400 0.294296 10.50000 0.20353
C28 1 0.420596 0.619572 0.445723 10.50000 0.17321 0.08275 =
0.37011 -0.00090 0.03429 0.09545
AFIX 3
H28A 2 0.381846 0.577832 0.425713 10.50000 -1.50000
H28B 2 0.415906 0.667322 0.442783 10.50000 -1.50000
H28C 2 0.410216 0.600982 0.477263 10.50000 -1.50000
AFIX 0
PART 0
PART 2
C4 1 0.402912 0.228150 0.725573 10.50000 0.14366 0.09490 =
0.04150 -0.01474 -0.01440 0.04153
AFIX 3
H4C 2 0.353512 0.222210 0.713013 10.50000 -1.50000
H4D 2 0.398912 0.223990 0.758763 10.50000 -1.50000
H4E 2 0.411732 0.186160 0.713473 10.50000 -1.50000
AFIX 0
C2AA 1 0.546756 0.327832 0.740533 10.50000 0.14366 0.09490 =
0.04150 -0.01474 -0.01440 0.04153
AFIX 3
H2AA 2 0.564626 0.289312 0.735753 10.50000 -1.50000
H2AB 2 0.530825 0.325892 0.772323 10.50000 -1.50000
H2AC 2 0.590166 0.381372 0.733413 10.50000 -1.50000
AFIX 0
PART 0
PART 1
C32 1 0.407573 0.291542 0.278836 10.50000 0.14726 0.08246 =
0.04583 -0.00665 -0.00674 0.04304
AFIX 3
H32A 2 0.403243 0.239092 0.279896 10.50000 -1.50000
H32B 2 0.389813 0.299262 0.249096 10.50000 -1.50000
H32C 2 0.374213 0.295042 0.302666 10.50000 -1.50000
AFIX 0
C1BA 1 0.206848 -0.053064 0.551721 10.33333 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
AFIX 3
H1BA 2 0.201378 -0.082684 0.523691 10.33333 -1.50000
H1BB 2 0.164408 -0.087014 0.572901 10.33333 -1.50000
H1BC 2 0.258598 -0.036774 0.565601 10.33333 -1.50000
AFIX 0
PART 0
PART 3
C5AA 1 0.151131 -0.041245 0.505222 10.33333 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
AFIX 3
H5AA 2 0.152001 -0.090195 0.512002 10.33333 -1.50000
H5AB 2 0.182641 -0.016505 0.477882 10.33333 -1.50000
H5AC 2 0.096151 -0.053895 0.500152 10.33333 -1.50000
AFIX 0
PART 0
PART 2
C4BA 1 0.196123 -0.054062 0.523316 10.33333 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
AFIX 3
H4BA 2 0.241443 -0.055762 0.536716 10.33333 -1.50000
H4BB 2 0.202533 -0.048762 0.490266 10.33333 -1.50000
H4BC 2 0.146893 -0.103252 0.530716 10.33333 -1.50000
AFIX 0
C7AA 1 0.450417 0.375113 0.724971 10.50000 0.14366 0.09490 =
0.04150 -0.01474 -0.01440 0.04153
AFIX 3
H7AA 2 0.497127 0.428453 0.722901 10.50000 -1.50000
H7AB 2 0.429407 0.365753 0.756031 10.50000 -1.50000
H7AC 2 0.409527 0.370803 0.703781 10.50000 -1.50000
AFIX 0
PART 0
PART 1
F6AA 4 0.260287 0.030510 0.367821 10.50000 0.19172
F7AA 4 0.404886 0.110935 0.298888 10.50000 0.15901
PART 0
PART 2
C6BA 1 0.514161 0.301518 0.260082 10.50000 0.14726 0.08246 =
0.04583 -0.00665 -0.00674 0.04304
AFIX 3
H6BA 2 0.502191 0.299928 0.227612 10.50000 -1.50000
H6BB 2 0.482731 0.248128 0.273022 10.50000 -1.50000
H6BC 2 0.570861 0.320018 0.264042 10.50000 -1.50000
AFIX 0
PART 0
PART 1
C0CA 1 0.128115 -0.007117 0.507506 10.33333 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
AFIX 3
H0CA 2 0.106625 0.029023 0.508146 10.33333 -1.50000
H0CB 2 0.085075 -0.061707 0.512776 10.33333 -1.50000
H0CC 2 0.152295 -0.003877 0.477796 10.33333 -1.50000
AFIX 0
F3BA 4 0.345432 0.140624 0.349837 10.50000 0.16678
PART 0
PART 2
F8AA 4 0.375654 -0.004392 0.337916 10.50000 0.14846
F31 4 0.245479 0.005546 0.312754 10.50000 0.20353
C17 1 0.590448 0.726260 0.461391 10.50000 0.18974 0.11340 =
0.21766 0.02392 0.09509 0.06587
AFIX 3
H17A 2 0.588278 0.774100 0.453291 10.50000 -1.50000
H17B 2 0.602859 0.705280 0.434251 10.50000 -1.50000
H17C 2 0.631798 0.739650 0.484351 10.50000 -1.50000
AFIX 0
PART 0
PART 3
C4AA 1 0.205077 -0.025062 0.584447 10.33333 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
AFIX 3
H4AA 2 0.233317 -0.052962 0.575617 10.33333 -1.50000
H4AB 2 0.152307 -0.063492 0.596147 10.33333 -1.50000
H4AC 2 0.235247 0.014048 0.608137 10.33333 -1.50000
AFIX 0
PART 0
PART 2
C18 1 0.130851 0.030750 0.518814 10.33333 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
AFIX 3
H18A 2 0.127411 0.075640 0.531404 10.33333 -1.50000
H18B 2 0.079481 -0.018160 0.522344 10.33333 -1.50000
H18C 2 0.144561 0.040160 0.486484 10.33333 -1.50000
AFIX 0
PART 0
PART 1
C30 1 0.535075 0.709281 0.496312 10.50000 0.42728 0.18354 =
0.18733 -0.08028 -0.04805 0.25410
AFIX 3
H30A 2 0.546615 0.759241 0.481672 10.50000 -1.50000
H30B 2 0.581525 0.702221 0.493792 10.50000 -1.50000
H30C 2 0.522705 0.710791 0.528432 10.50000 -1.50000
AFIX 0
C9 1 0.561413 0.691008 0.415856 10.50000 0.23687 0.07759 =
0.19356 0.06895 0.11597 0.10102
AFIX 3
H9C 2 0.616473 0.712228 0.405806 10.50000 -1.50000
H9D 2 0.545533 0.731068 0.411036 10.50000 -1.50000
H9E 2 0.526423 0.643128 0.398326 10.50000 -1.50000
AFIX 0
PART 0
PART 2
C6 1 0.449390 0.654543 0.488338 10.50000 0.17316 0.10393 =
0.10078 0.00858 0.04709 0.08863
AFIX 3
H6A 2 0.498900 0.700532 0.498938 10.50000 -1.50000
H6B 2 0.428360 0.613713 0.512108 10.50000 -1.50000
H6C 2 0.410380 0.671043 0.481548 10.50000 -1.50000
AFIX 0
C13 1 0.479551 0.639899 0.407512 10.50000 0.39142 0.14839 =
0.09656 0.00691 0.01806 0.20073
AFIX 3
H13A 2 0.489151 0.613849 0.381752 10.50000 -1.50000
H13B 2 0.477231 0.686449 0.396682 10.50000 -1.50000
H13C 2 0.428981 0.602539 0.421992 10.50000 -1.50000
AFIX 0
C0AA 1 0.170201 -0.000380 0.594774 10.33333 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
AFIX 3
H0AA 2 0.185121 0.049860 0.610194 10.33333 -1.50000
H0AB 2 0.200411 -0.023730 0.607704 10.33333 -1.50000
H0AC 2 0.113211 -0.037250 0.598904 10.33333 -1.50000
AFIX 0
PART 0
PART 3
C16 1 0.139556 0.052725 0.560098 10.33333 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
AFIX 3
H16A 2 0.110576 0.029035 0.588348 10.33333 -1.50000
H16B 2 0.101596 0.040435 0.535238 10.33333 -1.50000
H16C 2 0.171896 0.110505 0.563758 10.33333 -1.50000
AFIX 0
PART 0
PART 1
C19 1 0.161699 0.033636 0.589645 10.33333 0.10149 0.09260 =
0.11857 0.02393 -0.04821 0.01622
AFIX 3
H19A 2 0.113159 -0.014264 0.599505 10.33333 -1.50000
H19B 2 0.149649 0.076026 0.583295 10.33333 -1.50000
H19C 2 0.201749 0.050866 0.613775 10.33333 -1.50000
AFIX 0
F2AA 4 0.100673 0.098328 0.675260 10.16667 10.10000
F0AA 4 0.170188 0.171884 0.613524 10.16667 10.10000
F20 4 0.261823 0.268396 0.658304 10.16667 10.10000
F8 4 0.203529 0.199729 0.721653 10.16667 10.10000
PART 0
F18 4 0.236756 0.141564 0.665217 10.33333 0.13438
PART 2
F20A 4 0.245169 0.254649 0.699607 10.16666 10.10000
F0AB 4 0.223114 0.222730 0.619919 10.16666 10.10000
F2AB 4 0.106545 0.110546 0.643601 10.16666 10.10000
F8A 4 0.144496 0.149097 0.717621 10.16666 10.10000
PART 0
PART 1
F2 4 0.394712 0.068959 0.371551 10.50000 0.19172
HKLF 4
REM Bishwanath_27Sept16_Cu_0m_a.res in R3
REM R1 = 0.0812 for 3786 Fo > 4sig(Fo) and 0.1592 for all 6937 data
REM 488 parameters refined using 330 restraints
END
WGHT 0.1303 1.4366
REM Highest difference peak 0.687, deepest hole -1.068, 1-sigma level 0.081
Q1 1 0.6199 0.2473 0.5074 11.00000 0.05 0.69
Q2 1 0.3058 -0.0044 0.3856 11.00000 0.05 0.44
Q3 1 0.0317 0.0981 0.6659 11.00000 0.05 0.39
Q4 1 0.1384 0.1412 0.6670 11.00000 0.05 0.36
Q5 1 0.6667 0.3333 0.3763 10.33333 0.05 0.35
Q6 1 0.2725 -0.0151 0.3129 11.00000 0.05 0.35
Q7 1 0.5696 0.2792 0.4873 11.00000 0.05 0.32
Q8 1 0.6667 0.3333 0.3329 10.33333 0.05 0.31
Q9 1 0.3612 0.0166 0.2856 11.00000 0.05 0.31
Q10 1 0.4480 0.1535 0.4998 11.00000 0.05 0.30
Q11 1 0.4074 0.0755 0.3483 11.00000 0.05 0.30
Q12 1 0.6379 0.3422 0.3397 11.00000 0.05 0.29
Q13 1 0.1823 0.2564 0.6940 11.00000 0.05 0.29
Q14 1 0.5925 0.4063 0.2675 11.00000 0.05 0.28
Q15 1 0.4102 0.1016 0.3750 11.00000 0.05 0.28
Q16 1 0.0000 0.0000 0.6599 10.33333 0.05 0.28
Q17 1 0.0561 0.0143 0.6929 11.00000 0.05 0.27
Q18 1 0.4857 0.3703 0.6077 11.00000 0.05 0.27
Q19 1 0.2719 0.1985 0.6605 11.00000 0.05 0.27
Q20 1 0.0475 0.1108 0.6420 11.00000 0.05 0.26
Q21 1 0.4888 0.3753 0.7381 11.00000 0.05 0.26
Q22 1 0.3333 0.6667 0.4902 10.33333 0.05 0.26
Q23 1 0.5763 0.3544 0.6456 11.00000 0.05 0.26
Q24 1 0.5817 0.4308 0.4953 11.00000 0.05 0.26
Q25 1 0.4531 0.3070 0.2654 11.00000 0.05 0.25
Q26 1 0.3332 0.0539 0.4967 11.00000 0.05 0.25
Q27 1 0.1444 -0.1689 0.4943 11.00000 0.05 0.25
Q28 1 0.5173 0.2659 0.7393 11.00000 0.05 0.25
Q29 1 0.3333 0.6667 0.5284 10.33333 0.05 0.24
Q30 1 0.5528 0.3656 0.6226 11.00000 0.05 0.24
Q31 1 0.6023 0.6107 0.4994 11.00000 0.05 0.24
Q32 1 0.3392 -0.0080 0.3341 11.00000 0.05 0.24
;
_shelx_res_checksum 33099
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT215_bishwanath_27sept16_cu_0m_a
;
PROBLEM: Disordered C30 has ADP max/min Ratio ..... 4.3 Note
RESPONSE: The teminal t-butyl group exhibits extensive orientational
disorder, which is attempted to model over two major sites. The
high thermal anisotropies arise these alerts.
;
_vrf_PLAT341_bishwanath_27sept16_cu_0m_a
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.01986 Ang.
RESPONSE: All the terminal t-bytyl groups show orientational disorders, which
reduce the average accuracy of the C-C bond distance.
;
# end Validation Reply Form