# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
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# Audit and citation data items may have been added by the CCDC.
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data_1-dy-2ch2cl2
_database_code_depnum_ccdc_archive 'CCDC 1566106'
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_audit_creation_date 2017-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C42 H40 B4 Cl2 Dy2 N24 O4, 2(C H2 Cl2)'
_chemical_formula_sum 'C44 H44 B4 Cl6 Dy2 N24 O4'
_chemical_formula_weight 1553.97
_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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 13.934(3)
_cell_length_b 15.037(3)
_cell_length_c 14.836(3)
_cell_angle_alpha 90
_cell_angle_beta 107.72(3)
_cell_angle_gamma 90
_cell_volume 2961.1(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2829
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 32.089
_cell_measurement_theta_min 0.407
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.839
_exptl_absorpt_correction_T_max 0.7463
_exptl_absorpt_correction_T_min 0.6322
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0771 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.8471.
The \l/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'light purple'
_exptl_crystal_density_diffrn 1.743
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 1524
_exptl_crystal_size_max 0.008
_exptl_crystal_size_mid 0.005
_exptl_crystal_size_min 0.005
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0568
_diffrn_reflns_av_unetI/netI 0.0356
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 71573
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 32.026
_diffrn_reflns_theta_min 1.756
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type 'ADSC Quantum 210r'
_diffrn_measurement_method 'Phi Scan'
_diffrn_radiation_monochromator 'Silicon Double Crystal'
_diffrn_radiation_type Synchrotron
_diffrn_radiation_wavelength 0.71080
_diffrn_radiation_source 'MX1 Beamline Australian Synchrotron'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7552
_reflns_number_total 9096
_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 'XDS (Kabsch, 1993)'
_computing_data_collection 'BluIce (McPhillips, 2002)'
_computing_data_reduction 'XDS (Kabsch, 1993)'
_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 1.597
_refine_diff_density_min -2.030
_refine_diff_density_rms 0.186
_refine_ls_extinction_coef 0.0076(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 380
_refine_ls_number_reflns 9096
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0473
_refine_ls_R_factor_gt 0.0335
_refine_ls_restrained_S_all 1.054
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+4.4116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0795
_refine_ls_wR_factor_ref 0.0846
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
B1(H1), B2(H2)
2.b Secondary CH2 refined with riding coordinates:
C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
C16(H16), C15(H15), C17(H17), C5(H5), C13(H13), C14(H14), C10(H10), C18(H18),
C6(H6), C3(H3), C9(H9), C12(H12), C4(H4), C8(H8), C7(H7), C2(H2A), C11(H11),
C1(H1A)
;
_atom_sites_solution_hydrogens geom
_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
Dy1 Dy 0.41725(2) 0.63091(2) 0.72507(2) 0.00734(5) Uani 1 1 d . . . . .
C22 C 0.6862(5) 0.7282(4) 0.5372(4) 0.071(2) Uani 1 1 d . . . . .
H22A H 0.613305 0.724122 0.514852 0.085 Uiso 1 1 calc R . . . .
H22B H 0.711424 0.705180 0.487586 0.085 Uiso 1 1 calc R . . . .
Cl1 Cl 0.56674(6) 0.32947(5) 0.63171(5) 0.01789(15) Uani 1 1 d . . . . .
N1 N 0.66330(18) 0.68236(17) 0.84612(17) 0.0123(5) Uani 1 1 d . . . . .
Cl2 Cl 0.73073(13) 0.66124(11) 0.63662(9) 0.0611(4) Uani 1 1 d . . . . .
N12 N 0.36358(17) 0.52377(15) 0.82311(16) 0.0103(4) Uani 1 1 d . . . . .
Cl3 Cl 0.72012(12) 0.83961(9) 0.55578(12) 0.0637(4) Uani 1 1 d . . . . .
N7 N 0.19104(18) 0.67118(16) 0.75685(17) 0.0119(4) Uani 1 1 d . . . . .
O1 O 0.47177(15) 0.49726(13) 0.67123(14) 0.0115(4) Uani 1 1 d . . . . .
N9 N 0.18149(17) 0.53568(16) 0.65596(17) 0.0114(4) Uani 1 1 d . . . . .
O2 O 0.57232(16) 0.35782(13) 0.43089(15) 0.0132(4) Uani 1 1 d . . . . .
N5 N 0.56387(18) 0.81893(16) 0.77063(17) 0.0131(5) Uani 1 1 d . . . . .
N3 N 0.54735(18) 0.75545(16) 0.92198(17) 0.0123(5) Uani 1 1 d . . . . .
N6 N 0.48391(19) 0.77916(16) 0.70653(17) 0.0133(5) Uani 1 1 d . . . . .
N11 N 0.26773(17) 0.52546(15) 0.82991(17) 0.0102(4) Uani 1 1 d . . . . .
B1 B 0.6210(2) 0.7724(2) 0.8653(2) 0.0134(6) Uani 1 1 d . . . . .
H1 H 0.676146 0.810567 0.901881 0.016 Uiso 1 1 calc R . . . .
B2 B 0.1800(2) 0.5693(2) 0.7532(2) 0.0119(6) Uani 1 1 d . . . . .
H2 H 0.115962 0.552726 0.763216 0.014 Uiso 1 1 calc R . . . .
N2 N 0.60410(19) 0.61345(17) 0.80151(18) 0.0125(4) Uani 1 1 d . . . . .
N10 N 0.25807(18) 0.55703(16) 0.61989(17) 0.0111(4) Uani 1 1 d . . . . .
N8 N 0.26989(18) 0.71389(16) 0.73892(17) 0.0118(4) Uani 1 1 d . . . . .
N4 N 0.46552(18) 0.70163(16) 0.88669(17) 0.0118(4) Uani 1 1 d . . . . .
C16 C 0.2650(2) 0.47798(19) 0.9062(2) 0.0134(5) Uani 1 1 d . . . . .
H16 H 0.208502 0.469600 0.926103 0.016 Uiso 1 1 calc R . . . .
C15 C 0.2356(2) 0.5162(2) 0.5355(2) 0.0152(5) Uani 1 1 d . . . . .
H15 H 0.274610 0.519584 0.494637 0.018 Uiso 1 1 calc R . . . .
C21 C 0.5401(2) 0.42139(18) 0.46869(19) 0.0106(5) Uani 1 1 d . . . . .
C17 C 0.3595(2) 0.44390(19) 0.9498(2) 0.0155(6) Uani 1 1 d . . . . .
H17 H 0.379503 0.408503 1.003726 0.019 Uiso 1 1 calc R . . . .
C5 C 0.4721(2) 0.7468(2) 1.0331(2) 0.0170(6) Uani 1 1 d . . . . .
H5 H 0.456034 0.754261 1.089054 0.020 Uiso 1 1 calc R . . . .
C20 C 0.5299(2) 0.42163(18) 0.5595(2) 0.0116(5) Uani 1 1 d . . . . .
C13 C 0.1145(2) 0.4825(2) 0.5950(2) 0.0165(6) Uani 1 1 d . . . . .
H13 H 0.056347 0.459285 0.604234 0.020 Uiso 1 1 calc R . . . .
C14 C 0.1460(2) 0.4680(2) 0.5172(2) 0.0190(6) Uani 1 1 d . . . . .
H14 H 0.114645 0.433869 0.464119 0.023 Uiso 1 1 calc R . . . .
C10 C 0.1327(2) 0.7311(2) 0.7828(2) 0.0180(6) Uani 1 1 d . . . . .
H10 H 0.074693 0.717958 0.798795 0.022 Uiso 1 1 calc R . . . .
C19 C 0.4884(2) 0.49454(18) 0.59277(19) 0.0101(5) Uani 1 1 d . . . . .
C18 C 0.4181(2) 0.47416(18) 0.89545(19) 0.0126(5) Uani 1 1 d . . . . .
H18 H 0.486223 0.461605 0.907688 0.015 Uiso 1 1 calc R . . . .
C6 C 0.4201(2) 0.69675(19) 0.9541(2) 0.0137(5) Uani 1 1 d . . . . .
H6 H 0.361774 0.664430 0.948922 0.016 Uiso 1 1 calc R . . . .
C3 C 0.6653(2) 0.5433(2) 0.8089(2) 0.0151(5) Uani 1 1 d . . . . .
H3 H 0.644515 0.486948 0.784921 0.018 Uiso 1 1 calc R . . . .
C9 C 0.4530(2) 0.8364(2) 0.6339(2) 0.0161(6) Uani 1 1 d . . . . .
H9 H 0.399198 0.826269 0.579669 0.019 Uiso 1 1 calc R . . . .
C12 C 0.2585(2) 0.80070(19) 0.7541(2) 0.0157(6) Uani 1 1 d . . . . .
H12 H 0.301952 0.845296 0.747124 0.019 Uiso 1 1 calc R . . . .
C4 C 0.5528(2) 0.78266(19) 1.0100(2) 0.0156(6) Uani 1 1 d . . . . .
H4 H 0.602292 0.819265 1.048439 0.019 Uiso 1 1 calc R . . . .
C8 C 0.5123(2) 0.9129(2) 0.6506(2) 0.0201(6) Uani 1 1 d . . . . .
H8 H 0.506368 0.962275 0.611588 0.024 Uiso 1 1 calc R . . . .
C7 C 0.5820(2) 0.8987(2) 0.7386(2) 0.0195(6) Uani 1 1 d . . . . .
H7 H 0.632853 0.937811 0.770134 0.023 Uiso 1 1 calc R . . . .
C2 C 0.7644(2) 0.5665(2) 0.8574(2) 0.0192(6) Uani 1 1 d . . . . .
H2A H 0.821239 0.530385 0.871504 0.023 Uiso 1 1 calc R . . . .
C11 C 0.1723(3) 0.8149(2) 0.7819(2) 0.0206(6) Uani 1 1 d . . . . .
H11 H 0.147432 0.868678 0.796397 0.025 Uiso 1 1 calc R . . . .
C1 C 0.7596(2) 0.6547(2) 0.8798(2) 0.0158(6) Uani 1 1 d . . . . .
H1A H 0.814010 0.689683 0.912815 0.019 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.00994(7) 0.00647(7) 0.00505(7) -0.00151(4) 0.00146(5) -0.00081(4)
C22 0.103(5) 0.047(3) 0.042(3) 0.014(2) -0.009(3) -0.039(3)
Cl1 0.0278(4) 0.0132(3) 0.0154(3) 0.0050(3) 0.0107(3) 0.0070(3)
N1 0.0108(10) 0.0152(11) 0.0104(11) -0.0006(9) 0.0023(9) -0.0035(9)
Cl2 0.0893(10) 0.0709(9) 0.0334(6) 0.0181(6) 0.0340(7) 0.0217(8)
N12 0.0106(10) 0.0102(10) 0.0079(10) 0.0002(8) -0.0003(8) 0.0014(8)
Cl3 0.0834(10) 0.0377(6) 0.0989(11) -0.0121(7) 0.0708(9) -0.0074(6)
N7 0.0128(11) 0.0117(11) 0.0109(11) 0.0019(9) 0.0030(9) 0.0034(8)
O1 0.0147(9) 0.0122(9) 0.0081(9) -0.0006(7) 0.0043(8) 0.0005(7)
N9 0.0100(10) 0.0103(10) 0.0112(11) 0.0019(9) -0.0007(9) -0.0013(8)
O2 0.0191(10) 0.0091(9) 0.0124(10) -0.0028(7) 0.0061(8) 0.0015(7)
N5 0.0155(11) 0.0094(11) 0.0127(12) 0.0001(9) 0.0020(9) -0.0042(8)
N3 0.0152(11) 0.0103(11) 0.0090(11) -0.0042(9) 0.0002(9) -0.0017(9)
N6 0.0168(11) 0.0101(11) 0.0106(11) -0.0003(9) 0.0005(9) -0.0030(9)
N11 0.0109(10) 0.0094(10) 0.0099(11) 0.0016(8) 0.0029(9) -0.0008(8)
B1 0.0158(14) 0.0123(14) 0.0102(14) -0.0012(11) 0.0011(12) -0.0036(11)
B2 0.0105(13) 0.0108(13) 0.0134(14) 0.0030(11) 0.0023(11) 0.0014(11)
N2 0.0138(11) 0.0123(11) 0.0107(11) -0.0018(9) 0.0025(9) -0.0001(9)
N10 0.0123(10) 0.0100(10) 0.0094(11) -0.0015(8) 0.0008(9) -0.0011(8)
N8 0.0147(11) 0.0087(10) 0.0117(11) 0.0000(9) 0.0034(9) 0.0004(8)
N4 0.0142(11) 0.0117(11) 0.0084(10) -0.0007(8) 0.0019(9) -0.0015(9)
C16 0.0171(13) 0.0121(12) 0.0103(12) 0.0029(10) 0.0030(10) -0.0017(10)
C15 0.0173(13) 0.0146(13) 0.0113(13) -0.0015(10) 0.0006(11) -0.0001(11)
C21 0.0119(12) 0.0100(12) 0.0100(12) -0.0025(9) 0.0032(10) -0.0015(9)
C17 0.0193(14) 0.0129(13) 0.0115(13) 0.0035(10) 0.0003(11) -0.0018(11)
C5 0.0231(15) 0.0165(14) 0.0110(13) -0.0024(11) 0.0044(11) 0.0027(11)
C20 0.0165(12) 0.0090(12) 0.0095(12) 0.0013(10) 0.0042(10) 0.0021(10)
C13 0.0144(13) 0.0130(13) 0.0172(14) -0.0009(11) -0.0026(11) -0.0041(10)
C14 0.0198(14) 0.0154(14) 0.0162(14) -0.0063(11) -0.0028(12) -0.0038(11)
C10 0.0218(15) 0.0193(14) 0.0139(14) 0.0029(11) 0.0069(12) 0.0087(12)
C19 0.0109(11) 0.0108(12) 0.0083(12) -0.0014(9) 0.0024(10) -0.0007(9)
C18 0.0160(13) 0.0108(12) 0.0084(12) 0.0027(10) 0.0000(10) 0.0013(10)
C6 0.0152(13) 0.0142(13) 0.0122(13) -0.0016(10) 0.0049(11) 0.0014(10)
C3 0.0159(13) 0.0144(13) 0.0138(13) -0.0008(11) 0.0026(11) 0.0030(10)
C9 0.0200(14) 0.0144(13) 0.0121(13) 0.0044(11) 0.0021(11) 0.0005(11)
C12 0.0256(15) 0.0084(12) 0.0128(13) -0.0016(10) 0.0055(12) 0.0026(11)
C4 0.0218(14) 0.0110(12) 0.0098(13) -0.0047(10) -0.0013(11) 0.0008(11)
C8 0.0219(15) 0.0141(14) 0.0250(16) 0.0109(12) 0.0080(13) 0.0000(11)
C7 0.0203(14) 0.0126(13) 0.0252(16) 0.0032(12) 0.0066(12) -0.0044(11)
C2 0.0121(13) 0.0257(16) 0.0185(15) 0.0007(12) 0.0028(11) 0.0057(11)
C11 0.0308(17) 0.0148(14) 0.0173(15) 0.0026(11) 0.0088(13) 0.0097(12)
C1 0.0105(12) 0.0241(15) 0.0114(13) 0.0043(11) 0.0010(10) -0.0019(11)
_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
Dy1 N12 2.436(2) . ?
Dy1 O1 2.371(2) . ?
Dy1 O2 2.368(2) 3_666 ?
Dy1 N6 2.462(2) . ?
Dy1 N2 2.517(3) . ?
Dy1 N10 2.546(2) . ?
Dy1 N8 2.464(2) . ?
Dy1 N4 2.520(2) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 Cl2 1.737(5) . ?
C22 Cl3 1.740(5) . ?
Cl1 C20 1.731(3) . ?
N1 B1 1.538(4) . ?
N1 N2 1.364(3) . ?
N1 C1 1.347(4) . ?
N12 N11 1.370(3) . ?
N12 C18 1.338(4) . ?
N7 B2 1.540(4) . ?
N7 N8 1.367(3) . ?
N7 C10 1.346(4) . ?
O1 C19 1.255(3) . ?
N9 B2 1.534(4) . ?
N9 N10 1.370(3) . ?
N9 C13 1.347(4) . ?
O2 C21 1.258(3) . ?
N5 N6 1.363(3) . ?
N5 B1 1.554(4) . ?
N5 C7 1.342(4) . ?
N3 B1 1.533(4) . ?
N3 N4 1.366(3) . ?
N3 C4 1.348(4) . ?
N6 C9 1.343(4) . ?
N11 B2 1.542(4) . ?
N11 C16 1.348(4) . ?
B1 H1 0.9800 . ?
B2 H2 0.9800 . ?
N2 C3 1.340(4) . ?
N10 C15 1.343(4) . ?
N8 C12 1.342(4) . ?
N4 C6 1.338(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.376(4) . ?
C15 H15 0.9300 . ?
C15 C14 1.398(4) . ?
C21 C20 1.397(4) . ?
C21 C19 1.539(4) 3_666 ?
C17 H17 0.9300 . ?
C17 C18 1.388(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.396(4) . ?
C5 C4 1.381(4) . ?
C20 C19 1.398(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.371(5) . ?
C14 H14 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.378(5) . ?
C18 H18 0.9300 . ?
C6 H6 0.9300 . ?
C3 H3 0.9300 . ?
C3 C2 1.395(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.394(4) . ?
C12 H12 0.9300 . ?
C12 C11 1.400(5) . ?
C4 H4 0.9300 . ?
C8 H8 0.9300 . ?
C8 C7 1.387(5) . ?
C7 H7 0.9300 . ?
C2 H2A 0.9300 . ?
C2 C1 1.373(5) . ?
C11 H11 0.9300 . ?
C1 H1A 0.9300 . ?
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
N12 Dy1 N6 149.35(8) . . ?
N12 Dy1 N2 97.21(8) . . ?
N12 Dy1 N10 73.07(8) . . ?
N12 Dy1 N8 82.53(8) . . ?
N12 Dy1 N4 75.67(8) . . ?
O1 Dy1 N12 80.13(7) . . ?
O1 Dy1 N6 124.00(8) . . ?
O1 Dy1 N2 70.73(7) . . ?
O1 Dy1 N10 74.48(7) . . ?
O1 Dy1 N8 144.86(8) . . ?
O1 Dy1 N4 131.15(7) . . ?
O2 Dy1 N12 138.77(7) 3_666 . ?
O2 Dy1 O1 67.07(7) 3_666 . ?
O2 Dy1 N6 71.86(8) 3_666 . ?
O2 Dy1 N2 94.88(8) 3_666 . ?
O2 Dy1 N10 74.54(8) 3_666 . ?
O2 Dy1 N8 110.23(8) 3_666 . ?
O2 Dy1 N4 145.23(7) 3_666 . ?
N6 Dy1 N2 76.77(8) . . ?
N6 Dy1 N10 127.91(8) . . ?
N6 Dy1 N8 84.44(8) . . ?
N6 Dy1 N4 73.96(8) . . ?
N2 Dy1 N10 145.02(8) . . ?
N2 Dy1 N4 71.06(8) . . ?
N8 Dy1 N2 142.10(8) . . ?
N8 Dy1 N10 71.30(8) . . ?
N8 Dy1 N4 72.23(8) . . ?
N4 Dy1 N10 134.25(8) . . ?
H22A C22 H22B 107.6 . . ?
Cl2 C22 H22A 108.7 . . ?
Cl2 C22 H22B 108.7 . . ?
Cl2 C22 Cl3 114.4(3) . . ?
Cl3 C22 H22A 108.7 . . ?
Cl3 C22 H22B 108.7 . . ?
N2 N1 B1 123.3(2) . . ?
C1 N1 B1 126.7(3) . . ?
C1 N1 N2 109.4(2) . . ?
N11 N12 Dy1 121.01(17) . . ?
C18 N12 Dy1 130.20(19) . . ?
C18 N12 N11 106.2(2) . . ?
N8 N7 B2 122.6(2) . . ?
C10 N7 B2 127.9(3) . . ?
C10 N7 N8 109.4(2) . . ?
C19 O1 Dy1 120.57(18) . . ?
N10 N9 B2 121.7(2) . . ?
C13 N9 B2 128.4(3) . . ?
C13 N9 N10 109.9(2) . . ?
C21 O2 Dy1 121.16(18) . 3_666 ?
N6 N5 B1 121.2(2) . . ?
C7 N5 N6 110.3(2) . . ?
C7 N5 B1 128.5(2) . . ?
N4 N3 B1 120.6(2) . . ?
C4 N3 B1 129.1(2) . . ?
C4 N3 N4 110.2(2) . . ?
N5 N6 Dy1 125.12(18) . . ?
C9 N6 Dy1 129.0(2) . . ?
C9 N6 N5 105.9(2) . . ?
N12 N11 B2 121.7(2) . . ?
C16 N11 N12 109.2(2) . . ?
C16 N11 B2 128.9(2) . . ?
N1 B1 N5 110.4(2) . . ?
N1 B1 H1 109.7 . . ?
N5 B1 H1 109.7 . . ?
N3 B1 N1 108.2(2) . . ?
N3 B1 N5 109.1(2) . . ?
N3 B1 H1 109.7 . . ?
N7 B2 N11 110.5(2) . . ?
N7 B2 H2 109.5 . . ?
N9 B2 N7 109.3(2) . . ?
N9 B2 N11 108.6(2) . . ?
N9 B2 H2 109.5 . . ?
N11 B2 H2 109.5 . . ?
N1 N2 Dy1 121.96(18) . . ?
C3 N2 Dy1 131.6(2) . . ?
C3 N2 N1 106.4(2) . . ?
N9 N10 Dy1 119.99(17) . . ?
C15 N10 Dy1 133.1(2) . . ?
C15 N10 N9 105.6(2) . . ?
N7 N8 Dy1 121.19(17) . . ?
C12 N8 Dy1 130.6(2) . . ?
C12 N8 N7 106.3(2) . . ?
N3 N4 Dy1 124.38(18) . . ?
C6 N4 Dy1 129.62(19) . . ?
C6 N4 N3 106.0(2) . . ?
N11 C16 H16 125.5 . . ?
N11 C16 C17 109.0(3) . . ?
C17 C16 H16 125.5 . . ?
N10 C15 H15 124.5 . . ?
N10 C15 C14 111.0(3) . . ?
C14 C15 H15 124.5 . . ?
O2 C21 C20 125.9(3) . . ?
O2 C21 C19 115.0(2) . 3_666 ?
C20 C21 C19 119.1(2) . 3_666 ?
C16 C17 H17 127.7 . . ?
C16 C17 C18 104.6(3) . . ?
C18 C17 H17 127.7 . . ?
C6 C5 H5 127.6 . . ?
C4 C5 H5 127.6 . . ?
C4 C5 C6 104.8(3) . . ?
C21 C20 Cl1 119.8(2) . . ?
C21 C20 C19 121.1(2) . . ?
C19 C20 Cl1 119.1(2) . . ?
N9 C13 H13 125.5 . . ?
N9 C13 C14 109.0(3) . . ?
C14 C13 H13 125.5 . . ?
C15 C14 H14 127.8 . . ?
C13 C14 C15 104.5(3) . . ?
C13 C14 H14 127.8 . . ?
N7 C10 H10 125.3 . . ?
N7 C10 C11 109.3(3) . . ?
C11 C10 H10 125.3 . . ?
O1 C19 C21 115.8(2) . 3_666 ?
O1 C19 C20 124.5(3) . . ?
C20 C19 C21 119.7(2) . 3_666 ?
N12 C18 C17 111.0(3) . . ?
N12 C18 H18 124.5 . . ?
C17 C18 H18 124.5 . . ?
N4 C6 C5 110.8(3) . . ?
N4 C6 H6 124.6 . . ?
C5 C6 H6 124.6 . . ?
N2 C3 H3 124.7 . . ?
N2 C3 C2 110.5(3) . . ?
C2 C3 H3 124.7 . . ?
N6 C9 H9 124.5 . . ?
N6 C9 C8 111.0(3) . . ?
C8 C9 H9 124.5 . . ?
N8 C12 H12 124.6 . . ?
N8 C12 C11 110.7(3) . . ?
C11 C12 H12 124.6 . . ?
N3 C4 C5 108.2(3) . . ?
N3 C4 H4 125.9 . . ?
C5 C4 H4 125.9 . . ?
C9 C8 H8 127.8 . . ?
C7 C8 C9 104.4(3) . . ?
C7 C8 H8 127.8 . . ?
N5 C7 C8 108.5(3) . . ?
N5 C7 H7 125.8 . . ?
C8 C7 H7 125.8 . . ?
C3 C2 H2A 127.7 . . ?
C1 C2 C3 104.7(3) . . ?
C1 C2 H2A 127.7 . . ?
C10 C11 C12 104.2(3) . . ?
C10 C11 H11 127.9 . . ?
C12 C11 H11 127.9 . . ?
N1 C1 C2 108.9(3) . . ?
N1 C1 H1A 125.5 . . ?
C2 C1 H1A 125.5 . . ?
_shelx_res_file
;
TITL 1-Dy-2CH2Cl2_a.res in P2(1)/n
1-dy-2ch2cl2.res
created by SHELXL-2016/6 at 14:43:01 on 19-Jun-2017
REM Old TITL 1-Dy-2CH2Cl2 in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.071, Rweak 0.004, Alpha 0.037, Orientation as input
REM Formula found by SHELXT: C29 B N5 O2 Cl3 Dy
CELL 0.71073 13.934 15.037 14.836 90 107.718 90
ZERR 2 0.0028 0.003 0.003 0 0.03 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B N O Cl Dy
UNIT 88 88 8 48 8 12 4
L.S. 10
PLAN 10
BOND $H
LIST 6
fmap 2
acta
OMIT -5 9 19
OMIT -4 9 20
REM
REM
REM
WGHT 0.048600 4.411600
EXTI 0.007599
FVAR 0.28887
DY1 7 0.417252 0.630907 0.725067 11.00000 0.00994 0.00647 =
0.00505 -0.00151 0.00146 -0.00081
C22 1 0.686224 0.728151 0.537167 11.00000 0.10305 0.04697 =
0.04232 0.01418 -0.00869 -0.03854
AFIX 23
H22A 2 0.613305 0.724122 0.514852 11.00000 -1.20000
H22B 2 0.711424 0.705180 0.487586 11.00000 -1.20000
AFIX 0
CL1 6 0.566739 0.329468 0.631708 11.00000 0.02782 0.01320 =
0.01543 0.00495 0.01071 0.00697
N1 4 0.663297 0.682356 0.846120 11.00000 0.01076 0.01524 =
0.01040 -0.00059 0.00228 -0.00351
CL2 6 0.730729 0.661236 0.636621 11.00000 0.08933 0.07085 =
0.03344 0.01812 0.03396 0.02172
N12 4 0.363578 0.523768 0.823109 11.00000 0.01057 0.01021 =
0.00792 0.00015 -0.00033 0.00142
CL3 6 0.720123 0.839605 0.555779 11.00000 0.08341 0.03766 =
0.09887 -0.01207 0.07078 -0.00743
N7 4 0.191045 0.671184 0.756851 11.00000 0.01281 0.01169 =
0.01090 0.00193 0.00302 0.00344
O1 5 0.471773 0.497258 0.671235 11.00000 0.01474 0.01224 =
0.00812 -0.00062 0.00427 0.00051
N9 4 0.181494 0.535680 0.655964 11.00000 0.01002 0.01027 =
0.01116 0.00193 -0.00075 -0.00130
O2 5 0.572318 0.357823 0.430894 11.00000 0.01908 0.00910 =
0.01244 -0.00283 0.00614 0.00147
N5 4 0.563867 0.818932 0.770633 11.00000 0.01554 0.00940 =
0.01274 0.00007 0.00203 -0.00424
N3 4 0.547346 0.755448 0.921982 11.00000 0.01523 0.01027 =
0.00904 -0.00421 0.00021 -0.00173
N6 4 0.483913 0.779156 0.706534 11.00000 0.01682 0.01008 =
0.01060 -0.00032 0.00050 -0.00302
N11 4 0.267734 0.525464 0.829914 11.00000 0.01092 0.00944 =
0.00990 0.00158 0.00285 -0.00076
B1 3 0.620958 0.772448 0.865302 11.00000 0.01584 0.01229 =
0.01018 -0.00124 0.00107 -0.00362
AFIX 13
H1 2 0.676146 0.810567 0.901881 11.00000 -1.20000
AFIX 0
B2 3 0.179966 0.569260 0.753162 11.00000 0.01054 0.01083 =
0.01341 0.00302 0.00233 0.00142
AFIX 13
H2 2 0.115962 0.552726 0.763216 11.00000 -1.20000
AFIX 0
N2 4 0.604098 0.613451 0.801510 11.00000 0.01380 0.01227 =
0.01073 -0.00181 0.00255 -0.00007
N10 4 0.258071 0.557033 0.619886 11.00000 0.01232 0.01000 =
0.00937 -0.00152 0.00077 -0.00110
N8 4 0.269892 0.713886 0.738924 11.00000 0.01470 0.00866 =
0.01171 0.00004 0.00342 0.00045
N4 4 0.465522 0.701629 0.886693 11.00000 0.01416 0.01173 =
0.00839 -0.00072 0.00191 -0.00146
C16 1 0.265022 0.477976 0.906195 11.00000 0.01708 0.01213 =
0.01026 0.00290 0.00303 -0.00166
AFIX 43
H16 2 0.208502 0.469600 0.926103 11.00000 -1.20000
AFIX 0
C15 1 0.235638 0.516225 0.535480 11.00000 0.01725 0.01456 =
0.01127 -0.00147 0.00064 -0.00006
AFIX 43
H15 2 0.274610 0.519584 0.494637 11.00000 -1.20000
AFIX 0
C21 1 0.540118 0.421388 0.468691 11.00000 0.01187 0.01004 =
0.00996 -0.00248 0.00325 -0.00146
C17 1 0.359455 0.443905 0.949826 11.00000 0.01927 0.01292 =
0.01146 0.00345 0.00025 -0.00184
AFIX 43
H17 2 0.379503 0.408503 1.003726 11.00000 -1.20000
AFIX 0
C5 1 0.472140 0.746769 1.033126 11.00000 0.02307 0.01648 =
0.01104 -0.00238 0.00438 0.00270
AFIX 43
H5 2 0.456034 0.754261 1.089054 11.00000 -1.20000
AFIX 0
C20 1 0.529911 0.421630 0.559509 11.00000 0.01647 0.00904 =
0.00946 0.00134 0.00420 0.00211
C13 1 0.114520 0.482479 0.595010 11.00000 0.01435 0.01295 =
0.01716 -0.00085 -0.00257 -0.00411
AFIX 43
H13 2 0.056347 0.459285 0.604234 11.00000 -1.20000
AFIX 0
C14 1 0.145959 0.468042 0.517171 11.00000 0.01979 0.01542 =
0.01619 -0.00625 -0.00275 -0.00376
AFIX 43
H14 2 0.114645 0.433869 0.464119 11.00000 -1.20000
AFIX 0
C10 1 0.132670 0.731090 0.782781 11.00000 0.02178 0.01931 =
0.01388 0.00289 0.00686 0.00872
AFIX 43
H10 2 0.074693 0.717958 0.798795 11.00000 -1.20000
AFIX 0
C19 1 0.488380 0.494536 0.592772 11.00000 0.01094 0.01078 =
0.00826 -0.00139 0.00239 -0.00069
C18 1 0.418093 0.474157 0.895452 11.00000 0.01598 0.01085 =
0.00836 0.00267 -0.00003 0.00131
AFIX 43
H18 2 0.486223 0.461605 0.907688 11.00000 -1.20000
AFIX 0
C6 1 0.420103 0.696753 0.954058 11.00000 0.01522 0.01418 =
0.01218 -0.00163 0.00491 0.00145
AFIX 43
H6 2 0.361774 0.664430 0.948922 11.00000 -1.20000
AFIX 0
C3 1 0.665279 0.543285 0.808855 11.00000 0.01595 0.01441 =
0.01378 -0.00077 0.00262 0.00295
AFIX 43
H3 2 0.644515 0.486948 0.784921 11.00000 -1.20000
AFIX 0
C9 1 0.452987 0.836365 0.633889 11.00000 0.02004 0.01438 =
0.01208 0.00443 0.00205 0.00051
AFIX 43
H9 2 0.399198 0.826269 0.579669 11.00000 -1.20000
AFIX 0
C12 1 0.258511 0.800702 0.754102 11.00000 0.02565 0.00839 =
0.01275 -0.00156 0.00551 0.00264
AFIX 43
H12 2 0.301952 0.845296 0.747124 11.00000 -1.20000
AFIX 0
C4 1 0.552787 0.782656 1.009976 11.00000 0.02183 0.01100 =
0.00980 -0.00465 -0.00127 0.00082
AFIX 43
H4 2 0.602292 0.819265 1.048439 11.00000 -1.20000
AFIX 0
C8 1 0.512270 0.912874 0.650619 11.00000 0.02189 0.01412 =
0.02498 0.01090 0.00796 -0.00003
AFIX 43
H8 2 0.506368 0.962275 0.611588 11.00000 -1.20000
AFIX 0
C7 1 0.582036 0.898672 0.738616 11.00000 0.02033 0.01262 =
0.02517 0.00322 0.00657 -0.00439
AFIX 43
H7 2 0.632853 0.937811 0.770134 11.00000 -1.20000
AFIX 0
C2 1 0.764448 0.566547 0.857407 11.00000 0.01206 0.02568 =
0.01853 0.00067 0.00277 0.00573
AFIX 43
H2A 2 0.821239 0.530385 0.871504 11.00000 -1.20000
AFIX 0
C11 1 0.172285 0.814932 0.781877 11.00000 0.03079 0.01482 =
0.01729 0.00260 0.00875 0.00970
AFIX 43
H11 2 0.147432 0.868678 0.796397 11.00000 -1.20000
AFIX 0
C1 1 0.759618 0.654721 0.879784 11.00000 0.01047 0.02411 =
0.01138 0.00428 0.00097 -0.00189
AFIX 43
H1A 2 0.814010 0.689683 0.912815 11.00000 -1.20000
AFIX 0
HKLF 4
REM 1-Dy-2CH2Cl2_a.res in P2(1)/n
REM R1 = 0.0335 for 7552 Fo > 4sig(Fo) and 0.0473 for all 9096 data
REM 380 parameters refined using 0 restraints
END
WGHT 0.0486 4.4003
REM Highest difference peak 1.597, deepest hole -2.030, 1-sigma level 0.186
Q1 1 0.4173 0.6888 0.7809 11.00000 0.05 1.60
Q2 1 0.4215 0.6917 0.6752 11.00000 0.05 1.50
Q3 1 0.3969 0.5671 0.6783 11.00000 0.05 1.42
Q4 1 0.4194 0.5734 0.7805 11.00000 0.05 1.39
Q5 1 0.4335 0.5754 0.6782 11.00000 0.05 1.27
Q6 1 0.3835 0.6649 0.7000 11.00000 0.05 1.26
Q7 1 0.4382 0.6338 0.7640 11.00000 0.05 1.24
Q8 1 0.3824 0.6359 0.6758 11.00000 0.05 1.21
Q9 1 0.4952 0.6035 0.7627 11.00000 0.05 1.18
Q10 1 0.4428 0.6203 0.7066 11.00000 0.05 1.14
;
_shelx_res_checksum 56206
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT369_1-dy-2ch2cl2
;
PROBLEM: Long C(sp2)-C(sp2) Bond C19 - C21_a .. 1.54 Ang.
RESPONSE: Bond has similar observed mean bond length to that of
similar bonds in -C(=O)-C(=O)- systems.
;
_vrf_PLAT971_1-dy-2ch2cl2
;
PROBLEM: Check Calcd Residual Density 1.19A From Dy1 1.58 eA-3
RESPONSE: Slight inaccuracy of the absorption correction not
affecting the connectivity nor the integrity of the structure
;
_vrf_PLAT972_1-dy-2ch2cl2
;
PROBLEM: Check Calcd Residual Density 0.76A From Dy1 -1.79 eA-3
RESPONSE: Slight inaccuracy of the absorption correction not
affecting the connectivity nor the integrity of the structure
;
# 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_4-y-meoh
_database_code_depnum_ccdc_archive 'CCDC 1566111'
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_audit_creation_date 2017-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C36 H58 B4 N12 O14 Y2, 4.5(C H4 O)'
_chemical_formula_sum 'C40.50 H76 B4 N12 O18.50 Y2'
_chemical_formula_weight 1248.19
_chemical_melting_point ?
_chemical_oxdiff_formula 'C41 H77 B4 N12 O19 Y2'
_chemical_oxdiff_usercomment 'Owens mix *(Nd, Cs, S, N O Mn)'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 '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 10.3026(8)
_cell_length_b 11.8817(7)
_cell_length_c 13.8646(11)
_cell_angle_alpha 71.183(6)
_cell_angle_beta 81.824(6)
_cell_angle_gamma 87.703(6)
_cell_volume 1590.1(2)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 4537
_cell_measurement_temperature 130.01(10)
_cell_measurement_theta_max 73.0170
_cell_measurement_theta_min 4.2600
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.028
_exptl_absorpt_correction_T_max 0.884
_exptl_absorpt_correction_T_min 0.540
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'dark violet'
_exptl_crystal_colour_modifier dark
_exptl_crystal_colour_primary violet
_exptl_crystal_density_diffrn 1.303
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 649
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 1 -3 0.1576
0 -7 2 0.0342
1 -2 -9 0.0277
-1 7 -2 0.0476
7 -1 2 0.1082
1 -1 -9 0.0173
-1 1 8 0.0249
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.118
_exptl_crystal_size_min 0.051
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.4329 0.8728 -2.7161 0.6496 -0.7599 -0.0221
0.1474 -6.7091 1.6756 -0.1589 0.1845 0.9699
1.2062 -1.8459 -8.5082 0.7350 0.6286 -0.2543
-1.1167 6.6556 -1.6392 0.2148 -0.3133 -0.9251
6.5525 -0.9545 1.7639 -0.5666 0.8237 -0.0222
0.6040 -1.4304 -8.6756 0.7872 0.5412 -0.2958
-0.7213 0.7578 8.4996 -0.7624 -0.5241 0.3796
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0435
_diffrn_reflns_av_unetI/netI 0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 11043
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 73.915
_diffrn_reflns_theta_min 3.931
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 130.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -130.00 -20.00 1.00 1.00 -- -40.81 0.00 -90.00 110
2 \w -50.00 9.00 1.00 1.00 -- -40.81 38.00 -90.00 59
3 \w -43.00 35.00 1.00 1.00 -- -40.81 38.00 90.00 78
4 \w 32.00 81.00 1.00 1.00 -- 40.81-125.00-180.00 49
5 \w 27.00 89.00 1.00 1.00 -- 40.81-125.00 0.00 62
6 \w 61.00 87.00 1.00 15.00 -- 106.63 -45.00 120.00 26
7 \w 27.00 108.00 1.00 15.00 -- 106.63 -94.00 30.00 81
8 \w 56.00 87.00 1.00 15.00 -- 106.63 -45.00 -90.00 31
9 \w 144.00 170.00 1.00 15.00 -- 106.63 125.00 -90.00 26
10 \w 29.00 82.00 1.00 15.00 -- 106.63 -30.00 90.00 53
11 \w 94.00 127.00 1.00 15.00 -- 106.63 125.00 60.00 33
12 \w 29.00 91.00 1.00 15.00 -- 106.63 -30.00 30.00 62
13 \w 34.00 99.00 1.00 15.00 -- 106.63 -45.00-150.00 65
14 \w 46.00 107.00 1.00 15.00 -- 106.63 -94.00 120.00 61
15 \w 59.00 104.00 1.00 15.00 -- 106.63 -94.00 -60.00 45
16 \w 76.00 178.00 1.00 15.00 -- 106.63 30.00 0.00 102
17 \w 100.00 128.00 1.00 15.00 -- 106.63 125.00-180.00 28
18 \w 139.00 167.00 1.00 15.00 -- 106.63 125.00-180.00 28
19 \w 87.00 166.00 1.00 15.00 -- 106.63 45.00 60.00 79
20 \w 32.00 117.00 1.00 15.00 -- 106.63-125.00 -90.00 85
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0611545000
_diffrn_orient_matrix_UB_12 -0.0013313000
_diffrn_orient_matrix_UB_13 -0.0947698000
_diffrn_orient_matrix_UB_21 0.1330966000
_diffrn_orient_matrix_UB_22 -0.0363439000
_diffrn_orient_matrix_UB_23 -0.0471224000
_diffrn_orient_matrix_UB_31 -0.0369809000
_diffrn_orient_matrix_UB_32 -0.1320660000
_diffrn_orient_matrix_UB_33 0.0532986000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5445
_reflns_number_total 6215
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_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 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 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 1.546
_refine_diff_density_min -1.176
_refine_diff_density_rms 0.131
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.046
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 429
_refine_ls_number_reflns 6215
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0639
_refine_ls_R_factor_gt 0.0562
_refine_ls_restrained_S_all 1.046
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+0.6110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1509
_refine_ls_wR_factor_ref 0.1622
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
O7-H7A
0.85 with sigma of 0.01
O7-H7B
0.85 with sigma of 0.01
C18-H7A
1.873734 with sigma of 0.02
Y1-H7A
2.911315 with sigma of 0.02
C19-H7B
1.932896 with sigma of 0.02
Y1-H7B
2.879394 with sigma of 0.02
3. Others
Fixed Sof: H7A(0.5) H7B(0.5) O11(0.5) H11(0.5) O12(0.5) H12(0.5) C24(0.5)
H24A(0.5) H24B(0.5) H24C(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C18(0.5)
H18A(0.5) H18B(0.5) H18C(0.5) O9(0.5) H9A(0.5) C19(0.5) H19A(0.5) H19B(0.5)
H19C(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) O8(0.5) H8A(0.5) C20(0.5)
H20A(0.5) H20B(0.5) H20C(0.5) O10(0.25) H10(0.25) C22(0.25) H22A(0.25)
H22B(0.25) H22C(0.25)
4.a Ternary CH refined with riding coordinates:
B1(H1A)
4.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C8(H8), C7(H7), C6(H6), C5(H5), C9(H9), C4(H4), C3(H3)
4.c Idealised Me refined as rotating group:
C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C18(H18A,
H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C),
C22(H22A,H22B,H22C)
4.d Idealised tetrahedral OH refined as rotating group:
O11(H11), O12(H12), O9(H9A), O8(H8A), O10(H10)
;
_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
Y1 Y 0.21710(3) 0.23371(2) 0.18263(2) 0.02637(14) Uani 1 1 d D . . . .
O2 O 0.6943(3) 0.5779(2) -0.1573(2) 0.0312(5) Uani 1 1 d . . . . .
O3 O 0.3019(3) 0.0427(2) 0.2237(2) 0.0321(5) Uani 1 1 d . . . . .
O1 O 0.3608(3) 0.3037(2) 0.0293(2) 0.0323(5) Uani 1 1 d . . . . .
O7 O 0.1628(3) 0.2554(3) 0.3456(2) 0.0353(6) Uani 1 1 d D . . . .
H7A H 0.219(2) 0.280(8) 0.375(4) 0.053 Uiso 0.5 1 d D . P A 1
H7B H 0.120(7) 0.201(5) 0.3944(17) 0.053 Uiso 0.5 1 d D . P B 2
O4 O 0.4184(3) 0.1834(2) 0.2466(2) 0.0321(5) Uani 1 1 d . . . . .
O5 O 0.5426(3) 0.0243(3) 0.1956(3) 0.0393(6) Uani 1 1 d . . . . .
O6 O 0.4437(3) -0.0204(3) 0.3612(3) 0.0406(6) Uani 1 1 d . . . . .
N3 N -0.0021(3) 0.1833(3) 0.0378(2) 0.0300(6) Uani 1 1 d . . . . .
N4 N 0.1275(3) 0.1802(3) 0.0467(3) 0.0307(6) Uani 1 1 d . . . . .
N5 N -0.0933(3) 0.1148(3) 0.2251(2) 0.0292(6) Uani 1 1 d . . . . .
N1 N -0.0850(3) 0.3339(3) 0.1241(2) 0.0300(6) Uani 1 1 d . . . . .
N2 N 0.0307(3) 0.3672(3) 0.1436(2) 0.0297(6) Uani 1 1 d . . . . .
N6 N 0.0191(3) 0.1074(3) 0.2679(3) 0.0318(6) Uani 1 1 d . . . . .
C11 C 0.5350(4) 0.4291(3) -0.0711(3) 0.0328(7) Uani 1 1 d . . . . .
C14 C 0.2690(5) -0.0698(4) 0.2197(4) 0.0456(10) Uani 1 1 d . . . . .
H14A H 0.266021 -0.127460 0.286956 0.068 Uiso 1 1 calc GR . . . .
H14B H 0.333809 -0.092535 0.172600 0.068 Uiso 1 1 calc GR . . . .
H14C H 0.184690 -0.065747 0.196864 0.068 Uiso 1 1 calc GR . . . .
C12 C 0.6029(4) 0.5340(3) -0.0845(3) 0.0286(7) Uani 1 1 d . . . . .
C1 C -0.1693(4) 0.4251(4) 0.1103(3) 0.0347(8) Uani 1 1 d . . . . .
H1 H -0.254677 0.423505 0.096168 0.042 Uiso 1 1 calc R . . . .
C2 C -0.1094(4) 0.5211(4) 0.1203(3) 0.0384(9) Uani 1 1 d . . . . .
H2 H -0.144464 0.595999 0.114357 0.046 Uiso 1 1 calc R . . . .
C8 C -0.1232(4) -0.0366(4) 0.3690(3) 0.0367(8) Uani 1 1 d . . . . .
H8 H -0.159336 -0.101434 0.423123 0.044 Uiso 1 1 calc R . . . .
C7 C -0.1788(4) 0.0291(3) 0.2849(3) 0.0317(7) Uani 1 1 d . . . . .
H7 H -0.261877 0.016826 0.271076 0.038 Uiso 1 1 calc R . . . .
C6 C 0.1884(4) 0.1555(3) -0.0361(3) 0.0343(8) Uani 1 1 d . . . . .
H6 H 0.278765 0.148342 -0.050210 0.041 Uiso 1 1 calc R . . . .
C10 C 0.4318(4) 0.3941(3) 0.0110(3) 0.0289(7) Uani 1 1 d . . . . .
C5 C 0.0995(5) 0.1418(4) -0.0982(3) 0.0392(9) Uani 1 1 d . . . . .
H5 H 0.117035 0.124345 -0.159455 0.047 Uiso 1 1 calc R . . . .
C13 C 0.5693(5) 0.3593(4) -0.1436(4) 0.0489(11) Uani 1 1 d . . . . .
H13A H 0.569730 0.410909 -0.213033 0.073 Uiso 1 1 calc GR . . . .
H13B H 0.505584 0.297151 -0.129013 0.073 Uiso 1 1 calc GR . . . .
H13C H 0.654569 0.324964 -0.135183 0.073 Uiso 1 1 calc GR . . . .
C9 C 0.0002(4) 0.0153(4) 0.3556(3) 0.0368(8) Uani 1 1 d . . . . .
H9 H 0.061275 -0.010465 0.401370 0.044 Uiso 1 1 calc R . . . .
C4 C -0.0213(5) 0.1603(4) -0.0476(3) 0.0370(8) Uani 1 1 d . . . . .
H4 H -0.102127 0.157238 -0.069279 0.044 Uiso 1 1 calc R . . . .
C15 C 0.5241(4) 0.2383(4) 0.2705(4) 0.0405(9) Uani 1 1 d . . . . .
H15A H 0.604229 0.225500 0.230860 0.061 Uiso 1 1 calc GR . . . .
H15B H 0.531036 0.204358 0.342439 0.061 Uiso 1 1 calc GR . . . .
H15C H 0.508349 0.322114 0.254300 0.061 Uiso 1 1 calc GR . . . .
C3 C 0.0151(4) 0.4811(3) 0.1412(3) 0.0331(7) Uani 1 1 d . . . . .
H3 H 0.079283 0.526864 0.152028 0.040 Uiso 1 1 calc R . . . .
B1 B -0.1075(4) 0.2085(4) 0.1196(3) 0.0289(8) Uani 1 1 d . . . . .
H1A H -0.195130 0.203067 0.101773 0.035 Uiso 1 1 calc R . . . .
C16 C 0.5569(4) 0.0810(4) 0.0885(4) 0.0433(9) Uani 1 1 d . . . . .
H16A H 0.633796 0.051595 0.056721 0.065 Uiso 1 1 calc GR . . . .
H16B H 0.565387 0.165194 0.073832 0.065 Uiso 1 1 calc GR . . . .
H16C H 0.481164 0.064691 0.061900 0.065 Uiso 1 1 calc GR . . . .
C17 C 0.3494(5) -0.0103(5) 0.4430(4) 0.0469(10) Uani 1 1 d . . . . .
H17A H 0.327203 0.071762 0.431406 0.070 Uiso 1 1 calc GR . . . .
H17B H 0.385094 -0.041302 0.506657 0.070 Uiso 1 1 calc GR . . . .
H17C H 0.272160 -0.054720 0.446290 0.070 Uiso 1 1 calc GR . . . .
O11 O -0.0671(9) 0.4016(8) 0.5659(5) 0.0549(19) Uani 0.5 1 d . . P . .
H11 H -0.004915 0.406337 0.520677 0.082 Uiso 0.5 1 calc GR . P . .
O12 O 0.4376(13) 0.2264(7) 0.6006(6) 0.078(3) Uani 0.5 1 d . . P . .
H12 H 0.515578 0.210383 0.602598 0.117 Uiso 0.5 1 calc GR . P . .
B2 B 0.4315(4) 0.0550(4) 0.2574(4) 0.0340(9) Uani 1 1 d . . . . .
C24 C 0.3908(13) 0.2586(7) 0.6797(8) 0.052(2) Uani 0.5 1 d . . P . .
H24A H 0.297054 0.249980 0.691468 0.078 Uiso 0.5 1 calc GR . P . .
H24B H 0.413594 0.340214 0.666745 0.078 Uiso 0.5 1 calc GR . P . .
H24C H 0.426997 0.209472 0.739244 0.078 Uiso 0.5 1 calc GR . P . .
C23 C -0.0261(13) 0.3510(9) 0.6610(7) 0.051(2) Uani 0.5 1 d . . P . .
H23A H 0.063297 0.373567 0.657647 0.077 Uiso 0.5 1 calc GR . P . .
H23B H -0.032493 0.266041 0.680492 0.077 Uiso 0.5 1 calc GR . P . .
H23C H -0.080611 0.378348 0.711040 0.077 Uiso 0.5 1 calc GR . P . .
C18 C 0.0362(13) 0.2803(12) 0.3893(9) 0.061(3) Uani 0.5 1 d D . P C 1
H18A H -0.018167 0.311150 0.336011 0.092 Uiso 0.5 1 calc GR . P C 1
H18B H 0.043572 0.338073 0.423327 0.092 Uiso 0.5 1 calc GR . P C 1
H18C H -0.002283 0.208593 0.438281 0.092 Uiso 0.5 1 calc GR . P C 1
O9 O -0.0774(6) 0.2469(6) 0.4546(5) 0.0374(12) Uani 0.5 1 d . . P D 2
H9A H -0.042666 0.300868 0.466735 0.056 Uiso 0.5 1 calc GR . P D 2
C19 C 0.2346(13) 0.3229(11) 0.3970(9) 0.056(3) Uani 0.5 1 d D . P C 2
H19A H 0.315804 0.283885 0.413266 0.084 Uiso 0.5 1 calc GR . P C 2
H19B H 0.181558 0.325474 0.459034 0.084 Uiso 0.5 1 calc GR . P C 2
H19C H 0.252167 0.402478 0.351382 0.084 Uiso 0.5 1 calc GR . P C 2
C21 C -0.1832(8) 0.2934(8) 0.3972(7) 0.0401(17) Uani 0.5 1 d . . P D 2
H21A H -0.158159 0.369133 0.347251 0.060 Uiso 0.5 1 calc GR . P D 2
H21B H -0.258736 0.302959 0.443103 0.060 Uiso 0.5 1 calc GR . P D 2
H21C H -0.203819 0.239426 0.362821 0.060 Uiso 0.5 1 calc GR . P D 2
O8 O 0.3092(11) 0.3337(7) 0.4490(6) 0.067(3) Uani 0.5 1 d . . P E 1
H8A H 0.362352 0.292722 0.483712 0.101 Uiso 0.5 1 calc GR . P E 1
C20 C 0.3409(19) 0.4486(12) 0.4243(11) 0.077(4) Uani 0.5 1 d . . P E 1
H20A H 0.296735 0.494547 0.367923 0.116 Uiso 0.5 1 calc GR . P E 1
H20B H 0.433965 0.458398 0.404646 0.116 Uiso 0.5 1 calc GR . P E 1
H20C H 0.314728 0.475202 0.482549 0.116 Uiso 0.5 1 calc GR . P E 1
O10 O -0.303(3) 0.368(3) 0.506(2) 0.120(12) Uani 0.25 1 d . . P F 1
H10 H -0.327921 0.427729 0.520914 0.180 Uiso 0.25 1 calc GR . P F 1
C22 C -0.301(3) 0.392(2) 0.401(2) 0.066(6) Uani 0.25 1 d . . P F 1
H22A H -0.233956 0.450180 0.364718 0.099 Uiso 0.25 1 calc GR . P F 1
H22B H -0.384325 0.421521 0.381927 0.099 Uiso 0.25 1 calc GR . P F 1
H22C H -0.281585 0.319973 0.384586 0.099 Uiso 0.25 1 calc GR . P F 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
Y1 0.01860(19) 0.02662(19) 0.0311(2) -0.00553(13) -0.00227(12) -0.00335(11)
O2 0.0233(12) 0.0281(12) 0.0398(14) -0.0087(10) 0.0004(10) -0.0061(10)
O3 0.0237(12) 0.0273(12) 0.0441(15) -0.0080(11) -0.0086(11) -0.0010(9)
O1 0.0271(12) 0.0345(13) 0.0325(13) -0.0098(11) 0.0054(10) -0.0087(10)
O7 0.0292(13) 0.0437(14) 0.0312(13) -0.0104(11) -0.0006(10) -0.0052(11)
O4 0.0204(12) 0.0334(13) 0.0429(14) -0.0110(11) -0.0079(10) -0.0033(10)
O5 0.0265(13) 0.0402(14) 0.0525(17) -0.0160(13) -0.0075(12) 0.0029(11)
O6 0.0322(14) 0.0399(14) 0.0460(16) -0.0070(12) -0.0102(12) 0.0019(12)
N3 0.0257(15) 0.0309(14) 0.0315(15) -0.0074(12) -0.0033(12) -0.0034(12)
N4 0.0244(14) 0.0283(14) 0.0373(16) -0.0079(12) -0.0029(12) -0.0033(11)
N5 0.0194(13) 0.0326(15) 0.0339(15) -0.0081(12) -0.0032(11) -0.0022(11)
N1 0.0222(14) 0.0302(15) 0.0344(15) -0.0048(12) -0.0065(12) 0.0006(11)
N2 0.0241(14) 0.0283(14) 0.0332(15) -0.0057(12) -0.0015(12) -0.0046(11)
N6 0.0245(14) 0.0355(16) 0.0300(15) -0.0019(13) -0.0052(12) -0.0039(12)
C11 0.0273(17) 0.0318(17) 0.0369(19) -0.0093(15) 0.0016(14) -0.0062(14)
C14 0.036(2) 0.036(2) 0.068(3) -0.014(2) -0.018(2) -0.0033(16)
C12 0.0219(15) 0.0290(16) 0.0318(17) -0.0060(14) -0.0017(13) -0.0026(13)
C1 0.0256(17) 0.0379(19) 0.0341(18) -0.0037(15) -0.0025(14) 0.0043(15)
C2 0.036(2) 0.0296(18) 0.043(2) -0.0050(16) -0.0021(17) 0.0047(15)
C8 0.0306(19) 0.0354(19) 0.0348(19) 0.0004(15) 0.0002(15) -0.0078(15)
C7 0.0240(16) 0.0307(17) 0.0385(19) -0.0100(15) 0.0012(14) -0.0058(13)
C6 0.0350(19) 0.0315(17) 0.0359(19) -0.0124(15) 0.0014(15) -0.0017(15)
C10 0.0247(16) 0.0276(16) 0.0323(17) -0.0073(14) -0.0016(13) -0.0032(13)
C5 0.045(2) 0.0366(19) 0.037(2) -0.0145(16) -0.0021(17) -0.0057(17)
C13 0.050(3) 0.047(2) 0.050(2) -0.023(2) 0.016(2) -0.017(2)
C9 0.0289(19) 0.040(2) 0.0337(19) -0.0003(16) -0.0058(15) -0.0030(15)
C4 0.042(2) 0.0379(19) 0.0325(18) -0.0104(15) -0.0077(16) -0.0085(16)
C15 0.0289(19) 0.0368(19) 0.058(3) -0.0140(18) -0.0134(18) -0.0020(15)
C3 0.0335(19) 0.0301(17) 0.0334(18) -0.0084(14) -0.0006(14) -0.0026(14)
B1 0.0222(17) 0.0328(19) 0.0293(19) -0.0060(15) -0.0041(14) -0.0022(14)
C16 0.0312(19) 0.053(2) 0.052(2) -0.026(2) -0.0068(17) 0.0039(18)
C17 0.037(2) 0.050(2) 0.044(2) -0.0002(19) -0.0105(18) 0.0026(18)
O11 0.072(5) 0.073(4) 0.026(3) -0.024(3) -0.002(3) -0.031(4)
O12 0.149(10) 0.046(4) 0.043(4) -0.015(3) -0.041(5) 0.072(5)
B2 0.0226(19) 0.036(2) 0.044(2) -0.0117(18) -0.0102(17) 0.0004(15)
C24 0.085(7) 0.017(3) 0.052(5) -0.012(3) -0.006(5) 0.012(4)
C23 0.080(7) 0.049(5) 0.026(4) -0.012(4) -0.002(4) -0.020(5)
C18 0.062(7) 0.066(7) 0.048(5) -0.010(5) -0.006(5) 0.000(5)
O9 0.024(3) 0.047(3) 0.042(3) -0.018(3) -0.002(2) -0.005(2)
C19 0.063(7) 0.060(6) 0.049(5) -0.026(5) 0.004(5) -0.014(5)
C21 0.028(4) 0.051(5) 0.038(4) -0.010(4) 0.000(3) -0.007(3)
O8 0.096(7) 0.055(4) 0.054(4) -0.003(3) -0.049(5) -0.026(4)
C20 0.109(12) 0.062(7) 0.053(6) -0.001(5) -0.027(7) 0.000(7)
O10 0.069(14) 0.17(3) 0.091(15) 0.019(16) -0.031(12) -0.071(17)
C22 0.065(14) 0.063(13) 0.076(15) -0.019(12) -0.038(12) 0.000(11)
_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
Y1 O2 2.352(3) 2_665 ?
Y1 O3 2.320(3) . ?
Y1 O1 2.338(3) . ?
Y1 O7 2.342(3) . ?
Y1 O4 2.351(3) . ?
Y1 N4 2.475(3) . ?
Y1 N2 2.448(3) . ?
Y1 N6 2.495(3) . ?
O2 C12 1.268(5) . ?
O3 C14 1.412(5) . ?
O3 B2 1.503(5) . ?
O1 C10 1.261(5) . ?
O7 H7A 0.856(10) . ?
O7 H7B 0.855(10) . ?
O7 C18 1.420(14) . ?
O7 C19 1.505(11) . ?
O4 C15 1.421(5) . ?
O4 B2 1.486(5) . ?
O5 C16 1.407(6) . ?
O5 B2 1.438(6) . ?
O6 C17 1.417(6) . ?
O6 B2 1.449(6) . ?
N3 N4 1.356(5) . ?
N3 C4 1.340(5) . ?
N3 B1 1.549(5) . ?
N4 C6 1.339(5) . ?
N5 N6 1.362(5) . ?
N5 C7 1.349(5) . ?
N5 B1 1.548(5) . ?
N1 N2 1.360(5) . ?
N1 C1 1.344(5) . ?
N1 B1 1.538(5) . ?
N2 C3 1.347(5) . ?
N6 C9 1.343(5) . ?
C11 C12 1.400(5) . ?
C11 C10 1.409(5) . ?
C11 C13 1.495(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C12 C10 1.525(5) 2_665 ?
C1 H1 0.9300 . ?
C1 C2 1.372(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.388(6) . ?
C8 H8 0.9300 . ?
C8 C7 1.366(6) . ?
C8 C9 1.398(6) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C6 C5 1.390(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.385(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C9 H9 0.9300 . ?
C4 H4 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C3 H3 0.9300 . ?
B1 H1A 0.9800 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
O11 H11 0.8200 . ?
O11 C23 1.380(13) . ?
O12 H12 0.8200 . ?
O12 C24 1.299(13) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O9 H9A 0.8200 . ?
O9 C21 1.429(11) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
O8 H8A 0.8200 . ?
O8 C20 1.337(17) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
O10 H10 0.8200 . ?
O10 C22 1.38(4) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Y1 N4 123.33(10) 2_665 . ?
O2 Y1 N2 76.67(10) 2_665 . ?
O2 Y1 N6 141.56(10) 2_665 . ?
O3 Y1 O2 133.94(9) . 2_665 ?
O3 Y1 O1 93.65(10) . . ?
O3 Y1 O7 101.66(10) . . ?
O3 Y1 O4 56.86(9) . . ?
O3 Y1 N4 84.20(10) . . ?
O3 Y1 N2 149.39(10) . . ?
O3 Y1 N6 77.32(10) . . ?
O1 Y1 O2 67.05(10) . 2_665 ?
O1 Y1 O7 142.54(10) . . ?
O1 Y1 O4 80.27(10) . . ?
O1 Y1 N4 71.29(10) . . ?
O1 Y1 N2 101.17(10) . . ?
O1 Y1 N6 144.11(10) . . ?
O7 Y1 O2 77.92(10) . 2_665 ?
O7 Y1 O4 80.00(10) . . ?
O7 Y1 N4 143.60(10) . . ?
O7 Y1 N2 82.56(11) . . ?
O7 Y1 N6 73.15(11) . . ?
O4 Y1 O2 78.23(9) . 2_665 ?
O4 Y1 N4 129.84(10) . . ?
O4 Y1 N2 151.89(10) . . ?
O4 Y1 N6 119.93(10) . . ?
N4 Y1 N6 73.26(11) . . ?
N2 Y1 N4 75.60(11) . . ?
N2 Y1 N6 74.98(11) . . ?
C12 O2 Y1 120.7(2) . 2_665 ?
C14 O3 Y1 138.4(2) . . ?
C14 O3 B2 117.6(3) . . ?
B2 O3 Y1 103.9(2) . . ?
C10 O1 Y1 121.1(2) . . ?
Y1 O7 H7A 121.9(19) . . ?
Y1 O7 H7B 120.1(18) . . ?
C18 O7 Y1 126.0(5) . . ?
C18 O7 H7A 107(2) . . ?
C19 O7 Y1 129.0(5) . . ?
C19 O7 H7B 105.7(19) . . ?
C15 O4 Y1 139.7(2) . . ?
C15 O4 B2 117.1(3) . . ?
B2 O4 Y1 103.1(2) . . ?
C16 O5 B2 118.1(3) . . ?
C17 O6 B2 118.8(3) . . ?
N4 N3 B1 121.8(3) . . ?
C4 N3 N4 110.6(3) . . ?
C4 N3 B1 127.6(3) . . ?
N3 N4 Y1 123.5(2) . . ?
C6 N4 Y1 130.7(3) . . ?
C6 N4 N3 105.5(3) . . ?
N6 N5 B1 120.8(3) . . ?
C7 N5 N6 110.3(3) . . ?
C7 N5 B1 128.8(3) . . ?
N2 N1 B1 122.2(3) . . ?
C1 N1 N2 109.7(3) . . ?
C1 N1 B1 128.1(3) . . ?
N1 N2 Y1 123.9(2) . . ?
C3 N2 Y1 130.2(3) . . ?
C3 N2 N1 105.8(3) . . ?
N5 N6 Y1 123.8(2) . . ?
C9 N6 Y1 130.7(3) . . ?
C9 N6 N5 105.3(3) . . ?
C12 C11 C10 117.5(4) . . ?
C12 C11 C13 120.7(4) . . ?
C10 C11 C13 121.7(4) . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C12 C11 124.1(4) . . ?
O2 C12 C10 114.9(3) . 2_665 ?
C11 C12 C10 121.0(3) . 2_665 ?
N1 C1 H1 125.4 . . ?
N1 C1 C2 109.2(4) . . ?
C2 C1 H1 125.4 . . ?
C1 C2 H2 127.8 . . ?
C1 C2 C3 104.4(3) . . ?
C3 C2 H2 127.8 . . ?
C7 C8 H8 127.7 . . ?
C7 C8 C9 104.5(3) . . ?
C9 C8 H8 127.7 . . ?
N5 C7 C8 108.7(3) . . ?
N5 C7 H7 125.6 . . ?
C8 C7 H7 125.6 . . ?
N4 C6 H6 124.3 . . ?
N4 C6 C5 111.4(4) . . ?
C5 C6 H6 124.3 . . ?
O1 C10 C11 123.6(4) . . ?
O1 C10 C12 114.9(3) . 2_665 ?
C11 C10 C12 121.4(3) . 2_665 ?
C6 C5 H5 128.0 . . ?
C4 C5 C6 104.0(4) . . ?
C4 C5 H5 128.0 . . ?
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 . . ?
N6 C9 C8 111.1(4) . . ?
N6 C9 H9 124.4 . . ?
C8 C9 H9 124.4 . . ?
N3 C4 C5 108.5(4) . . ?
N3 C4 H4 125.8 . . ?
C5 C4 H4 125.8 . . ?
O4 C15 H15A 109.5 . . ?
O4 C15 H15B 109.5 . . ?
O4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C3 C2 110.9(4) . . ?
N2 C3 H3 124.5 . . ?
C2 C3 H3 124.5 . . ?
N3 B1 H1A 109.9 . . ?
N5 B1 N3 108.2(3) . . ?
N5 B1 H1A 109.9 . . ?
N1 B1 N3 109.2(3) . . ?
N1 B1 N5 109.8(3) . . ?
N1 B1 H1A 109.9 . . ?
O5 C16 H16A 109.5 . . ?
O5 C16 H16B 109.5 . . ?
O5 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O6 C17 H17A 109.5 . . ?
O6 C17 H17B 109.5 . . ?
O6 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 O11 H11 109.5 . . ?
C24 O12 H12 109.5 . . ?
O4 B2 O3 96.1(3) . . ?
O5 B2 O3 114.0(4) . . ?
O5 B2 O4 115.6(3) . . ?
O5 B2 O6 104.1(3) . . ?
O6 B2 O3 113.7(3) . . ?
O6 B2 O4 113.7(4) . . ?
O12 C24 H24A 109.5 . . ?
O12 C24 H24B 109.5 . . ?
O12 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O11 C23 H23A 109.5 . . ?
O11 C23 H23B 109.5 . . ?
O11 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O7 C18 H18A 109.5 . . ?
O7 C18 H18B 109.5 . . ?
O7 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 O9 H9A 109.5 . . ?
O7 C19 H19A 109.5 . . ?
O7 C19 H19B 109.5 . . ?
O7 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O9 C21 H21A 109.5 . . ?
O9 C21 H21B 109.5 . . ?
O9 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 O8 H8A 109.5 . . ?
O8 C20 H20A 109.5 . . ?
O8 C20 H20B 109.5 . . ?
O8 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 O10 H10 109.5 . . ?
O10 C22 H22A 109.5 . . ?
O10 C22 H22B 109.5 . . ?
O10 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
_shelx_res_file
;
TITL 4-Y-MeOH_a.res in P-1
4-y-meoh.res
created by SHELXL-2016/6 at 17:51:55 on 19-Jun-2017
REM Old TITL 4-Y-MeOH in P-1 #2
REM SHELXT solution in P-1
REM R1 0.113, Rweak 0.010, Alpha 0.045, Orientation as input
REM Formula found by SHELXT: C28 B N4 O7 Y
CELL 1.54184 10.302582 11.881681 13.864562 71.1833 81.8238 87.7034
ZERR 1 0.000779 0.000727 0.001063 0.0062 0.0064 0.0055
LATT 1
SFAC C H B N O Y
UNIT 40.5 76 4 12 18.5 2
DFIX 0.85 0.01 O7 H7a
DFIX 0.85 0.01 O7 H7b
DANG 1.873734 0.02 C18 H7a
DANG 2.911315 0.02 Y1 H7a
DANG 1.932896 0.02 C19 H7b
DANG 2.879394 0.02 Y1 H7b
L.S. 10
PLAN 10
FREE B2 Y1
BOND $H
LIST 6
fmap 2
acta
OMIT 0 -1 2
REM
REM
REM
WGHT 0.107000 0.611000
FVAR 0.61389
Y1 6 0.217098 0.233714 0.182633 11.00000 0.01860 0.02662 =
0.03114 -0.00553 -0.00227 -0.00335
O2 5 0.694270 0.577945 -0.157283 11.00000 0.02326 0.02807 =
0.03977 -0.00873 0.00038 -0.00606
O3 5 0.301875 0.042748 0.223681 11.00000 0.02367 0.02730 =
0.04410 -0.00804 -0.00855 -0.00097
O1 5 0.360799 0.303708 0.029259 11.00000 0.02712 0.03449 =
0.03250 -0.00982 0.00543 -0.00875
O7 5 0.162754 0.255378 0.345565 11.00000 0.02919 0.04367 =
0.03120 -0.01041 -0.00065 -0.00521
PART 1
H7A 2 0.218636 0.279901 0.374587 10.50000 -1.50000
PART 0
PART 2
H7B 2 0.119875 0.200622 0.394360 10.50000 -1.50000
PART 0
O4 5 0.418398 0.183416 0.246563 11.00000 0.02035 0.03338 =
0.04294 -0.01102 -0.00789 -0.00326
O5 5 0.542600 0.024333 0.195588 11.00000 0.02652 0.04017 =
0.05252 -0.01599 -0.00747 0.00285
O6 5 0.443671 -0.020357 0.361213 11.00000 0.03221 0.03989 =
0.04603 -0.00699 -0.01015 0.00194
N3 4 -0.002132 0.183251 0.037819 11.00000 0.02568 0.03094 =
0.03155 -0.00740 -0.00328 -0.00341
N4 4 0.127453 0.180155 0.046677 11.00000 0.02443 0.02825 =
0.03733 -0.00794 -0.00288 -0.00331
N5 4 -0.093341 0.114792 0.225076 11.00000 0.01943 0.03257 =
0.03386 -0.00805 -0.00322 -0.00216
N1 4 -0.084986 0.333859 0.124114 11.00000 0.02217 0.03023 =
0.03439 -0.00481 -0.00653 0.00057
N2 4 0.030738 0.367194 0.143595 11.00000 0.02414 0.02834 =
0.03322 -0.00566 -0.00152 -0.00464
N6 4 0.019099 0.107377 0.267913 11.00000 0.02454 0.03551 =
0.02997 -0.00190 -0.00522 -0.00391
C11 1 0.534995 0.429123 -0.071143 11.00000 0.02732 0.03183 =
0.03687 -0.00934 0.00160 -0.00616
C14 1 0.268965 -0.069753 0.219707 11.00000 0.03559 0.03566 =
0.06756 -0.01421 -0.01846 -0.00334
AFIX 137
H14A 2 0.266021 -0.127460 0.286956 11.00000 -1.50000
H14B 2 0.333809 -0.092535 0.172600 11.00000 -1.50000
H14C 2 0.184690 -0.065747 0.196864 11.00000 -1.50000
AFIX 0
C12 1 0.602890 0.534020 -0.084474 11.00000 0.02185 0.02898 =
0.03182 -0.00599 -0.00173 -0.00261
C1 1 -0.169308 0.425125 0.110274 11.00000 0.02558 0.03793 =
0.03407 -0.00366 -0.00255 0.00426
AFIX 43
H1 2 -0.254677 0.423505 0.096168 11.00000 -1.20000
AFIX 0
C2 1 -0.109448 0.521080 0.120261 11.00000 0.03605 0.02964 =
0.04327 -0.00496 -0.00207 0.00472
AFIX 43
H2 2 -0.144464 0.595999 0.114357 11.00000 -1.20000
AFIX 0
C8 1 -0.123191 -0.036640 0.369030 11.00000 0.03060 0.03540 =
0.03485 0.00044 0.00018 -0.00783
AFIX 43
H8 2 -0.159336 -0.101434 0.423123 11.00000 -1.20000
AFIX 0
C7 1 -0.178805 0.029119 0.284861 11.00000 0.02401 0.03068 =
0.03853 -0.01004 0.00118 -0.00581
AFIX 43
H7 2 -0.261877 0.016826 0.271076 11.00000 -1.20000
AFIX 0
C6 1 0.188395 0.155462 -0.036074 11.00000 0.03504 0.03147 =
0.03587 -0.01235 0.00142 -0.00166
AFIX 43
H6 2 0.278765 0.148342 -0.050210 11.00000 -1.20000
AFIX 0
C10 1 0.431834 0.394149 0.011046 11.00000 0.02466 0.02758 =
0.03233 -0.00735 -0.00162 -0.00318
C5 1 0.099461 0.141818 -0.098169 11.00000 0.04525 0.03659 =
0.03721 -0.01453 -0.00211 -0.00568
AFIX 43
H5 2 0.117035 0.124345 -0.159455 11.00000 -1.20000
AFIX 0
C13 1 0.569288 0.359290 -0.143572 11.00000 0.05022 0.04686 =
0.04960 -0.02291 0.01563 -0.01670
AFIX 137
H13A 2 0.569730 0.410909 -0.213033 11.00000 -1.50000
H13B 2 0.505584 0.297151 -0.129013 11.00000 -1.50000
H13C 2 0.654569 0.324964 -0.135183 11.00000 -1.50000
AFIX 0
C9 1 0.000228 0.015324 0.355594 11.00000 0.02885 0.04024 =
0.03374 -0.00030 -0.00577 -0.00296
AFIX 43
H9 2 0.061275 -0.010465 0.401370 11.00000 -1.20000
AFIX 0
C4 1 -0.021333 0.160273 -0.047614 11.00000 0.04157 0.03795 =
0.03249 -0.01038 -0.00769 -0.00849
AFIX 43
H4 2 -0.102127 0.157238 -0.069279 11.00000 -1.20000
AFIX 0
C15 1 0.524076 0.238299 0.270481 11.00000 0.02888 0.03677 =
0.05756 -0.01404 -0.01340 -0.00199
AFIX 137
H15A 2 0.604229 0.225500 0.230860 11.00000 -1.50000
H15B 2 0.531036 0.204358 0.342439 11.00000 -1.50000
H15C 2 0.508349 0.322114 0.254300 11.00000 -1.50000
AFIX 0
C3 1 0.015139 0.481112 0.141159 11.00000 0.03348 0.03014 =
0.03339 -0.00838 -0.00065 -0.00260
AFIX 43
H3 2 0.079283 0.526864 0.152028 11.00000 -1.20000
AFIX 0
B1 3 -0.107455 0.208550 0.119649 11.00000 0.02217 0.03281 =
0.02930 -0.00604 -0.00415 -0.00215
AFIX 13
H1A 2 -0.195130 0.203067 0.101773 11.00000 -1.20000
AFIX 0
C16 1 0.556871 0.080951 0.088504 11.00000 0.03120 0.05348 =
0.05209 -0.02613 -0.00683 0.00387
AFIX 137
H16A 2 0.633796 0.051595 0.056721 11.00000 -1.50000
H16B 2 0.565387 0.165194 0.073832 11.00000 -1.50000
H16C 2 0.481164 0.064691 0.061900 11.00000 -1.50000
AFIX 0
C17 1 0.349440 -0.010348 0.442979 11.00000 0.03653 0.05046 =
0.04430 -0.00024 -0.01047 0.00258
AFIX 137
H17A 2 0.327203 0.071762 0.431406 11.00000 -1.50000
H17B 2 0.385094 -0.041302 0.506657 11.00000 -1.50000
H17C 2 0.272160 -0.054720 0.446290 11.00000 -1.50000
AFIX 0
O11 5 -0.067061 0.401596 0.565917 10.50000 0.07249 0.07265 =
0.02620 -0.02366 -0.00154 -0.03084
AFIX 147
H11 2 -0.004915 0.406337 0.520677 10.50000 -1.50000
AFIX 0
O12 5 0.437639 0.226397 0.600610 10.50000 0.14916 0.04626 =
0.04254 -0.01515 -0.04121 0.07213
AFIX 147
H12 2 0.515578 0.210383 0.602598 10.50000 -1.50000
AFIX 0
B2 3 0.431488 0.055034 0.257396 11.00000 0.02264 0.03582 =
0.04437 -0.01165 -0.01024 0.00044
C24 1 0.390765 0.258616 0.679672 10.50000 0.08479 0.01673 =
0.05197 -0.01172 -0.00575 0.01156
AFIX 137
H24A 2 0.297054 0.249980 0.691468 10.50000 -1.50000
H24B 2 0.413594 0.340214 0.666745 10.50000 -1.50000
H24C 2 0.426997 0.209472 0.739244 10.50000 -1.50000
AFIX 0
C23 1 -0.026101 0.351042 0.661008 10.50000 0.07965 0.04884 =
0.02580 -0.01174 -0.00167 -0.02002
AFIX 137
H23A 2 0.063297 0.373567 0.657647 10.50000 -1.50000
H23B 2 -0.032493 0.266041 0.680492 10.50000 -1.50000
H23C 2 -0.080611 0.378348 0.711040 10.50000 -1.50000
AFIX 0
PART 1
C18 1 0.036228 0.280317 0.389339 10.50000 0.06238 0.06642 =
0.04787 -0.01018 -0.00561 -0.00050
AFIX 137
H18A 2 -0.018167 0.311150 0.336011 10.50000 -1.50000
H18B 2 0.043572 0.338073 0.423327 10.50000 -1.50000
H18C 2 -0.002283 0.208593 0.438281 10.50000 -1.50000
AFIX 0
PART 0
PART 2
O9 5 -0.077352 0.246914 0.454567 10.50000 0.02442 0.04747 =
0.04217 -0.01752 -0.00166 -0.00488
AFIX 147
H9A 2 -0.042666 0.300868 0.466735 10.50000 -1.50000
AFIX 0
C19 1 0.234575 0.322921 0.396967 10.50000 0.06322 0.06014 =
0.04894 -0.02555 0.00441 -0.01380
AFIX 137
H19A 2 0.315804 0.283885 0.413266 10.50000 -1.50000
H19B 2 0.181558 0.325474 0.459034 10.50000 -1.50000
H19C 2 0.252167 0.402478 0.351382 10.50000 -1.50000
AFIX 0
C21 1 -0.183198 0.293423 0.397233 10.50000 0.02792 0.05054 =
0.03794 -0.00974 -0.00050 -0.00678
AFIX 137
H21A 2 -0.158159 0.369133 0.347251 10.50000 -1.50000
H21B 2 -0.258736 0.302959 0.443103 10.50000 -1.50000
H21C 2 -0.203819 0.239426 0.362821 10.50000 -1.50000
AFIX 0
PART 0
PART 1
O8 5 0.309153 0.333743 0.448953 10.50000 0.09628 0.05483 =
0.05399 -0.00255 -0.04921 -0.02589
AFIX 147
H8A 2 0.362352 0.292722 0.483712 10.50000 -1.50000
AFIX 0
C20 1 0.340883 0.448570 0.424277 10.50000 0.10880 0.06183 =
0.05294 -0.00121 -0.02674 0.00038
AFIX 137
H20A 2 0.296735 0.494547 0.367923 10.50000 -1.50000
H20B 2 0.433965 0.458398 0.404646 10.50000 -1.50000
H20C 2 0.314728 0.475202 0.482549 10.50000 -1.50000
AFIX 0
O10 5 -0.303245 0.368447 0.505620 10.25000 0.06857 0.16944 =
0.09078 0.01890 -0.03058 -0.07051
AFIX 147
H10 2 -0.327921 0.427729 0.520914 10.25000 -1.50000
AFIX 0
C22 1 -0.300575 0.391803 0.401295 10.25000 0.06517 0.06305 =
0.07555 -0.01933 -0.03809 -0.00040
AFIX 137
H22A 2 -0.233956 0.450180 0.364718 10.25000 -1.50000
H22B 2 -0.384325 0.421521 0.381927 10.25000 -1.50000
H22C 2 -0.281585 0.319973 0.384586 10.25000 -1.50000
AFIX 0
HKLF 4
REM 4-Y-MeOH_a.res in P-1
REM R1 = 0.0562 for 5445 Fo > 4sig(Fo) and 0.0639 for all 6215 data
REM 429 parameters refined using 6 restraints
END
WGHT 0.1072 0.6111
REM Highest difference peak 1.546, deepest hole -1.176, 1-sigma level 0.131
Q1 1 0.4736 0.2401 0.6105 11.00000 0.05 1.55
Q2 1 0.3837 0.2008 0.6211 11.00000 0.05 1.35
Q3 1 0.2177 0.1814 0.1486 11.00000 0.05 1.26
Q4 1 0.2125 0.2848 0.2191 11.00000 0.05 1.12
Q5 1 0.2395 0.1652 0.2405 11.00000 0.05 1.00
Q6 1 -0.0075 0.3821 0.5615 11.00000 0.05 1.00
Q7 1 0.1944 0.3036 0.1259 11.00000 0.05 0.92
Q8 1 -0.3384 0.3941 0.5814 11.00000 0.05 0.55
Q9 1 0.7248 0.6562 -0.1464 11.00000 0.05 0.52
Q10 1 0.2881 0.3662 0.4901 11.00000 0.05 0.46
;
_shelx_res_checksum 42856
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.778
# start Validation Reply Form
_vrf_PLAT077_4-y-meoh
;
PROBLEM: Unitcell contains non-integer number of atoms .. Please Check
RESPONSE: Due to the disorder and partial occupency of a methanol molecule .
;
_vrf_PLAT216_4-y-meoh
;
PROBLEM: Disordered O12 (An/Solv) ADP max/min Ratio 5.1 Note
RESPONSE: Due to a residual disorder on a solvent molecule that could
not be modelled.
;
_vrf_PLAT234_4-y-meoh
;
PROBLEM: Large Hirshfeld Difference O7 -- C18 .. 0.17 Ang.
RESPONSE: Due to disorder on a coordinated methanol molecule that could
not be better modelled.
;
_vrf_PLAT341_4-y-meoh
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0061 Ang.
RESPONSE: ...
;
_vrf_PLAT369_4-y-meoh
;
PROBLEM: Long C(sp2)-C(sp2) Bond C10 - C12_a .. 1.53 Ang.
RESPONSE: Consequence of the heavy atoms and a partial disorder.
;
_vrf_PLAT911_4-y-meoh
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 17 Report
RESPONSE: Not all reflections are measured as some were in
the detector rejection region.
;
_vrf_PLAT934_4-y-meoh
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers .... 1 Check
RESPONSE: Due to one reflexion at 9.91. No obvious reason for wy the
intensity should be an error. Refinement was continued with this reflexion in teh dataset.
;
_vrf_PLAT971_4-y-meoh
;
PROBLEM: Check Calcd Residual Density 0.46A From O12 1.59 eA-3
RESPONSE: Due to a residual disorder that could notbe modelled
;
_vrf_PLAT976_4-y-meoh
;
PROBLEM: Check Calcd Residual Density 0.96A From O7 -0.47 eA-3
RESPONSE: Due to a residual disorder that could notbe modelled
;
# 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_1-y-2ch2cl2
_database_code_depnum_ccdc_archive 'CCDC 1566107'
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_audit_creation_date 2017-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C42 H40 B4 Cl2 N24 O4 Y2, 2(C H2 Cl2)'
_chemical_formula_sum 'C44 H44 B4 Cl6 N24 O4 Y2'
_chemical_formula_weight 1406.79
_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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 13.940(3)
_cell_length_b 15.052(3)
_cell_length_c 14.280(3)
_cell_angle_alpha 90
_cell_angle_beta 107.57(3)
_cell_angle_gamma 90
_cell_volume 2856.4(11)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2162
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 32.089
_cell_measurement_theta_min 0.407
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.369
_exptl_absorpt_correction_T_max 0.4343
_exptl_absorpt_correction_T_min 0.3098
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1245 before and 0.0842 after correction.
The Ratio of minimum to maximum transmission is 0.7133.
The \l/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'light purple'
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary purple
_exptl_crystal_density_diffrn 1.636
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1416
_exptl_crystal_size_max 0.01
_exptl_crystal_size_mid 0.01
_exptl_crystal_size_min 0.005
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0901
_diffrn_reflns_av_unetI/netI 0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.720
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 55283
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.720
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 32.849
_diffrn_reflns_theta_min 1.789
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_device_type 'ADSC Quantum 210r'
_diffrn_measurement_method 'Phi Scan'
_diffrn_radiation_monochromator 'Silicon Double Crystal'
_diffrn_radiation_type Synchrotron
_diffrn_radiation_wavelength 0.71080
_diffrn_radiation_source 'MX1 Beamline Australian Synchrotron'
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6344
_reflns_number_total 7662
_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 'XDS (Kabsch, 1993)'
_computing_data_collection 'BluIce (McPhillips, 2002)'
_computing_data_reduction 'XDS (Kabsch, 1993)'
_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 'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max 1.146
_refine_diff_density_min -1.115
_refine_diff_density_rms 0.123
_refine_ls_extinction_coef 0.0185(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 380
_refine_ls_number_reflns 7662
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0589
_refine_ls_R_factor_gt 0.0454
_refine_ls_restrained_S_all 1.049
_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^)+(0.0658P)^2^+3.6926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1156
_refine_ls_wR_factor_ref 0.1241
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
B1(H1A), B2(H2A)
2.b Secondary CH2 refined with riding coordinates:
C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
C9(H9), C7(H7), C8(H8), C12(H12), C10(H10), C6(H6), C11(H11), C3(H3), C5(H5),
C13(H13), C1(H1), C18(H18), C2(H2), C4(H4), C15(H15), C17(H17), C14(H14),
C16(H16)
;
_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
Y1 Y 0.58243(2) 0.63029(2) 0.27497(2) 0.01084(9) Uani 1 1 d . . . . .
Cl1 Cl 0.56552(6) 0.67074(5) 0.63096(5) 0.02160(16) Uani 1 1 d . . . . .
Cl3 Cl 0.26895(13) 0.66128(11) 0.36348(9) 0.0716(4) Uani 1 1 d . . . . .
Cl2 Cl 0.28026(13) 0.83972(9) 0.44431(13) 0.0740(5) Uani 1 1 d . . . . .
O2 O 0.47106(15) 0.50276(13) 0.67133(12) 0.0145(4) Uani 1 1 d . . . . .
O1 O 0.57195(16) 0.64191(12) 0.43022(13) 0.0160(4) Uani 1 1 d . . . . .
N7 N 0.45281(18) 0.75446(15) 0.07799(15) 0.0155(4) Uani 1 1 d . . . . .
N8 N 0.53388(18) 0.70032(15) 0.11275(15) 0.0148(4) Uani 1 1 d . . . . .
N5 N 0.73116(18) 0.52563(15) 0.16980(15) 0.0137(4) Uani 1 1 d . . . . .
N3 N 0.80729(18) 0.67182(16) 0.24281(15) 0.0158(4) Uani 1 1 d . . . . .
N6 N 0.63605(18) 0.52436(15) 0.17730(15) 0.0133(4) Uani 1 1 d . . . . .
N1 N 0.81789(18) 0.53604(15) 0.34407(15) 0.0154(4) Uani 1 1 d . . . . .
N2 N 0.74110(18) 0.55738(15) 0.38018(15) 0.0146(4) Uani 1 1 d . . . . .
N12 N 0.51648(19) 0.77783(16) 0.29397(15) 0.0178(5) Uani 1 1 d . . . . .
N4 N 0.72835(18) 0.71389(15) 0.26102(15) 0.0152(4) Uani 1 1 d . . . . .
N9 N 0.33730(19) 0.68177(16) 0.15468(16) 0.0172(5) Uani 1 1 d . . . . .
N10 N 0.39747(19) 0.61320(16) 0.19987(16) 0.0162(4) Uani 1 1 d . . . . .
N11 N 0.43717(19) 0.81749(16) 0.22976(16) 0.0177(5) Uani 1 1 d . . . . .
C9 C 0.5815(2) 0.47428(18) 0.10523(18) 0.0156(5) Uani 1 1 d . . . . .
H9 H 0.513596 0.461439 0.093432 0.019 Uiso 1 1 calc R . . . .
C7 C 0.7343(2) 0.47816(18) 0.09370(18) 0.0166(5) Uani 1 1 d . . . . .
H7 H 0.790613 0.469246 0.072859 0.020 Uiso 1 1 calc R . . . .
C8 C 0.6402(2) 0.44394(19) 0.05018(19) 0.0194(5) Uani 1 1 d . . . . .
H8 H 0.620246 0.407733 -0.005102 0.023 Uiso 1 1 calc R . . . .
C12 C 0.5798(2) 0.69616(19) 0.04535(18) 0.0170(5) Uani 1 1 d . . . . .
H12 H 0.638284 0.664267 0.050247 0.020 Uiso 1 1 calc R . . . .
C21 C 0.4885(2) 0.50570(17) 0.59282(17) 0.0135(5) Uani 1 1 d . . . . .
C10 C 0.4480(2) 0.78232(19) -0.00975(18) 0.0204(6) Uani 1 1 d . . . . .
H10 H 0.399238 0.819782 -0.049068 0.024 Uiso 1 1 calc R . . . .
C20 C 0.5296(2) 0.57880(17) 0.55937(18) 0.0156(5) Uani 1 1 d . . . . .
C19 C 0.5397(2) 0.57823(17) 0.46794(17) 0.0136(5) Uani 1 1 d . . . . .
C6 C 0.7395(2) 0.80066(19) 0.24573(19) 0.0196(5) Uani 1 1 d . . . . .
H6 H 0.695789 0.844921 0.252999 0.023 Uiso 1 1 calc R . . . .
C11 C 0.5279(2) 0.7464(2) -0.03347(19) 0.0205(6) Uani 1 1 d . . . . .
H11 H 0.543650 0.754495 -0.091678 0.025 Uiso 1 1 calc R . . . .
C3 C 0.7638(2) 0.51696(19) 0.46491(18) 0.0187(5) Uani 1 1 d . . . . .
H3 H 0.725011 0.519629 0.507635 0.022 Uiso 1 1 calc R . . . .
C5 C 0.8244(3) 0.8154(2) 0.2178(2) 0.0245(6) Uani 1 1 d . . . . .
H5 H 0.848946 0.869435 0.203131 0.029 Uiso 1 1 calc R . . . .
C13 C 0.2413(2) 0.6539(2) 0.1211(2) 0.0214(6) Uani 1 1 d . . . . .
H13 H 0.186609 0.688810 0.087948 0.026 Uiso 1 1 calc R . . . .
C1 C 0.8847(2) 0.48341(19) 0.4047(2) 0.0196(5) Uani 1 1 d . . . . .
H1 H 0.942696 0.460495 0.394583 0.024 Uiso 1 1 calc R . . . .
C18 C 0.5476(2) 0.8346(2) 0.3667(2) 0.0202(5) Uani 1 1 d . . . . .
H18 H 0.601886 0.824718 0.422527 0.024 Uiso 1 1 calc R . . . .
C2 C 0.8533(2) 0.4693(2) 0.4834(2) 0.0226(6) Uani 1 1 d . . . . .
H2 H 0.884451 0.435116 0.538411 0.027 Uiso 1 1 calc R . . . .
C4 C 0.8648(2) 0.7322(2) 0.2166(2) 0.0219(6) Uani 1 1 d . . . . .
H4 H 0.923103 0.719858 0.200189 0.026 Uiso 1 1 calc R . . . .
C15 C 0.3354(2) 0.5429(2) 0.1924(2) 0.0204(6) Uani 1 1 d . . . . .
H15 H 0.356168 0.486520 0.216959 0.024 Uiso 1 1 calc R . . . .
C17 C 0.4891(2) 0.9114(2) 0.3497(2) 0.0239(6) Uani 1 1 d . . . . .
H17 H 0.496274 0.961112 0.389984 0.029 Uiso 1 1 calc R . . . .
C14 C 0.2371(2) 0.5658(2) 0.1435(2) 0.0238(6) Uani 1 1 d . . . . .
H14 H 0.180518 0.529498 0.129054 0.029 Uiso 1 1 calc R . . . .
C16 C 0.4198(3) 0.8977(2) 0.2620(2) 0.0236(6) Uani 1 1 d . . . . .
H16 H 0.368980 0.936911 0.229680 0.028 Uiso 1 1 calc R . . . .
B1 B 0.8187(2) 0.5703(2) 0.2463(2) 0.0154(5) Uani 1 1 d . . . . .
H1A H 0.882173 0.553972 0.234561 0.018 Uiso 1 1 calc R . . . .
B2 B 0.3798(3) 0.7722(2) 0.1354(2) 0.0192(6) Uani 1 1 d . . . . .
H2A H 0.325083 0.810556 0.097391 0.023 Uiso 1 1 calc R . . . .
C22 C 0.3119(5) 0.7280(4) 0.4627(4) 0.080(2) Uani 1 1 d . . . . .
H22A H 0.384695 0.723295 0.485982 0.096 Uiso 1 1 calc R . . . .
H22B H 0.286436 0.705751 0.514320 0.096 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.01631(16) 0.01121(13) 0.00550(11) 0.00105(7) 0.00407(8) 0.00046(8)
Cl1 0.0356(4) 0.0179(3) 0.0150(3) -0.0053(2) 0.0131(3) -0.0073(3)
Cl3 0.1031(12) 0.0879(10) 0.0350(5) -0.0193(6) 0.0377(6) -0.0240(8)
Cl2 0.1039(12) 0.0499(7) 0.1020(11) 0.0118(7) 0.0819(10) 0.0084(7)
O2 0.0225(11) 0.0156(9) 0.0070(7) 0.0007(6) 0.0070(6) -0.0005(7)
O1 0.0258(12) 0.0138(9) 0.0108(8) 0.0006(6) 0.0088(7) -0.0015(7)
N7 0.0221(13) 0.0149(10) 0.0081(9) 0.0032(8) 0.0024(8) 0.0023(8)
N8 0.0179(13) 0.0152(10) 0.0105(9) 0.0018(8) 0.0032(7) 0.0014(8)
N5 0.0178(13) 0.0144(10) 0.0099(9) -0.0021(7) 0.0056(8) -0.0003(8)
N3 0.0186(13) 0.0172(11) 0.0120(9) -0.0018(8) 0.0050(8) -0.0040(8)
N6 0.0170(13) 0.0146(10) 0.0084(8) 0.0001(7) 0.0041(7) -0.0009(8)
N1 0.0158(13) 0.0167(11) 0.0111(9) -0.0026(8) 0.0002(7) -0.0003(8)
N2 0.0146(13) 0.0175(11) 0.0101(9) 0.0014(8) 0.0014(7) 0.0009(8)
N12 0.0276(14) 0.0163(11) 0.0088(9) 0.0007(8) 0.0043(8) 0.0041(9)
N4 0.0222(13) 0.0144(11) 0.0088(9) 0.0009(7) 0.0043(8) -0.0010(8)
N9 0.0193(14) 0.0214(12) 0.0111(9) -0.0012(8) 0.0047(8) 0.0020(9)
N10 0.0186(13) 0.0192(11) 0.0106(9) 0.0015(8) 0.0041(8) 0.0006(8)
N11 0.0229(14) 0.0160(11) 0.0137(10) 0.0012(8) 0.0049(8) 0.0049(8)
C9 0.0171(15) 0.0181(12) 0.0100(10) -0.0003(9) 0.0020(9) -0.0018(9)
C7 0.0232(16) 0.0167(12) 0.0111(10) -0.0034(9) 0.0069(9) 0.0020(9)
C8 0.0273(17) 0.0191(13) 0.0103(10) -0.0050(9) 0.0035(9) 0.0008(10)
C12 0.0202(15) 0.0211(13) 0.0104(10) 0.0014(9) 0.0058(9) -0.0030(10)
C21 0.0179(15) 0.0168(12) 0.0068(9) 0.0011(8) 0.0051(8) 0.0010(9)
C10 0.0324(18) 0.0167(13) 0.0091(10) 0.0052(9) 0.0020(9) -0.0012(11)
C20 0.0248(16) 0.0145(12) 0.0096(10) -0.0026(9) 0.0080(9) -0.0019(9)
C19 0.0198(14) 0.0136(11) 0.0087(10) 0.0023(8) 0.0065(8) 0.0008(9)
C6 0.0305(17) 0.0140(13) 0.0138(11) -0.0020(9) 0.0061(10) -0.0038(10)
C11 0.0293(17) 0.0226(14) 0.0092(10) 0.0029(9) 0.0052(10) -0.0041(11)
C3 0.0227(16) 0.0204(13) 0.0109(10) 0.0022(9) 0.0017(9) -0.0010(10)
C5 0.040(2) 0.0186(14) 0.0159(12) -0.0022(10) 0.0100(11) -0.0119(12)
C13 0.0146(16) 0.0354(16) 0.0133(11) -0.0046(10) 0.0032(9) 0.0014(11)
C1 0.0177(16) 0.0195(13) 0.0180(12) -0.0015(10) -0.0001(10) 0.0015(10)
C18 0.0267(17) 0.0201(14) 0.0140(11) -0.0037(10) 0.0063(10) 0.0003(11)
C2 0.0224(17) 0.0236(14) 0.0166(12) 0.0048(10) -0.0020(10) 0.0030(11)
C4 0.0282(18) 0.0233(14) 0.0169(12) -0.0041(10) 0.0107(10) -0.0104(11)
C15 0.0236(17) 0.0224(14) 0.0153(11) 0.0003(10) 0.0060(10) -0.0058(11)
C17 0.0267(18) 0.0210(14) 0.0247(13) -0.0075(11) 0.0087(11) 0.0020(11)
C14 0.0191(17) 0.0356(17) 0.0167(12) -0.0033(11) 0.0052(10) -0.0060(12)
C16 0.0307(18) 0.0180(13) 0.0229(13) -0.0029(11) 0.0095(11) 0.0063(11)
B1 0.0132(16) 0.0194(14) 0.0140(12) -0.0029(10) 0.0047(9) -0.0023(10)
B2 0.0232(18) 0.0184(15) 0.0139(12) 0.0010(10) 0.0025(10) 0.0055(11)
C22 0.107(5) 0.062(3) 0.047(3) -0.021(2) -0.013(3) 0.037(3)
_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
Y1 O2 2.3452(19) 3_666 ?
Y1 O1 2.2722(18) . ?
Y1 N8 2.447(2) . ?
Y1 N6 2.382(2) . ?
Y1 N2 2.519(2) . ?
Y1 N12 2.450(2) . ?
Y1 N4 2.451(2) . ?
Y1 N10 2.489(3) . ?
Cl1 C20 1.704(3) . ?
Cl3 C22 1.691(5) . ?
Cl2 C22 1.739(6) . ?
O2 C21 1.218(3) . ?
O1 C19 1.248(3) . ?
N7 N8 1.360(3) . ?
N7 C10 1.304(3) . ?
N7 B2 1.511(4) . ?
N8 C12 1.309(3) . ?
N5 N6 1.362(3) . ?
N5 C7 1.312(3) . ?
N5 B1 1.526(4) . ?
N3 N4 1.361(3) . ?
N3 C4 1.338(4) . ?
N3 B1 1.535(4) . ?
N6 C9 1.317(3) . ?
N1 N2 1.360(3) . ?
N1 C1 1.326(4) . ?
N1 B1 1.492(3) . ?
N2 C3 1.305(3) . ?
N12 N11 1.344(3) . ?
N12 C18 1.313(3) . ?
N4 C6 1.341(3) . ?
N9 N10 1.363(3) . ?
N9 C13 1.345(4) . ?
N9 B2 1.542(4) . ?
N10 C15 1.351(4) . ?
N11 C16 1.341(4) . ?
N11 B2 1.507(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.373(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.371(4) . ?
C8 H8 0.9300 . ?
C12 H12 0.9300 . ?
C12 C11 1.368(4) . ?
C21 C20 1.390(4) . ?
C21 C19 1.516(4) 3_666 ?
C10 H10 0.9300 . ?
C10 C11 1.369(4) . ?
C20 C19 1.355(3) . ?
C6 H6 0.9300 . ?
C6 C5 1.376(4) . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C3 C2 1.394(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.375(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.369(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.340(4) . ?
C18 H18 0.9300 . ?
C18 C17 1.394(4) . ?
C2 H2 0.9300 . ?
C4 H4 0.9300 . ?
C15 H15 0.9300 . ?
C15 C14 1.381(5) . ?
C17 H17 0.9300 . ?
C17 C16 1.346(4) . ?
C14 H14 0.9300 . ?
C16 H16 0.9300 . ?
B1 H1A 0.9800 . ?
B2 H2A 0.9800 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
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
O2 Y1 N8 130.77(7) 3_666 . ?
O2 Y1 N6 78.86(7) 3_666 . ?
O2 Y1 N2 75.02(7) 3_666 . ?
O2 Y1 N12 124.81(8) 3_666 . ?
O2 Y1 N4 144.96(7) 3_666 . ?
O2 Y1 N10 70.27(7) 3_666 . ?
O1 Y1 O2 68.05(6) . 3_666 ?
O1 Y1 N8 144.05(7) . . ?
O1 Y1 N6 138.31(7) . . ?
O1 Y1 N2 75.83(8) . . ?
O1 Y1 N12 71.66(7) . . ?
O1 Y1 N4 109.84(7) . . ?
O1 Y1 N10 93.72(8) . . ?
N8 Y1 N2 133.97(8) . . ?
N8 Y1 N12 73.05(7) . . ?
N8 Y1 N4 72.60(8) . . ?
N8 Y1 N10 71.47(8) . . ?
N6 Y1 N8 77.30(7) . . ?
N6 Y1 N2 71.55(7) . . ?
N6 Y1 N12 150.01(7) . . ?
N6 Y1 N4 83.18(8) . . ?
N6 Y1 N10 98.39(8) . . ?
N12 Y1 N2 128.33(8) . . ?
N12 Y1 N4 83.80(8) . . ?
N12 Y1 N10 76.51(8) . . ?
N4 Y1 N2 70.81(8) . . ?
N4 Y1 N10 142.69(7) . . ?
N10 Y1 N2 145.15(8) . . ?
C21 O2 Y1 120.25(17) . 3_666 ?
C19 O1 Y1 119.98(16) . . ?
N8 N7 B2 122.0(2) . . ?
C10 N7 N8 109.8(2) . . ?
C10 N7 B2 128.1(2) . . ?
N7 N8 Y1 124.44(16) . . ?
C12 N8 Y1 128.22(19) . . ?
C12 N8 N7 107.3(2) . . ?
N6 N5 B1 122.5(2) . . ?
C7 N5 N6 109.5(2) . . ?
C7 N5 B1 127.8(2) . . ?
N4 N3 B1 122.6(2) . . ?
C4 N3 N4 108.9(2) . . ?
C4 N3 B1 128.3(3) . . ?
N5 N6 Y1 121.44(16) . . ?
C9 N6 Y1 129.16(19) . . ?
C9 N6 N5 107.0(2) . . ?
N2 N1 B1 120.2(2) . . ?
C1 N1 N2 111.8(2) . . ?
C1 N1 B1 128.0(3) . . ?
N1 N2 Y1 121.79(15) . . ?
C3 N2 Y1 132.8(2) . . ?
C3 N2 N1 104.1(2) . . ?
N11 N12 Y1 125.87(17) . . ?
C18 N12 Y1 129.2(2) . . ?
C18 N12 N11 105.0(2) . . ?
N3 N4 Y1 121.03(16) . . ?
C6 N4 Y1 130.8(2) . . ?
C6 N4 N3 106.4(2) . . ?
N10 N9 B2 122.5(2) . . ?
C13 N9 N10 109.6(2) . . ?
C13 N9 B2 127.3(3) . . ?
N9 N10 Y1 122.35(18) . . ?
C15 N10 Y1 132.1(2) . . ?
C15 N10 N9 105.6(2) . . ?
N12 N11 B2 120.9(2) . . ?
C16 N11 N12 111.3(2) . . ?
C16 N11 B2 127.8(2) . . ?
N6 C9 H9 125.2 . . ?
N6 C9 C8 109.6(3) . . ?
C8 C9 H9 125.2 . . ?
N5 C7 H7 125.9 . . ?
N5 C7 C8 108.3(2) . . ?
C8 C7 H7 125.9 . . ?
C9 C8 H8 127.2 . . ?
C7 C8 C9 105.6(2) . . ?
C7 C8 H8 127.2 . . ?
N8 C12 H12 125.6 . . ?
N8 C12 C11 108.9(3) . . ?
C11 C12 H12 125.6 . . ?
O2 C21 C20 124.2(2) . . ?
O2 C21 C19 114.0(2) . 3_666 ?
C20 C21 C19 121.7(2) . 3_666 ?
N7 C10 H10 126.2 . . ?
N7 C10 C11 107.5(3) . . ?
C11 C10 H10 126.2 . . ?
C21 C20 Cl1 120.93(18) . . ?
C19 C20 Cl1 119.1(2) . . ?
C19 C20 C21 120.0(2) . . ?
O1 C19 C21 117.3(2) . 3_666 ?
O1 C19 C20 124.5(2) . . ?
C20 C19 C21 118.2(2) . 3_666 ?
N4 C6 H6 124.5 . . ?
N4 C6 C5 110.9(3) . . ?
C5 C6 H6 124.5 . . ?
C12 C11 C10 106.4(2) . . ?
C12 C11 H11 126.8 . . ?
C10 C11 H11 126.8 . . ?
N2 C3 H3 124.2 . . ?
N2 C3 C2 111.6(3) . . ?
C2 C3 H3 124.2 . . ?
C6 C5 H5 127.8 . . ?
C4 C5 C6 104.3(3) . . ?
C4 C5 H5 127.8 . . ?
N9 C13 H13 125.4 . . ?
N9 C13 C14 109.1(3) . . ?
C14 C13 H13 125.4 . . ?
N1 C1 H1 126.3 . . ?
N1 C1 C2 107.4(3) . . ?
C2 C1 H1 126.3 . . ?
N12 C18 H18 124.3 . . ?
N12 C18 C17 111.4(3) . . ?
C17 C18 H18 124.3 . . ?
C3 C2 H2 127.5 . . ?
C1 C2 C3 105.1(3) . . ?
C1 C2 H2 127.5 . . ?
N3 C4 C5 109.5(3) . . ?
N3 C4 H4 125.3 . . ?
C5 C4 H4 125.3 . . ?
N10 C15 H15 124.5 . . ?
N10 C15 C14 111.0(3) . . ?
C14 C15 H15 124.5 . . ?
C18 C17 H17 127.7 . . ?
C16 C17 C18 104.6(3) . . ?
C16 C17 H17 127.7 . . ?
C13 C14 C15 104.7(3) . . ?
C13 C14 H14 127.7 . . ?
C15 C14 H14 127.7 . . ?
N11 C16 C17 107.7(3) . . ?
N11 C16 H16 126.1 . . ?
C17 C16 H16 126.1 . . ?
N5 B1 N3 111.3(2) . . ?
N5 B1 H1A 109.6 . . ?
N3 B1 H1A 109.6 . . ?
N1 B1 N5 106.6(2) . . ?
N1 B1 N3 110.1(2) . . ?
N1 B1 H1A 109.6 . . ?
N7 B2 N9 107.4(2) . . ?
N7 B2 H2A 110.0 . . ?
N9 B2 H2A 110.0 . . ?
N11 B2 N7 107.6(3) . . ?
N11 B2 N9 111.6(2) . . ?
N11 B2 H2A 110.0 . . ?
Cl3 C22 Cl2 116.0(3) . . ?
Cl3 C22 H22A 108.3 . . ?
Cl3 C22 H22B 108.3 . . ?
Cl2 C22 H22A 108.3 . . ?
Cl2 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
_shelx_res_file
;
TITL 1-Y-2CH2Cl2_a.res in P2(1)/n
1-y-2ch2cl2.res
created by SHELXL-2016/6 at 17:41:38 on 16-Jun-2017
REM Old TITL 1-Y-2CH2Cl2 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.119, Rweak 0.007, Alpha 0.027, Orientation as input
REM Formula found by SHELXT: C31 B N4 O2 Cl3 Y
CELL 0.71073 13.94 15.052 14.28 90 107.575 90
ZERR 2 0.0028 0.003 0.0029 0 0.03 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B N O Cl Y
UNIT 88 88 8 48 8 12 4
L.S. 4
PLAN 10
BOND $H
LIST 6
fmap 2
acta 52
REM
REM
REM
WGHT 0.065800 3.692600
EXTI 0.018533
FVAR 0.43326
Y1 7 0.582433 0.630292 0.274969 11.00000 0.01631 0.01121 =
0.00550 0.00105 0.00407 0.00046
CL1 6 0.565519 0.670743 0.630963 11.00000 0.03559 0.01786 =
0.01498 -0.00531 0.01310 -0.00734
CL3 6 0.268954 0.661285 0.363480 11.00000 0.10309 0.08791 =
0.03501 -0.01928 0.03767 -0.02399
CL2 6 0.280261 0.839723 0.444306 11.00000 0.10387 0.04992 =
0.10200 0.01184 0.08193 0.00836
O2 5 0.471056 0.502758 0.671330 11.00000 0.02250 0.01565 =
0.00697 0.00073 0.00696 -0.00050
O1 5 0.571946 0.641909 0.430222 11.00000 0.02575 0.01381 =
0.01077 0.00064 0.00879 -0.00150
N7 4 0.452812 0.754461 0.077994 11.00000 0.02211 0.01495 =
0.00809 0.00319 0.00242 0.00225
N8 4 0.533876 0.700323 0.112754 11.00000 0.01787 0.01517 =
0.01053 0.00175 0.00320 0.00140
N5 4 0.731164 0.525626 0.169799 11.00000 0.01781 0.01444 =
0.00989 -0.00213 0.00564 -0.00032
N3 4 0.807287 0.671818 0.242809 11.00000 0.01862 0.01718 =
0.01197 -0.00175 0.00499 -0.00399
N6 4 0.636046 0.524365 0.177302 11.00000 0.01700 0.01462 =
0.00838 0.00010 0.00409 -0.00092
N1 4 0.817893 0.536043 0.344069 11.00000 0.01583 0.01675 =
0.01109 -0.00264 0.00019 -0.00030
N2 4 0.741100 0.557381 0.380179 11.00000 0.01459 0.01746 =
0.01015 0.00140 0.00140 0.00093
N12 4 0.516481 0.777832 0.293965 11.00000 0.02760 0.01625 =
0.00885 0.00074 0.00426 0.00410
N4 4 0.728354 0.713888 0.261021 11.00000 0.02221 0.01445 =
0.00879 0.00092 0.00430 -0.00099
N9 4 0.337298 0.681772 0.154680 11.00000 0.01927 0.02140 =
0.01110 -0.00122 0.00466 0.00202
N10 4 0.397469 0.613204 0.199872 11.00000 0.01858 0.01919 =
0.01061 0.00147 0.00411 0.00060
N11 4 0.437175 0.817487 0.229763 11.00000 0.02290 0.01603 =
0.01370 0.00125 0.00491 0.00491
C9 1 0.581478 0.474285 0.105231 11.00000 0.01710 0.01813 =
0.01004 -0.00034 0.00196 -0.00182
AFIX 43
H9 2 0.513596 0.461439 0.093432 11.00000 -1.20000
AFIX 0
C7 1 0.734258 0.478156 0.093701 11.00000 0.02319 0.01674 =
0.01110 -0.00343 0.00692 0.00196
AFIX 43
H7 2 0.790613 0.469246 0.072859 11.00000 -1.20000
AFIX 0
C8 1 0.640158 0.443941 0.050178 11.00000 0.02730 0.01908 =
0.01035 -0.00501 0.00348 0.00075
AFIX 43
H8 2 0.620246 0.407733 -0.005102 11.00000 -1.20000
AFIX 0
C12 1 0.579831 0.696163 0.045346 11.00000 0.02022 0.02107 =
0.01045 0.00139 0.00578 -0.00298
AFIX 43
H12 2 0.638284 0.664267 0.050247 11.00000 -1.20000
AFIX 0
C21 1 0.488517 0.505699 0.592819 11.00000 0.01790 0.01679 =
0.00675 0.00108 0.00505 0.00104
C10 1 0.448012 0.782321 -0.009754 11.00000 0.03237 0.01674 =
0.00913 0.00523 0.00199 -0.00122
AFIX 43
H10 2 0.399238 0.819782 -0.049068 11.00000 -1.20000
AFIX 0
C20 1 0.529562 0.578802 0.559374 11.00000 0.02475 0.01449 =
0.00957 -0.00263 0.00802 -0.00187
C19 1 0.539679 0.578228 0.467937 11.00000 0.01984 0.01362 =
0.00873 0.00228 0.00650 0.00081
C6 1 0.739546 0.800662 0.245727 11.00000 0.03046 0.01402 =
0.01378 -0.00199 0.00608 -0.00382
AFIX 43
H6 2 0.695789 0.844921 0.252999 11.00000 -1.20000
AFIX 0
C11 1 0.527862 0.746373 -0.033465 11.00000 0.02927 0.02256 =
0.00918 0.00294 0.00521 -0.00410
AFIX 43
H11 2 0.543650 0.754495 -0.091678 11.00000 -1.20000
AFIX 0
C3 1 0.763767 0.516964 0.464905 11.00000 0.02266 0.02038 =
0.01091 0.00223 0.00169 -0.00101
AFIX 43
H3 2 0.725011 0.519629 0.507635 11.00000 -1.20000
AFIX 0
C5 1 0.824435 0.815432 0.217837 11.00000 0.04004 0.01858 =
0.01594 -0.00216 0.01005 -0.01195
AFIX 43
H5 2 0.848946 0.869435 0.203131 11.00000 -1.20000
AFIX 0
C13 1 0.241346 0.653867 0.121110 11.00000 0.01464 0.03545 =
0.01331 -0.00458 0.00322 0.00139
AFIX 43
H13 2 0.186609 0.688810 0.087948 11.00000 -1.20000
AFIX 0
C1 1 0.884685 0.483413 0.404747 11.00000 0.01771 0.01945 =
0.01801 -0.00151 -0.00009 0.00146
AFIX 43
H1 2 0.942696 0.460495 0.394583 11.00000 -1.20000
AFIX 0
C18 1 0.547636 0.834565 0.366726 11.00000 0.02666 0.02015 =
0.01399 -0.00374 0.00626 0.00027
AFIX 43
H18 2 0.601886 0.824718 0.422527 11.00000 -1.20000
AFIX 0
C2 1 0.853271 0.469310 0.483390 11.00000 0.02244 0.02355 =
0.01656 0.00481 -0.00203 0.00297
AFIX 43
H2 2 0.884451 0.435116 0.538411 11.00000 -1.20000
AFIX 0
C4 1 0.864831 0.732224 0.216638 11.00000 0.02820 0.02330 =
0.01686 -0.00407 0.01066 -0.01037
AFIX 43
H4 2 0.923103 0.719858 0.200189 11.00000 -1.20000
AFIX 0
C15 1 0.335432 0.542885 0.192428 11.00000 0.02356 0.02243 =
0.01533 0.00027 0.00602 -0.00576
AFIX 43
H15 2 0.356168 0.486520 0.216959 11.00000 -1.20000
AFIX 0
C17 1 0.489071 0.911436 0.349719 11.00000 0.02670 0.02098 =
0.02468 -0.00754 0.00870 0.00204
AFIX 43
H17 2 0.496274 0.961112 0.389984 11.00000 -1.20000
AFIX 0
C14 1 0.237082 0.565819 0.143530 11.00000 0.01906 0.03559 =
0.01668 -0.00328 0.00518 -0.00598
AFIX 43
H14 2 0.180518 0.529498 0.129054 11.00000 -1.20000
AFIX 0
C16 1 0.419778 0.897745 0.262041 11.00000 0.03071 0.01802 =
0.02289 -0.00291 0.00947 0.00632
AFIX 43
H16 2 0.368980 0.936911 0.229680 11.00000 -1.20000
AFIX 0
B1 3 0.818717 0.570344 0.246265 11.00000 0.01315 0.01941 =
0.01400 -0.00294 0.00465 -0.00226
AFIX 13
H1A 2 0.882173 0.553972 0.234561 11.00000 -1.20000
AFIX 0
B2 3 0.379799 0.772162 0.135405 11.00000 0.02322 0.01842 =
0.01386 0.00095 0.00255 0.00553
AFIX 13
H2A 2 0.325083 0.810556 0.097391 11.00000 -1.20000
AFIX 0
C22 1 0.311925 0.727981 0.462652 11.00000 0.10725 0.06192 =
0.04668 -0.02073 -0.01294 0.03708
AFIX 23
H22A 2 0.384695 0.723295 0.485982 11.00000 -1.20000
H22B 2 0.286436 0.705751 0.514320 11.00000 -1.20000
AFIX 0
HKLF 4
REM 1-Y-2CH2Cl2_a.res in P2(1)/n
REM R1 = 0.0454 for 6344 Fo > 4sig(Fo) and 0.0589 for all 7662 data
REM 380 parameters refined using 0 restraints
END
WGHT 0.0657 3.7057
REM Highest difference peak 1.146, deepest hole -1.115, 1-sigma level 0.123
Q1 1 0.5382 0.6319 0.3002 11.00000 0.05 1.15
Q2 1 0.6219 0.6313 0.3178 11.00000 0.05 1.01
Q3 1 0.4575 0.8761 0.5572 11.00000 0.05 0.70
Q4 1 0.6252 0.6273 0.2514 11.00000 0.05 0.68
Q5 1 0.5202 0.6232 0.2177 11.00000 0.05 0.67
Q6 1 0.0947 0.6338 0.2721 11.00000 0.05 0.57
Q7 1 0.5617 0.7012 0.0822 11.00000 0.05 0.54
Q8 1 0.2379 0.6188 0.1569 11.00000 0.05 0.52
Q9 1 0.5545 0.6305 0.2454 11.00000 0.05 0.51
Q10 1 0.7670 0.5489 0.3613 11.00000 0.05 0.50
;
_shelx_res_checksum 38762
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT029_1-y-2ch2cl2
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.932 Note
RESPONSE: Crystals suffer radiation damage, preventing a collection to higher
completeness.
;
_vrf_PLAT911_1-y-2ch2cl2
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 333 Report
RESPONSE: Crystals suffer radiation damage, preventing a collection to higher
completeness.
;
_vrf_PLAT975_1-y-2ch2cl2
;
PROBLEM: Check Calcd Residual Density 0.69A From N2 0.45 eA-3
RESPONSE: Atom was correctly assigned, no hydrogen atom nearby.
;
# 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_2-y
_database_code_depnum_ccdc_archive 'CCDC 1566109'
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_audit_creation_date 2017-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C42 H42 B4 N24 O4 Y2'
_chemical_formula_sum 'C42 H42 B4 N24 O4 Y2'
_chemical_formula_weight 1168.05
_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'
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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 11.590(2)
_cell_length_b 18.380(4)
_cell_length_c 12.150(2)
_cell_angle_alpha 90
_cell_angle_beta 104.12(3)
_cell_angle_gamma 90
_cell_volume 2510.0(9)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 670
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 32.036
_cell_measurement_theta_min 0.407
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.369
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
XDS was used for absorption correction.
No further details are reported by XDS.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'light pink'
_exptl_crystal_colour_lustre ?
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary pink
_exptl_crystal_density_diffrn 1.545
_exptl_crystal_density_meas ?
_exptl_crystal_density_method "not measured'"
_exptl_crystal_description needle
_exptl_crystal_F_000 1184
_exptl_crystal_size_max 0.01
_exptl_crystal_size_mid 0.005
_exptl_crystal_size_min 0.005
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1528
_diffrn_reflns_av_unetI/netI 0.0755
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 71257
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 31.870
_diffrn_reflns_theta_min 2.053
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type 'ADSC Quantum 210r'
_diffrn_measurement_method 'Phi Scan'
_diffrn_radiation_monochromator 'Silicon Double Crystal'
_diffrn_radiation_type Synchrotron
_diffrn_radiation_wavelength 0.7108
_diffrn_source 'MX1 Beamline Australian Synchrotron'
_diffrn_special_details ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4914
_reflns_number_total 7549
_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 'XDS (Kabsch, 1993)'
_computing_data_collection 'BluIce (McPhillips, 2002)'
_computing_data_reduction 'XDS (Kabsch, 1993)'
_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 0.550
_refine_diff_density_min -1.704
_refine_diff_density_rms 0.134
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 343
_refine_ls_number_reflns 7549
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1144
_refine_ls_R_factor_gt 0.0595
_refine_ls_restrained_S_all 1.061
_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^)+(0.0661P)^2^+3.2829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1272
_refine_ls_wR_factor_ref 0.1499
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups
2.a Ternary CH refined with riding coordinates:
B1(H1A), B2(H2A)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
C18(H18), C20(H20)
;
_atom_sites_solution_hydrogens geom
_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
Y1 Y 0.44984(3) 0.66287(2) 0.73476(3) 0.02187(10) Uani 1 1 d . . . . .
O1 O 0.4116(2) 0.62818(15) 0.5463(2) 0.0271(6) Uani 1 1 d . . . . .
O2 O 0.4617(2) 0.44927(15) 0.2863(2) 0.0260(6) Uani 1 1 d . . . . .
N1 N 0.2228(3) 0.55978(17) 0.7945(3) 0.0279(7) Uani 1 1 d . . . . .
N2 N 0.2873(3) 0.56670(18) 0.7151(3) 0.0271(7) Uani 1 1 d . . . . .
N3 N 0.3745(3) 0.59852(17) 0.9684(3) 0.0264(7) Uani 1 1 d . . . . .
N4 N 0.4690(3) 0.61178(17) 0.9233(3) 0.0261(7) Uani 1 1 d . . . . .
N5 N 0.2212(3) 0.68804(18) 0.8623(3) 0.0269(7) Uani 1 1 d . . . . .
N6 N 0.2779(3) 0.72038(17) 0.7873(3) 0.0251(6) Uani 1 1 d . . . . .
N7 N 0.5998(3) 0.81888(17) 0.8466(3) 0.0256(7) Uani 1 1 d . . . . .
N8 N 0.5369(3) 0.76130(18) 0.8727(3) 0.0264(7) Uani 1 1 d . . . . .
N9 N 0.5139(3) 0.82879(17) 0.6363(3) 0.0267(7) Uani 1 1 d . . . . .
N10 N 0.4316(3) 0.77453(18) 0.6183(3) 0.0268(7) Uani 1 1 d . . . . .
N11 N 0.7012(3) 0.75718(19) 0.7124(3) 0.0295(7) Uani 1 1 d . . . . .
N12 N 0.6557(3) 0.68836(19) 0.7110(3) 0.0291(7) Uani 1 1 d . . . . .
C1 C 0.1452(4) 0.5040(2) 0.7670(4) 0.0371(10) Uani 1 1 d . . . . .
H1 H 0.090426 0.488781 0.809150 0.045 Uiso 1 1 calc R . . . .
C2 C 0.1584(4) 0.4732(2) 0.6687(4) 0.0370(10) Uani 1 1 d . . . . .
H2 H 0.115573 0.433211 0.628821 0.044 Uiso 1 1 calc R . . . .
C3 C 0.2473(4) 0.5128(2) 0.6401(3) 0.0287(8) Uani 1 1 d . . . . .
H3 H 0.277158 0.503335 0.575303 0.034 Uiso 1 1 calc R . . . .
C4 C 0.4141(4) 0.5734(2) 1.0754(3) 0.0330(9) Uani 1 1 d . . . . .
H4 H 0.365364 0.559811 1.124533 0.040 Uiso 1 1 calc R . . . .
C5 C 0.5357(4) 0.5707(2) 1.1016(3) 0.0325(9) Uani 1 1 d . . . . .
H5 H 0.587411 0.555390 1.170987 0.039 Uiso 1 1 calc R . . . .
C6 C 0.5671(4) 0.5951(2) 1.0048(3) 0.0296(8) Uani 1 1 d . . . . .
H6 H 0.646392 0.599477 0.997130 0.036 Uiso 1 1 calc R . . . .
C7 C 0.1462(4) 0.7359(2) 0.8917(4) 0.0329(9) Uani 1 1 d . . . . .
H7 H 0.097508 0.726814 0.942768 0.039 Uiso 1 1 calc R . . . .
C8 C 0.1520(4) 0.8010(2) 0.8350(4) 0.0344(9) Uani 1 1 d . . . . .
H8 H 0.108548 0.844497 0.838311 0.041 Uiso 1 1 calc R . . . .
C9 C 0.2354(4) 0.7882(2) 0.7725(3) 0.0296(8) Uani 1 1 d . . . . .
H9 H 0.259405 0.823285 0.725178 0.036 Uiso 1 1 calc R . . . .
C10 C 0.6250(4) 0.8661(2) 0.9330(3) 0.0297(8) Uani 1 1 d . . . . .
H10 H 0.667380 0.910507 0.934729 0.036 Uiso 1 1 calc R . . . .
C11 C 0.5785(4) 0.8390(2) 1.0191(3) 0.0309(8) Uani 1 1 d . . . . .
H11 H 0.582942 0.860224 1.091305 0.037 Uiso 1 1 calc R . . . .
C12 C 0.5244(4) 0.7747(2) 0.9775(3) 0.0287(8) Uani 1 1 d . . . . .
H12 H 0.483520 0.743790 1.017920 0.034 Uiso 1 1 calc R . . . .
C13 C 0.4801(4) 0.8807(2) 0.5564(3) 0.0310(8) Uani 1 1 d . . . . .
H13 H 0.522016 0.924515 0.551247 0.037 Uiso 1 1 calc R . . . .
C14 C 0.3756(4) 0.8599(2) 0.4844(3) 0.0340(9) Uani 1 1 d . . . . .
H14 H 0.331149 0.885420 0.419901 0.041 Uiso 1 1 calc R . . . .
C15 C 0.3479(4) 0.7928(2) 0.5260(3) 0.0309(8) Uani 1 1 d . . . . .
H15 H 0.279639 0.764474 0.493258 0.037 Uiso 1 1 calc R . . . .
C16 C 0.8111(4) 0.7546(3) 0.6955(4) 0.0381(10) Uani 1 1 d . . . . .
H16 H 0.860777 0.795427 0.693237 0.046 Uiso 1 1 calc R . . . .
C17 C 0.8401(4) 0.6837(3) 0.6821(4) 0.0442(11) Uani 1 1 d . . . . .
H17 H 0.912549 0.665539 0.669354 0.053 Uiso 1 1 calc R . . . .
C18 C 0.7406(4) 0.6435(3) 0.6910(4) 0.0366(10) Uani 1 1 d . . . . .
H18 H 0.733612 0.592144 0.683968 0.044 Uiso 1 1 calc R . . . .
C19 C 0.4515(3) 0.5689(2) 0.5176(3) 0.0241(7) Uani 1 1 d . . . . .
C20 C 0.4306(4) 0.5438(2) 0.4060(3) 0.0255(7) Uani 1 1 d . . . . .
H20 H 0.385324 0.572270 0.345355 0.031 Uiso 1 1 calc R . . . .
C21 C 0.4763(3) 0.4770(2) 0.3843(3) 0.0250(7) Uani 1 1 d . . . . .
B1 B 0.2455(4) 0.6087(2) 0.8997(4) 0.0278(9) Uani 1 1 d . . . . .
H1A H 0.190354 0.594316 0.947605 0.033 Uiso 1 1 calc R . . . .
B2 B 0.6296(4) 0.8246(2) 0.7308(4) 0.0289(9) Uani 1 1 d . . . . .
H2A H 0.678082 0.869366 0.728839 0.035 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.02622(17) 0.02191(16) 0.01741(14) -0.00211(14) 0.00517(11) -0.00077(15)
O1 0.0324(15) 0.0251(13) 0.0229(12) -0.0031(11) 0.0050(11) 0.0037(11)
O2 0.0309(14) 0.0304(14) 0.0163(11) -0.0026(10) 0.0048(10) 0.0011(11)
N1 0.0315(17) 0.0230(15) 0.0294(16) 0.0018(13) 0.0078(14) -0.0031(13)
N2 0.0298(17) 0.0257(16) 0.0250(15) 0.0007(13) 0.0054(13) 0.0009(13)
N3 0.0346(18) 0.0249(16) 0.0213(14) 0.0006(12) 0.0099(13) 0.0016(13)
N4 0.0305(17) 0.0243(15) 0.0230(14) -0.0026(12) 0.0054(13) -0.0017(13)
N5 0.0312(17) 0.0246(15) 0.0265(15) 0.0028(13) 0.0102(13) 0.0046(13)
N6 0.0287(16) 0.0223(15) 0.0245(15) 0.0005(12) 0.0064(12) -0.0016(13)
N7 0.0293(16) 0.0263(16) 0.0210(14) -0.0027(12) 0.0058(12) -0.0033(13)
N8 0.0282(17) 0.0286(16) 0.0234(15) -0.0030(13) 0.0083(13) -0.0045(13)
N9 0.0330(17) 0.0240(16) 0.0244(15) -0.0015(13) 0.0092(13) -0.0048(13)
N10 0.0287(17) 0.0287(16) 0.0222(14) -0.0020(13) 0.0048(12) -0.0041(13)
N11 0.0275(17) 0.0354(18) 0.0272(16) -0.0020(14) 0.0098(13) -0.0026(14)
N12 0.0308(18) 0.0310(17) 0.0270(16) -0.0038(13) 0.0096(14) -0.0013(14)
C1 0.035(2) 0.033(2) 0.044(2) 0.0026(19) 0.0106(19) -0.0095(18)
C2 0.042(2) 0.025(2) 0.039(2) -0.0015(17) -0.0006(19) -0.0063(18)
C3 0.030(2) 0.0263(19) 0.0268(18) -0.0016(15) 0.0007(15) -0.0015(16)
C4 0.059(3) 0.0201(17) 0.0213(17) 0.0021(14) 0.0129(18) 0.0042(18)
C5 0.049(3) 0.0242(19) 0.0188(16) -0.0025(15) -0.0017(16) 0.0054(18)
C6 0.032(2) 0.0267(19) 0.0258(18) -0.0022(15) -0.0021(15) 0.0017(16)
C7 0.033(2) 0.034(2) 0.035(2) 0.0056(17) 0.0155(17) 0.0064(17)
C8 0.037(2) 0.031(2) 0.038(2) 0.0057(18) 0.0159(18) 0.0071(18)
C9 0.035(2) 0.0259(18) 0.0294(19) 0.0042(16) 0.0098(16) 0.0015(16)
C10 0.033(2) 0.0287(19) 0.0273(18) -0.0091(16) 0.0075(16) -0.0039(17)
C11 0.032(2) 0.037(2) 0.0222(16) -0.0074(17) 0.0044(14) -0.0007(18)
C12 0.033(2) 0.034(2) 0.0204(16) -0.0045(15) 0.0091(15) -0.0028(17)
C13 0.040(2) 0.029(2) 0.0278(19) 0.0019(16) 0.0153(17) 0.0013(17)
C14 0.039(2) 0.039(2) 0.0252(18) 0.0055(17) 0.0096(17) 0.0032(18)
C15 0.030(2) 0.038(2) 0.0229(17) 0.0003(16) 0.0023(15) 0.0005(17)
C16 0.030(2) 0.048(3) 0.040(2) 0.005(2) 0.0154(18) -0.0066(19)
C17 0.036(2) 0.054(3) 0.050(3) 0.005(2) 0.025(2) 0.007(2)
C18 0.037(2) 0.040(2) 0.036(2) -0.0007(18) 0.0139(18) 0.0054(19)
C19 0.0254(18) 0.0233(17) 0.0248(17) 0.0004(14) 0.0085(14) 0.0024(14)
C20 0.0307(19) 0.0223(17) 0.0234(17) 0.0035(14) 0.0062(15) 0.0053(15)
C21 0.0297(19) 0.0264(18) 0.0185(16) -0.0004(14) 0.0051(14) -0.0025(15)
B1 0.030(2) 0.027(2) 0.029(2) 0.0049(17) 0.0121(17) -0.0008(18)
B2 0.032(2) 0.030(2) 0.0263(19) -0.0029(17) 0.0090(17) -0.0043(18)
_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
Y1 O1 2.313(3) . ?
Y1 O2 2.344(3) 3_666 ?
Y1 N2 2.552(3) . ?
Y1 N4 2.435(3) . ?
Y1 N6 2.473(3) . ?
Y1 N8 2.505(3) . ?
Y1 N10 2.472(3) . ?
Y1 N12 2.516(3) . ?
O1 C19 1.264(4) . ?
O2 C21 1.267(4) . ?
N1 N2 1.362(5) . ?
N1 C1 1.351(5) . ?
N1 B1 1.532(6) . ?
N2 C3 1.350(5) . ?
N3 N4 1.361(5) . ?
N3 C4 1.349(5) . ?
N3 B1 1.536(6) . ?
N4 C6 1.348(5) . ?
N5 N6 1.381(4) . ?
N5 C7 1.346(5) . ?
N5 B1 1.533(5) . ?
N6 C9 1.336(5) . ?
N7 N8 1.366(4) . ?
N7 C10 1.338(5) . ?
N7 B2 1.531(5) . ?
N8 C12 1.339(5) . ?
N9 N10 1.360(4) . ?
N9 C13 1.349(5) . ?
N9 B2 1.540(6) . ?
N10 C15 1.335(5) . ?
N11 N12 1.369(5) . ?
N11 C16 1.340(5) . ?
N11 B2 1.538(6) . ?
N12 C18 1.351(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.364(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.374(6) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.368(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.387(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.390(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.388(6) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.381(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.375(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.365(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.398(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.366(7) . ?
C17 H17 0.9500 . ?
C17 C18 1.396(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(5) . ?
C19 C21 1.532(5) 3_666 ?
C20 H20 0.9500 . ?
C20 C21 1.389(5) . ?
B1 H1A 1.0000 . ?
B2 H2A 1.0000 . ?
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
O1 Y1 O2 68.45(9) . 3_666 ?
O1 Y1 N2 75.99(10) . . ?
O1 Y1 N4 140.93(10) . . ?
O1 Y1 N6 113.67(10) . . ?
O1 Y1 N8 144.10(10) . . ?
O1 Y1 N10 72.14(10) . . ?
O1 Y1 N12 84.01(11) . . ?
O2 Y1 N2 73.33(10) 3_666 . ?
O2 Y1 N4 79.72(10) 3_666 . ?
O2 Y1 N6 143.65(10) 3_666 . ?
O2 Y1 N8 126.35(10) 3_666 . ?
O2 Y1 N10 130.26(10) 3_666 . ?
O2 Y1 N12 72.49(11) 3_666 . ?
N4 Y1 N2 73.54(11) . . ?
N4 Y1 N6 79.42(11) . . ?
N4 Y1 N8 73.72(11) . . ?
N4 Y1 N10 146.50(11) . . ?
N4 Y1 N12 107.95(11) . . ?
N6 Y1 N2 72.37(11) . . ?
N6 Y1 N8 74.76(11) . . ?
N6 Y1 N12 142.78(11) . . ?
N8 Y1 N2 136.92(10) . . ?
N8 Y1 N12 72.77(11) . . ?
N10 Y1 N2 124.29(11) . . ?
N10 Y1 N6 80.28(11) . . ?
N10 Y1 N8 75.39(11) . . ?
N10 Y1 N12 74.39(11) . . ?
N12 Y1 N2 144.82(11) . . ?
C19 O1 Y1 121.0(2) . . ?
C21 O2 Y1 119.6(2) . 3_666 ?
N2 N1 B1 121.6(3) . . ?
C1 N1 N2 110.1(3) . . ?
C1 N1 B1 128.3(4) . . ?
N1 N2 Y1 121.2(2) . . ?
C3 N2 Y1 134.1(3) . . ?
C3 N2 N1 104.6(3) . . ?
N4 N3 B1 122.1(3) . . ?
C4 N3 N4 109.4(3) . . ?
C4 N3 B1 128.5(4) . . ?
N3 N4 Y1 123.4(2) . . ?
C6 N4 Y1 130.2(3) . . ?
C6 N4 N3 106.3(3) . . ?
N6 N5 B1 121.5(3) . . ?
C7 N5 N6 109.6(3) . . ?
C7 N5 B1 128.9(3) . . ?
N5 N6 Y1 121.9(2) . . ?
C9 N6 Y1 131.1(3) . . ?
C9 N6 N5 105.7(3) . . ?
N8 N7 B2 121.3(3) . . ?
C10 N7 N8 110.3(3) . . ?
C10 N7 B2 128.4(3) . . ?
N7 N8 Y1 123.7(2) . . ?
C12 N8 Y1 130.5(3) . . ?
C12 N8 N7 105.4(3) . . ?
N10 N9 B2 122.1(3) . . ?
C13 N9 N10 109.5(3) . . ?
C13 N9 B2 128.2(3) . . ?
N9 N10 Y1 123.9(2) . . ?
C15 N10 Y1 129.3(3) . . ?
C15 N10 N9 106.7(3) . . ?
N12 N11 B2 121.7(3) . . ?
C16 N11 N12 110.1(4) . . ?
C16 N11 B2 128.2(4) . . ?
N11 N12 Y1 123.0(2) . . ?
C18 N12 Y1 131.3(3) . . ?
C18 N12 N11 105.7(3) . . ?
N1 C1 H1 125.6 . . ?
N1 C1 C2 108.8(4) . . ?
C2 C1 H1 125.6 . . ?
C1 C2 H2 127.7 . . ?
C1 C2 C3 104.6(4) . . ?
C3 C2 H2 127.7 . . ?
N2 C3 C2 111.9(4) . . ?
N2 C3 H3 124.0 . . ?
C2 C3 H3 124.0 . . ?
N3 C4 H4 125.5 . . ?
N3 C4 C5 109.0(4) . . ?
C5 C4 H4 125.5 . . ?
C4 C5 H5 127.5 . . ?
C4 C5 C6 105.0(4) . . ?
C6 C5 H5 127.5 . . ?
N4 C6 C5 110.4(4) . . ?
N4 C6 H6 124.8 . . ?
C5 C6 H6 124.8 . . ?
N5 C7 H7 125.7 . . ?
N5 C7 C8 108.6(4) . . ?
C8 C7 H7 125.7 . . ?
C7 C8 H8 127.8 . . ?
C9 C8 C7 104.4(4) . . ?
C9 C8 H8 127.8 . . ?
N6 C9 C8 111.6(4) . . ?
N6 C9 H9 124.2 . . ?
C8 C9 H9 124.2 . . ?
N7 C10 H10 126.0 . . ?
N7 C10 C11 108.0(4) . . ?
C11 C10 H10 126.0 . . ?
C10 C11 H11 127.5 . . ?
C12 C11 C10 105.0(3) . . ?
C12 C11 H11 127.5 . . ?
N8 C12 C11 111.2(4) . . ?
N8 C12 H12 124.4 . . ?
C11 C12 H12 124.4 . . ?
N9 C13 H13 125.7 . . ?
N9 C13 C14 108.6(4) . . ?
C14 C13 H13 125.7 . . ?
C13 C14 H14 127.4 . . ?
C13 C14 C15 105.2(4) . . ?
C15 C14 H14 127.4 . . ?
N10 C15 C14 110.0(4) . . ?
N10 C15 H15 125.0 . . ?
C14 C15 H15 125.0 . . ?
N11 C16 H16 125.6 . . ?
N11 C16 C17 108.8(4) . . ?
C17 C16 H16 125.6 . . ?
C16 C17 H17 127.4 . . ?
C16 C17 C18 105.3(4) . . ?
C18 C17 H17 127.4 . . ?
N12 C18 C17 110.1(4) . . ?
N12 C18 H18 124.9 . . ?
C17 C18 H18 124.9 . . ?
O1 C19 C20 124.3(3) . . ?
O1 C19 C21 115.2(3) . 3_666 ?
C20 C19 C21 120.4(3) . 3_666 ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.5(3) . . ?
C21 C20 H20 120.2 . . ?
O2 C21 C19 115.6(3) . 3_666 ?
O2 C21 C20 124.3(3) . . ?
C20 C21 C19 120.0(3) . 3_666 ?
N1 B1 N3 109.2(3) . . ?
N1 B1 N5 109.2(3) . . ?
N1 B1 H1A 109.1 . . ?
N3 B1 H1A 109.1 . . ?
N5 B1 N3 111.2(3) . . ?
N5 B1 H1A 109.1 . . ?
N7 B2 N9 109.8(3) . . ?
N7 B2 N11 109.2(3) . . ?
N7 B2 H2A 109.4 . . ?
N9 B2 H2A 109.4 . . ?
N11 B2 N9 109.5(3) . . ?
N11 B2 H2A 109.4 . . ?
_shelx_res_file
;
TITL 2-Y_a.res in P2(1)/n
2-y.res
created by SHELXL-2016/6 at 16:05:52 on 19-Jun-2017
REM Old TITL 2-Y in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.106, Rweak 0.013, Alpha 0.075, Orientation as input
REM Formula found by SHELXT: C30 N5 O2 Y
CELL 0.71073 11.59 18.38 12.15 90 104.123 90
ZERR 2 0.0023 0.0037 0.0024 0 0.03 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B N O Y
UNIT 84 84 8 48 8 4
L.S. 10
PLAN 10
TEMP -173(2)
BOND $H
LIST 6
fmap 2
acta
REM
REM
REM
WGHT 0.066100 3.282900
FVAR 0.46003
Y1 6 0.449840 0.662872 0.734757 11.00000 0.02622 0.02191 =
0.01741 -0.00211 0.00517 -0.00077
O1 5 0.411639 0.628182 0.546278 11.00000 0.03238 0.02512 =
0.02294 -0.00307 0.00499 0.00365
O2 5 0.461725 0.449268 0.286286 11.00000 0.03093 0.03037 =
0.01628 -0.00262 0.00479 0.00111
N1 4 0.222813 0.559782 0.794477 11.00000 0.03150 0.02304 =
0.02940 0.00180 0.00784 -0.00306
N2 4 0.287301 0.566703 0.715118 11.00000 0.02984 0.02573 =
0.02497 0.00071 0.00544 0.00091
N3 4 0.374508 0.598518 0.968443 11.00000 0.03463 0.02495 =
0.02128 0.00063 0.00990 0.00156
N4 4 0.468990 0.611778 0.923285 11.00000 0.03048 0.02425 =
0.02298 -0.00262 0.00536 -0.00167
N5 4 0.221214 0.688041 0.862275 11.00000 0.03115 0.02459 =
0.02649 0.00280 0.01019 0.00458
N6 4 0.277886 0.720384 0.787263 11.00000 0.02866 0.02230 =
0.02446 0.00045 0.00643 -0.00160
N7 4 0.599834 0.818877 0.846592 11.00000 0.02934 0.02632 =
0.02100 -0.00268 0.00580 -0.00332
N8 4 0.536899 0.761298 0.872740 11.00000 0.02822 0.02862 =
0.02341 -0.00304 0.00827 -0.00454
N9 4 0.513860 0.828795 0.636292 11.00000 0.03296 0.02397 =
0.02443 -0.00151 0.00917 -0.00476
N10 4 0.431601 0.774525 0.618303 11.00000 0.02874 0.02868 =
0.02220 -0.00202 0.00480 -0.00411
N11 4 0.701195 0.757178 0.712357 11.00000 0.02750 0.03543 =
0.02720 -0.00204 0.00985 -0.00261
N12 4 0.655662 0.688361 0.711036 11.00000 0.03078 0.03097 =
0.02697 -0.00378 0.00959 -0.00125
C1 1 0.145182 0.504010 0.766966 11.00000 0.03508 0.03311 =
0.04361 0.00258 0.01059 -0.00951
AFIX 43
H1 2 0.090426 0.488781 0.809150 11.00000 -1.20000
AFIX 0
C2 1 0.158360 0.473168 0.668667 11.00000 0.04200 0.02495 =
0.03865 -0.00147 -0.00058 -0.00626
AFIX 43
H2 2 0.115573 0.433211 0.628821 11.00000 -1.20000
AFIX 0
C3 1 0.247338 0.512782 0.640113 11.00000 0.02983 0.02633 =
0.02684 -0.00157 0.00068 -0.00151
AFIX 43
H3 2 0.277158 0.503335 0.575303 11.00000 -1.20000
AFIX 0
C4 1 0.414087 0.573406 1.075383 11.00000 0.05911 0.02013 =
0.02126 0.00215 0.01295 0.00417
AFIX 43
H4 2 0.365364 0.559811 1.124533 11.00000 -1.20000
AFIX 0
C5 1 0.535688 0.570684 1.101600 11.00000 0.04919 0.02419 =
0.01877 -0.00252 -0.00171 0.00543
AFIX 43
H5 2 0.587411 0.555390 1.170987 11.00000 -1.20000
AFIX 0
C6 1 0.567066 0.595112 1.004838 11.00000 0.03162 0.02667 =
0.02581 -0.00223 -0.00208 0.00167
AFIX 43
H6 2 0.646392 0.599477 0.997130 11.00000 -1.20000
AFIX 0
C7 1 0.146235 0.735947 0.891733 11.00000 0.03324 0.03407 =
0.03498 0.00562 0.01550 0.00640
AFIX 43
H7 2 0.097508 0.726814 0.942768 11.00000 -1.20000
AFIX 0
C8 1 0.151961 0.801040 0.835031 11.00000 0.03706 0.03144 =
0.03826 0.00573 0.01592 0.00714
AFIX 43
H8 2 0.108548 0.844497 0.838311 11.00000 -1.20000
AFIX 0
C9 1 0.235430 0.788195 0.772549 11.00000 0.03460 0.02590 =
0.02938 0.00419 0.00982 0.00152
AFIX 43
H9 2 0.259405 0.823285 0.725178 11.00000 -1.20000
AFIX 0
C10 1 0.624984 0.866115 0.932957 11.00000 0.03331 0.02872 =
0.02728 -0.00912 0.00753 -0.00391
AFIX 43
H10 2 0.667380 0.910507 0.934729 11.00000 -1.20000
AFIX 0
C11 1 0.578512 0.839031 1.019077 11.00000 0.03237 0.03692 =
0.02222 -0.00735 0.00441 -0.00068
AFIX 43
H11 2 0.582942 0.860224 1.091305 11.00000 -1.20000
AFIX 0
C12 1 0.524433 0.774708 0.977507 11.00000 0.03301 0.03405 =
0.02042 -0.00445 0.00909 -0.00281
AFIX 43
H12 2 0.483520 0.743790 1.017920 11.00000 -1.20000
AFIX 0
C13 1 0.480077 0.880743 0.556447 11.00000 0.04033 0.02853 =
0.02777 0.00191 0.01532 0.00130
AFIX 43
H13 2 0.522016 0.924515 0.551247 11.00000 -1.20000
AFIX 0
C14 1 0.375559 0.859881 0.484397 11.00000 0.03886 0.03882 =
0.02520 0.00553 0.00959 0.00322
AFIX 43
H14 2 0.331149 0.885420 0.419901 11.00000 -1.20000
AFIX 0
C15 1 0.347930 0.792833 0.525951 11.00000 0.02977 0.03793 =
0.02286 0.00027 0.00229 0.00051
AFIX 43
H15 2 0.279639 0.764474 0.493258 11.00000 -1.20000
AFIX 0
C16 1 0.811126 0.754606 0.695488 11.00000 0.03017 0.04818 =
0.03963 0.00525 0.01544 -0.00659
AFIX 43
H16 2 0.860777 0.795427 0.693237 11.00000 -1.20000
AFIX 0
C17 1 0.840130 0.683666 0.682053 11.00000 0.03645 0.05353 =
0.05002 0.00543 0.02456 0.00666
AFIX 43
H17 2 0.912549 0.665539 0.669354 11.00000 -1.20000
AFIX 0
C18 1 0.740606 0.643530 0.690979 11.00000 0.03666 0.04017 =
0.03559 -0.00067 0.01387 0.00536
AFIX 43
H18 2 0.733612 0.592144 0.683968 11.00000 -1.20000
AFIX 0
C19 1 0.451505 0.568947 0.517598 11.00000 0.02537 0.02335 =
0.02476 0.00044 0.00851 0.00239
C20 1 0.430558 0.543826 0.405995 11.00000 0.03068 0.02234 =
0.02338 0.00348 0.00616 0.00531
AFIX 43
H20 2 0.385324 0.572270 0.345355 11.00000 -1.20000
AFIX 0
C21 1 0.476321 0.476957 0.384250 11.00000 0.02965 0.02639 =
0.01848 -0.00044 0.00512 -0.00248
B1 3 0.245529 0.608700 0.899657 11.00000 0.03009 0.02709 =
0.02877 0.00491 0.01209 -0.00084
AFIX 13
H1A 2 0.190354 0.594316 0.947605 11.00000 -1.20000
AFIX 0
B2 3 0.629596 0.824603 0.730850 11.00000 0.03155 0.02974 =
0.02633 -0.00287 0.00897 -0.00428
AFIX 13
H2A 2 0.678082 0.869366 0.728839 11.00000 -1.20000
AFIX 0
HKLF 4
REM 2-Y_a.res in P2(1)/n
REM R1 = 0.0595 for 4914 Fo > 4sig(Fo) and 0.1144 for all 7549 data
REM 343 parameters refined using 0 restraints
END
WGHT 0.0661 3.2837
REM Highest difference peak 0.550, deepest hole -1.704, 1-sigma level 0.134
Q1 1 0.6527 0.9322 0.7440 11.00000 0.05 0.55
Q2 1 0.5489 0.7014 0.7734 11.00000 0.05 0.46
Q3 1 0.1748 0.6639 0.8816 11.00000 0.05 0.46
Q4 1 0.5894 0.9567 0.7578 11.00000 0.05 0.45
Q5 1 0.5351 0.6632 0.8759 11.00000 0.05 0.44
Q6 1 0.0111 0.5108 0.7135 11.00000 0.05 0.44
Q7 1 0.8673 0.5946 0.6931 11.00000 0.05 0.44
Q8 1 0.5915 0.8328 0.5823 11.00000 0.05 0.44
Q9 1 0.3788 0.7170 0.7596 11.00000 0.05 0.42
Q10 1 0.3773 0.6636 0.5997 11.00000 0.05 0.42
;
_shelx_res_checksum 6821
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_RINTA01_2-y
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Every attempt was made to achieve a better structure collection,
however the only crystals obtained were small and poorly diffracting,
and therefore collected at the synchrotron.
;
_vrf_PLAT369_2-y
;
PROBLEM: Long C(sp2)-C(sp2) Bond C19 - C21_a .. 1.53 Ang.
RESPONSE: Bond has similar observed mean bond length to that of similar bonds
in -C(=O)-C(=O)- systems.
;
_vrf_PLAT906_2-y
;
PROBLEM: Large K value in the Analysis of Variance ...... 3.438 Check
RESPONSE: Due to a slight overestimation of intensities of weak reflections
;
_vrf_PLAT972_2-y
;
PROBLEM: Check Calcd Residual Density 0.74A From Y1 -1.66 eA-3
RESPONSE: Slight inaccuracy of the absorption correction not affecting the
connectivity nor the integrity of the structure
;
_vrf_PLAT976_2-y
;
PROBLEM: Check Calcd Residual Density 0.78A From N12 -0.47 eA-3
RESPONSE: Slight inaccuracy of the absorption correction not affecting the
connectivity nor the integrity of the structure
;
# 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_1-y-2me2co
_database_code_depnum_ccdc_archive 'CCDC 1566108'
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_audit_creation_date 2017-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C42 H40 B4 Cl2 N24 O4 Y2, 2(C3 H6 O)'
_chemical_formula_sum 'C48 H52 B4 Cl2 N24 O6 Y2'
_chemical_formula_weight 1353.09
_chemical_melting_point ?
_chemical_oxdiff_formula Y2Cl2N24H4O4C42B4
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.2804(4)
_cell_length_b 15.0832(3)
_cell_length_c 14.6373(4)
_cell_angle_alpha 90
_cell_angle_beta 108.072(3)
_cell_angle_gamma 90
_cell_volume 2997.25(13)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 10029
_cell_measurement_temperature 130.01(10)
_cell_measurement_theta_max 76.8330
_cell_measurement_theta_min 4.2970
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.975
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.85054
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'light purple'
_exptl_crystal_colour_lustre light
_exptl_crystal_colour_primary purple
_exptl_crystal_density_diffrn 1.499
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 1376
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 -8 -1 0.0901
8 4 -3 0.0427
-8 4 6 0.0382
-3 -9 3 0.0987
-5 -1 -5 0.0636
-3 -8 -3 0.0576
-3 -8 -3 0.0614
4 7 4 0.0405
1 10 -1 0.1032
8 0 -7 0.0219
-8 1 7 0.0190
_exptl_crystal_size_max 0.277
_exptl_crystal_size_mid 0.103
_exptl_crystal_size_min 0.051
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.5322 -7.8448 -1.4555 -0.1322 -0.5552 -0.8211
8.3404 4.2650 -2.9125 -0.2132 -0.8882 0.4069
-7.5199 3.6120 6.4903 -0.2643 0.8897 0.3724
-3.1840 -8.8264 3.3881 -0.1221 0.4144 -0.9019
-5.4952 -0.8736 -5.4818 0.9233 0.3829 -0.0300
-3.2185 -7.9836 -3.1649 0.5781 0.2403 -0.7798
-2.9507 -8.3018 -2.8955 0.5349 0.2225 -0.8151
3.8968 6.9685 3.8484 -0.6864 -0.2852 0.6690
0.8700 9.6732 -1.3746 0.0405 -0.1397 0.9894
7.9898 -0.3961 -7.1085 0.2842 -0.9578 -0.0435
-7.9332 1.4905 6.9904 -0.2811 0.9470 0.1555
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0508
_diffrn_reflns_av_unetI/netI 0.0459
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 30166
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 77.185
_diffrn_reflns_theta_min 3.778
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 130.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -121.00 -1.00 1.00 2.50 -- -40.81 -19.00 0.00 120
2 \w -46.00 -2.00 1.00 2.50 -- -40.81 38.00 0.00 44
3 \w -49.00 30.00 1.00 2.50 -- -40.81 38.00-180.00 79
4 \w 2.00 52.00 1.00 2.50 -- 40.81 -99.00 -90.00 50
5 \w 58.00 84.00 1.00 2.50 -- 40.81-125.00 150.00 26
6 \w 23.00 98.00 1.00 2.50 -- 40.81-125.00 60.00 75
7 \w 31.00 89.00 1.00 2.50 -- 40.81-125.00 -90.00 58
8 \w 68.00 125.00 1.00 22.50 -- 113.00 -61.00 60.00 57
9 \w 147.00 173.00 1.00 22.50 -- 113.00 111.00 60.00 26
10 \w 103.00 138.00 1.00 22.50 -- 113.00 178.00 -30.00 35
11 \w 100.00 170.00 1.00 22.50 -- 113.00 45.00-150.00 70
12 \w 36.00 90.00 1.00 22.50 -- 113.00 -30.00-180.00 54
13 \w 136.00 161.00 1.00 22.50 -- 113.00 111.00 30.00 25
14 \w 42.00 67.00 1.00 22.50 -- 113.00-111.00 90.00 25
15 \w 76.00 112.00 1.00 22.50 -- 113.00-111.00 0.00 36
16 \w 45.00 71.00 1.00 22.50 -- 113.00-111.00 0.00 26
17 \w 107.00 133.00 1.00 22.50 -- 113.00 111.00 60.00 26
18 \w 49.00 74.00 1.00 22.50 -- 113.00-111.00-120.00 25
19 \w 87.00 114.00 1.00 22.50 -- 113.00-111.00-120.00 27
20 \w 49.00 141.00 1.00 22.50 -- 113.00 -61.00 -30.00 92
21 \w 57.00 82.00 1.00 22.50 -- 113.00 -30.00-150.00 25
22 \w 29.00 55.00 1.00 22.50 -- 113.00 -94.00 120.00 26
23 \w 74.00 109.00 1.00 22.50 -- 113.00 -94.00 120.00 35
24 \w 67.00 92.00 1.00 22.50 -- 113.00 178.00 30.00 25
25 \w 120.00 175.00 1.00 22.50 -- 113.00 45.00-180.00 55
26 \w 30.00 80.00 1.00 22.50 -- 113.00 -94.00 -30.00 50
27 \w 89.00 177.00 1.00 22.50 -- 113.00 61.00 150.00 88
28 \w 102.00 157.00 1.00 22.50 -- 113.00 77.00 60.00 55
29 \w 62.00 108.00 1.00 22.50 -- 113.00 -94.00 -90.00 46
30 \w 33.00 58.00 1.00 22.50 -- 113.00 -94.00 60.00 25
31 \w 43.00 69.00 1.00 22.50 -- 113.00 -94.00 0.00 26
32 \w 73.00 102.00 1.00 22.50 -- 113.00-111.00-150.00 29
33 \w 91.00 116.00 1.00 22.50 -- 113.00-111.00 90.00 25
34 \w 78.00 107.00 1.00 22.50 -- 113.00 -94.00 60.00 29
35 \w 39.00 74.00 1.00 22.50 -- 113.00 -45.00 -30.00 35
36 \w 61.00 87.00 1.00 22.50 -- 113.00 178.00 -30.00 26
37 \w 54.00 98.00 1.00 22.50 -- 113.00 -45.00 120.00 44
38 \w 78.00 111.00 1.00 22.50 -- 113.00-111.00 30.00 33
39 \w 89.00 175.00 1.00 22.50 -- 113.00 61.00 120.00 86
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0601299000
_diffrn_orient_matrix_UB_12 -0.0056487000
_diffrn_orient_matrix_UB_13 -0.1072506000
_diffrn_orient_matrix_UB_21 -0.0961174000
_diffrn_orient_matrix_UB_22 -0.0019862000
_diffrn_orient_matrix_UB_23 0.0268136000
_diffrn_orient_matrix_UB_31 -0.0052721000
_diffrn_orient_matrix_UB_32 0.1019742000
_diffrn_orient_matrix_UB_33 -0.0054859000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5362
_reflns_number_total 6302
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_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 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 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 'XT (Sheldrick, 2015)'
_refine_diff_density_max 0.830
_refine_diff_density_min -0.551
_refine_diff_density_rms 0.076
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 390
_refine_ls_number_reflns 6302
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0433
_refine_ls_R_factor_gt 0.0338
_refine_ls_restrained_S_all 1.036
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+1.9334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0825
_refine_ls_wR_factor_ref 0.0884
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
B1(H1A), B2(H2A)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
C18(H18)
2.c Idealised Me refined as rotating group:
C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_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
Y1 Y 0.41339(2) 0.36857(2) 0.22173(2) 0.02003(7) Uani 1 1 d . . . . .
Cl1 Cl 0.44163(5) 0.32876(4) -0.13296(4) 0.03080(13) Uani 1 1 d . . . . .
O1 O 0.42307(13) 0.35984(11) 0.06518(13) 0.0247(3) Uani 1 1 d . . . . .
O2 O 0.53659(13) 0.49670(11) -0.16926(12) 0.0232(3) Uani 1 1 d . . . . .
N1 N 0.54915(17) 0.24415(14) 0.41698(16) 0.0276(4) Uani 1 1 d . . . . .
N2 N 0.46903(16) 0.29768(14) 0.38440(16) 0.0267(4) Uani 1 1 d . . . . .
N3 N 0.55523(17) 0.17991(14) 0.26093(17) 0.0294(4) Uani 1 1 d . . . . .
N4 N 0.47676(17) 0.22130(14) 0.19693(16) 0.0291(4) Uani 1 1 d . . . . .
N5 N 0.65676(17) 0.31469(15) 0.33306(16) 0.0286(4) Uani 1 1 d . . . . .
N6 N 0.59713(16) 0.38374(15) 0.29096(16) 0.0273(4) Uani 1 1 d . . . . .
N7 N 0.18262(15) 0.46162(13) 0.15323(16) 0.0256(4) Uani 1 1 d . . . . .
N8 N 0.25664(15) 0.44003(13) 0.11663(15) 0.0249(4) Uani 1 1 d . . . . .
N9 N 0.19464(16) 0.32688(14) 0.25678(16) 0.0271(4) Uani 1 1 d . . . . .
N10 N 0.27296(16) 0.28552(14) 0.23971(16) 0.0259(4) Uani 1 1 d . . . . .
N11 N 0.26932(15) 0.47262(13) 0.33001(15) 0.0245(4) Uani 1 1 d . . . . .
N12 N 0.36243(15) 0.47325(13) 0.32272(15) 0.0234(4) Uani 1 1 d . . . . .
C1 C 0.5578(2) 0.21528(17) 0.50661(19) 0.0304(5) Uani 1 1 d . . . . .
H1 H 0.606931 0.178016 0.543545 0.036 Uiso 1 1 calc R . . . .
C2 C 0.4818(2) 0.25025(18) 0.53393(19) 0.0328(5) Uani 1 1 d . . . . .
H2 H 0.469002 0.241928 0.591869 0.039 Uiso 1 1 calc R . . . .
C3 C 0.4280(2) 0.30109(17) 0.45544(19) 0.0292(5) Uani 1 1 d . . . . .
H3 H 0.371505 0.332987 0.452730 0.035 Uiso 1 1 calc R . . . .
C4 C 0.5700(2) 0.10024(18) 0.2268(2) 0.0369(6) Uani 1 1 d . . . . .
H4 H 0.618660 0.059869 0.257882 0.044 Uiso 1 1 calc R . . . .
C5 C 0.5013(2) 0.08836(19) 0.1383(2) 0.0396(6) Uani 1 1 d . . . . .
H5 H 0.493999 0.039610 0.097809 0.047 Uiso 1 1 calc R . . . .
C6 C 0.4449(2) 0.16540(18) 0.1227(2) 0.0331(5) Uani 1 1 d . . . . .
H6 H 0.392047 0.176565 0.067891 0.040 Uiso 1 1 calc R . . . .
C7 C 0.7516(2) 0.3414(2) 0.3643(2) 0.0345(6) Uani 1 1 d . . . . .
H7 H 0.805407 0.305797 0.394806 0.041 Uiso 1 1 calc R . . . .
C8 C 0.7555(2) 0.4294(2) 0.3435(2) 0.0379(6) Uani 1 1 d . . . . .
H8 H 0.811043 0.465299 0.356996 0.046 Uiso 1 1 calc R . . . .
C9 C 0.6577(2) 0.45351(18) 0.2975(2) 0.0315(5) Uani 1 1 d . . . . .
H9 H 0.637266 0.510063 0.274611 0.038 Uiso 1 1 calc R . . . .
C10 C 0.1165(2) 0.51452(17) 0.0915(2) 0.0315(5) Uani 1 1 d . . . . .
H10 H 0.060060 0.537959 0.101119 0.038 Uiso 1 1 calc R . . . .
C11 C 0.1466(2) 0.52810(18) 0.0117(2) 0.0338(6) Uani 1 1 d . . . . .
H11 H 0.115626 0.561672 -0.042589 0.041 Uiso 1 1 calc R . . . .
C12 C 0.2339(2) 0.48016(17) 0.03070(19) 0.0294(5) Uani 1 1 d . . . . .
H12 H 0.271551 0.476424 -0.010818 0.035 Uiso 1 1 calc R . . . .
C13 C 0.1385(2) 0.26646(19) 0.2838(2) 0.0346(6) Uani 1 1 d . . . . .
H13 H 0.081261 0.278538 0.299025 0.041 Uiso 1 1 calc R . . . .
C14 C 0.1805(2) 0.18376(18) 0.2851(2) 0.0356(6) Uani 1 1 d . . . . .
H14 H 0.158026 0.129919 0.301250 0.043 Uiso 1 1 calc R . . . .
C15 C 0.2635(2) 0.19873(16) 0.25708(19) 0.0299(5) Uani 1 1 d . . . . .
H15 H 0.306810 0.154735 0.251063 0.036 Uiso 1 1 calc R . . . .
C16 C 0.2674(2) 0.52112(17) 0.40686(19) 0.0290(5) Uani 1 1 d . . . . .
H16 H 0.212371 0.530217 0.426923 0.035 Uiso 1 1 calc R . . . .
C17 C 0.3598(2) 0.55486(17) 0.45066(19) 0.0308(5) Uani 1 1 d . . . . .
H17 H 0.379973 0.590446 0.505159 0.037 Uiso 1 1 calc R . . . .
C18 C 0.41628(19) 0.52394(17) 0.39530(19) 0.0279(5) Uani 1 1 d . . . . .
H18 H 0.482689 0.536721 0.407041 0.033 Uiso 1 1 calc R . . . .
C19 C 0.45766(17) 0.42264(15) 0.02901(17) 0.0216(4) Uani 1 1 d . . . . .
C20 C 0.47223(18) 0.42184(15) -0.06050(17) 0.0234(4) Uani 1 1 d . . . . .
C21 C 0.51611(17) 0.49381(15) -0.09213(17) 0.0211(4) Uani 1 1 d . . . . .
B1 B 0.6159(2) 0.2252(2) 0.3556(2) 0.0302(6) Uani 1 1 d . . . . .
H1A H 0.670391 0.186596 0.390812 0.036 Uiso 1 1 calc R . . . .
B2 B 0.1824(2) 0.42823(19) 0.2522(2) 0.0273(5) Uani 1 1 d . . . . .
H2A H 0.120136 0.444321 0.262830 0.033 Uiso 1 1 calc R . . . .
O3 O 0.3549(2) 0.1885(2) 0.6828(2) 0.0664(8) Uani 1 1 d . . . . .
C22 C 0.2786(3) 0.2247(3) 0.6337(3) 0.0534(9) Uani 1 1 d . . . . .
C23 C 0.1862(3) 0.1728(3) 0.5924(3) 0.0605(10) Uani 1 1 d . . . . .
H23A H 0.172821 0.167142 0.524237 0.091 Uiso 1 1 calc GR . . . .
H23B H 0.132398 0.202949 0.605296 0.091 Uiso 1 1 calc GR . . . .
H23C H 0.193853 0.114995 0.621171 0.091 Uiso 1 1 calc GR . . . .
C24 C 0.2737(4) 0.3201(3) 0.6136(5) 0.0757(14) Uani 1 1 d . . . . .
H24A H 0.248050 0.350267 0.658453 0.114 Uiso 1 1 calc GR . . . .
H24B H 0.231396 0.330516 0.549403 0.114 Uiso 1 1 calc GR . . . .
H24C H 0.338581 0.341896 0.619927 0.114 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.02215(10) 0.01914(11) 0.01923(10) 0.00187(7) 0.00703(7) 0.00068(7)
Cl1 0.0412(3) 0.0253(3) 0.0303(3) -0.0070(2) 0.0173(2) -0.0088(2)
O1 0.0292(8) 0.0214(7) 0.0250(8) 0.0020(6) 0.0108(7) -0.0018(6)
O2 0.0266(8) 0.0219(7) 0.0225(8) 0.0017(6) 0.0098(6) -0.0015(6)
N1 0.0317(10) 0.0242(9) 0.0244(10) 0.0026(8) 0.0050(8) 0.0036(8)
N2 0.0266(10) 0.0263(10) 0.0269(10) 0.0031(8) 0.0076(8) 0.0034(8)
N3 0.0335(11) 0.0256(10) 0.0295(11) 0.0003(8) 0.0102(9) 0.0055(8)
N4 0.0345(11) 0.0254(10) 0.0270(10) 0.0015(8) 0.0088(9) 0.0025(8)
N5 0.0269(10) 0.0321(11) 0.0264(10) 0.0007(8) 0.0076(8) 0.0036(8)
N6 0.0281(10) 0.0281(10) 0.0257(10) 0.0021(8) 0.0084(8) 0.0007(8)
N7 0.0233(9) 0.0232(9) 0.0276(10) -0.0032(8) 0.0040(8) -0.0003(7)
N8 0.0246(9) 0.0240(9) 0.0243(10) 0.0011(7) 0.0050(8) -0.0005(7)
N9 0.0273(10) 0.0277(10) 0.0267(10) -0.0020(8) 0.0090(8) -0.0053(8)
N10 0.0270(10) 0.0231(9) 0.0268(10) 0.0000(8) 0.0071(8) -0.0013(8)
N11 0.0243(9) 0.0235(9) 0.0253(10) -0.0023(7) 0.0069(8) 0.0002(7)
N12 0.0248(9) 0.0210(9) 0.0233(9) 0.0002(7) 0.0060(8) -0.0006(7)
C1 0.0351(13) 0.0262(11) 0.0257(12) 0.0064(9) 0.0035(10) 0.0002(10)
C2 0.0392(14) 0.0345(13) 0.0240(12) 0.0052(10) 0.0087(10) -0.0038(11)
C3 0.0300(12) 0.0310(12) 0.0271(12) 0.0026(9) 0.0097(10) -0.0008(10)
C4 0.0400(14) 0.0270(12) 0.0443(16) -0.0014(11) 0.0141(12) 0.0080(11)
C5 0.0454(16) 0.0288(13) 0.0452(16) -0.0107(11) 0.0151(13) 0.0011(12)
C6 0.0385(14) 0.0301(12) 0.0305(13) -0.0041(10) 0.0105(11) -0.0020(11)
C7 0.0218(11) 0.0479(15) 0.0318(13) -0.0041(11) 0.0055(10) 0.0030(11)
C8 0.0278(13) 0.0480(16) 0.0367(15) -0.0014(12) 0.0082(11) -0.0090(11)
C9 0.0310(13) 0.0323(12) 0.0293(12) 0.0006(10) 0.0067(10) -0.0063(10)
C10 0.0250(11) 0.0272(12) 0.0363(14) -0.0039(10) 0.0011(10) 0.0029(9)
C11 0.0318(13) 0.0291(12) 0.0329(13) 0.0054(10) -0.0012(10) 0.0022(10)
C12 0.0302(12) 0.0281(11) 0.0261(12) 0.0041(9) 0.0033(9) -0.0028(10)
C13 0.0356(13) 0.0374(14) 0.0354(14) -0.0057(11) 0.0179(11) -0.0141(11)
C14 0.0473(16) 0.0273(12) 0.0345(14) -0.0017(10) 0.0159(12) -0.0144(11)
C15 0.0403(14) 0.0199(11) 0.0283(12) 0.0003(9) 0.0090(10) -0.0038(9)
C16 0.0344(13) 0.0268(11) 0.0276(12) -0.0030(9) 0.0124(10) 0.0036(10)
C17 0.0372(13) 0.0283(12) 0.0249(12) -0.0044(9) 0.0064(10) 0.0016(10)
C18 0.0268(11) 0.0280(11) 0.0257(12) 0.0005(9) 0.0035(9) -0.0019(9)
C19 0.0204(10) 0.0215(10) 0.0231(11) 0.0021(8) 0.0069(8) 0.0003(8)
C20 0.0269(11) 0.0218(10) 0.0229(11) -0.0010(8) 0.0096(9) -0.0015(8)
C21 0.0211(10) 0.0211(10) 0.0211(10) 0.0022(8) 0.0066(8) 0.0008(8)
B1 0.0310(14) 0.0293(13) 0.0284(14) 0.0025(10) 0.0065(11) 0.0069(11)
B2 0.0250(12) 0.0293(13) 0.0286(14) -0.0050(10) 0.0096(10) -0.0024(10)
O3 0.0537(16) 0.093(2) 0.0543(16) -0.0004(15) 0.0199(13) -0.0095(15)
C22 0.056(2) 0.066(2) 0.0461(19) -0.0132(16) 0.0284(17) -0.0146(18)
C23 0.056(2) 0.073(3) 0.056(2) -0.0108(19) 0.0221(18) -0.0180(19)
C24 0.079(3) 0.061(2) 0.103(4) -0.021(3) 0.050(3) -0.013(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 O1 2.3417(17) . ?
Y1 O2 2.3601(16) 3_665 ?
Y1 N2 2.504(2) . ?
Y1 N4 2.467(2) . ?
Y1 N6 2.513(2) . ?
Y1 N8 2.530(2) . ?
Y1 N10 2.447(2) . ?
Y1 N12 2.424(2) . ?
Cl1 C20 1.732(2) . ?
O1 C19 1.258(3) . ?
O2 C21 1.252(3) . ?
N1 N2 1.360(3) . ?
N1 C1 1.351(3) . ?
N1 B1 1.526(4) . ?
N2 C3 1.343(3) . ?
N3 N4 1.368(3) . ?
N3 C4 1.343(4) . ?
N3 B1 1.547(4) . ?
N4 C6 1.339(4) . ?
N5 N6 1.365(3) . ?
N5 C7 1.350(4) . ?
N5 B1 1.546(4) . ?
N6 C9 1.347(4) . ?
N7 N8 1.364(3) . ?
N7 C10 1.347(4) . ?
N7 B2 1.535(4) . ?
N8 C12 1.342(3) . ?
N9 N10 1.370(3) . ?
N9 C13 1.351(3) . ?
N9 B2 1.538(3) . ?
N10 C15 1.348(3) . ?
N11 N12 1.367(3) . ?
N11 C16 1.349(3) . ?
N11 B2 1.551(3) . ?
N12 C18 1.341(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.373(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.397(4) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.372(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.366(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.397(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.380(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.392(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.381(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.388(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.373(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.390(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.389(3) . ?
C19 C21 1.539(3) 3_665 ?
C20 C21 1.402(3) . ?
B1 H1A 0.9800 . ?
B2 H2A 0.9800 . ?
O3 C22 1.232(6) . ?
C22 C23 1.491(5) . ?
C22 C24 1.465(6) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Y1 O2 67.31(6) . 3_665 ?
O1 Y1 N2 143.98(6) . . ?
O1 Y1 N4 70.72(7) . . ?
O1 Y1 N6 91.64(7) . . ?
O1 Y1 N8 74.85(7) . . ?
O1 Y1 N10 112.06(7) . . ?
O1 Y1 N12 138.89(6) . . ?
O2 Y1 N2 129.67(7) 3_665 . ?
O2 Y1 N4 124.44(7) 3_665 . ?
O2 Y1 N6 70.69(7) 3_665 . ?
O2 Y1 N8 74.65(6) 3_665 . ?
O2 Y1 N10 144.75(6) 3_665 . ?
O2 Y1 N12 79.40(6) 3_665 . ?
N2 Y1 N6 70.84(7) . . ?
N2 Y1 N8 136.04(7) . . ?
N4 Y1 N2 74.50(7) . . ?
N4 Y1 N6 75.91(7) . . ?
N4 Y1 N8 126.14(7) . . ?
N6 Y1 N8 145.34(7) . . ?
N10 Y1 N2 73.02(7) . . ?
N10 Y1 N4 84.56(7) . . ?
N10 Y1 N6 142.31(7) . . ?
N10 Y1 N8 71.55(7) . . ?
N12 Y1 N2 76.40(7) . . ?
N12 Y1 N4 150.37(7) . . ?
N12 Y1 N6 99.69(7) . . ?
N12 Y1 N8 73.56(7) . . ?
N12 Y1 N10 81.76(7) . . ?
C19 O1 Y1 121.29(15) . . ?
C21 O2 Y1 120.16(14) . 3_665 ?
N2 N1 B1 121.1(2) . . ?
C1 N1 N2 110.2(2) . . ?
C1 N1 B1 128.7(2) . . ?
N1 N2 Y1 124.83(16) . . ?
C3 N2 Y1 129.34(17) . . ?
C3 N2 N1 105.8(2) . . ?
N4 N3 B1 121.6(2) . . ?
C4 N3 N4 110.1(2) . . ?
C4 N3 B1 128.3(2) . . ?
N3 N4 Y1 124.74(17) . . ?
C6 N4 Y1 129.67(19) . . ?
C6 N4 N3 105.6(2) . . ?
N6 N5 B1 122.6(2) . . ?
C7 N5 N6 110.2(2) . . ?
C7 N5 B1 126.4(2) . . ?
N5 N6 Y1 122.65(16) . . ?
C9 N6 Y1 131.86(18) . . ?
C9 N6 N5 105.5(2) . . ?
N8 N7 B2 121.4(2) . . ?
C10 N7 N8 110.2(2) . . ?
C10 N7 B2 128.4(2) . . ?
N7 N8 Y1 120.66(15) . . ?
C12 N8 Y1 132.34(18) . . ?
C12 N8 N7 105.6(2) . . ?
N10 N9 B2 122.2(2) . . ?
C13 N9 N10 109.8(2) . . ?
C13 N9 B2 127.9(2) . . ?
N9 N10 Y1 121.96(15) . . ?
C15 N10 Y1 130.61(18) . . ?
C15 N10 N9 105.8(2) . . ?
N12 N11 B2 121.4(2) . . ?
C16 N11 N12 109.5(2) . . ?
C16 N11 B2 128.8(2) . . ?
N11 N12 Y1 121.78(15) . . ?
C18 N12 Y1 130.37(17) . . ?
C18 N12 N11 106.0(2) . . ?
N1 C1 H1 125.8 . . ?
N1 C1 C2 108.4(2) . . ?
C2 C1 H1 125.8 . . ?
C1 C2 H2 127.6 . . ?
C1 C2 C3 104.7(2) . . ?
C3 C2 H2 127.6 . . ?
N2 C3 C2 110.8(2) . . ?
N2 C3 H3 124.6 . . ?
C2 C3 H3 124.6 . . ?
N3 C4 H4 125.7 . . ?
N3 C4 C5 108.6(3) . . ?
C5 C4 H4 125.7 . . ?
C4 C5 H5 127.6 . . ?
C4 C5 C6 104.7(2) . . ?
C6 C5 H5 127.6 . . ?
N4 C6 C5 111.0(3) . . ?
N4 C6 H6 124.5 . . ?
C5 C6 H6 124.5 . . ?
N5 C7 H7 125.7 . . ?
N5 C7 C8 108.7(3) . . ?
C8 C7 H7 125.7 . . ?
C7 C8 H8 127.6 . . ?
C7 C8 C9 104.9(2) . . ?
C9 C8 H8 127.6 . . ?
N6 C9 C8 110.8(3) . . ?
N6 C9 H9 124.6 . . ?
C8 C9 H9 124.6 . . ?
N7 C10 H10 125.7 . . ?
N7 C10 C11 108.5(2) . . ?
C11 C10 H10 125.7 . . ?
C10 C11 H11 127.8 . . ?
C10 C11 C12 104.4(2) . . ?
C12 C11 H11 127.8 . . ?
N8 C12 C11 111.3(3) . . ?
N8 C12 H12 124.3 . . ?
C11 C12 H12 124.3 . . ?
N9 C13 H13 125.7 . . ?
N9 C13 C14 108.6(2) . . ?
C14 C13 H13 125.7 . . ?
C13 C14 H14 127.6 . . ?
C13 C14 C15 104.8(2) . . ?
C15 C14 H14 127.6 . . ?
N10 C15 C14 111.0(2) . . ?
N10 C15 H15 124.5 . . ?
C14 C15 H15 124.5 . . ?
N11 C16 H16 125.5 . . ?
N11 C16 C17 109.0(2) . . ?
C17 C16 H16 125.5 . . ?
C16 C17 H17 127.7 . . ?
C16 C17 C18 104.5(2) . . ?
C18 C17 H17 127.7 . . ?
N12 C18 C17 111.1(2) . . ?
N12 C18 H18 124.5 . . ?
C17 C18 H18 124.5 . . ?
O1 C19 C20 125.7(2) . . ?
O1 C19 C21 114.7(2) . 3_665 ?
C20 C19 C21 119.6(2) . 3_665 ?
C19 C20 Cl1 120.10(18) . . ?
C19 C20 C21 121.2(2) . . ?
C21 C20 Cl1 118.63(18) . . ?
O2 C21 C19 115.6(2) . 3_665 ?
O2 C21 C20 125.3(2) . . ?
C20 C21 C19 119.1(2) . 3_665 ?
N1 B1 N3 109.3(2) . . ?
N1 B1 N5 108.0(2) . . ?
N1 B1 H1A 109.9 . . ?
N3 B1 H1A 109.9 . . ?
N5 B1 N3 109.7(2) . . ?
N5 B1 H1A 109.9 . . ?
N7 B2 N9 109.5(2) . . ?
N7 B2 N11 108.4(2) . . ?
N7 B2 H2A 109.6 . . ?
N9 B2 N11 110.1(2) . . ?
N9 B2 H2A 109.6 . . ?
N11 B2 H2A 109.6 . . ?
O3 C22 C23 121.0(4) . . ?
O3 C22 C24 122.1(4) . . ?
C24 C22 C23 117.0(4) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
_shelx_res_file
;
TITL 1-Y-2Me2CO_a.res in P2(1)/n
1-y-2me2co.res
created by SHELXL-2016/6 at 14:23:55 on 16-Jun-2017
REM Old TITL 1-Y-2Me2CO in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.078, Rweak 0.016, Alpha 0.052, Orientation as input
REM Formula found by SHELXT: C31 N7 O3 Cl Y
CELL 1.54184 14.280371 15.083225 14.637281 90 108.0721 90
ZERR 2 0.000372 0.000263 0.000389 0 0.0027 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B Cl N O Y
UNIT 96 104 8 4 48 12 4
L.S. 10 0 0
PLAN 10
BOND $H
LIST 6
fmap 2 53
acta
OMIT 4 14 10
REM
REM
REM
WGHT 0.041000 1.933400
FVAR 0.42954
Y1 7 0.413394 0.368568 0.221726 11.00000 0.02215 0.01914 =
0.01923 0.00187 0.00703 0.00068
CL1 4 0.441628 0.328762 -0.132959 11.00000 0.04115 0.02527 =
0.03028 -0.00705 0.01733 -0.00881
O1 6 0.423070 0.359842 0.065176 11.00000 0.02922 0.02136 =
0.02505 0.00197 0.01085 -0.00177
O2 6 0.536594 0.496697 -0.169262 11.00000 0.02661 0.02189 =
0.02247 0.00174 0.00979 -0.00154
N1 5 0.549147 0.244154 0.416985 11.00000 0.03169 0.02421 =
0.02442 0.00261 0.00496 0.00365
N2 5 0.469026 0.297680 0.384396 11.00000 0.02656 0.02628 =
0.02688 0.00307 0.00758 0.00336
N3 5 0.555229 0.179912 0.260931 11.00000 0.03354 0.02557 =
0.02950 0.00030 0.01021 0.00548
N4 5 0.476763 0.221299 0.196932 11.00000 0.03454 0.02536 =
0.02701 0.00148 0.00881 0.00252
N5 5 0.656760 0.314686 0.333058 11.00000 0.02693 0.03205 =
0.02639 0.00073 0.00761 0.00361
N6 5 0.597131 0.383740 0.290959 11.00000 0.02814 0.02813 =
0.02569 0.00206 0.00837 0.00070
N7 5 0.182620 0.461618 0.153227 11.00000 0.02326 0.02315 =
0.02763 -0.00318 0.00398 -0.00031
N8 5 0.256641 0.440029 0.116629 11.00000 0.02461 0.02396 =
0.02433 0.00114 0.00501 -0.00045
N9 5 0.194645 0.326883 0.256779 11.00000 0.02729 0.02767 =
0.02674 -0.00203 0.00899 -0.00525
N10 5 0.272962 0.285525 0.239714 11.00000 0.02704 0.02310 =
0.02680 -0.00004 0.00709 -0.00125
N11 5 0.269318 0.472617 0.330012 11.00000 0.02425 0.02351 =
0.02532 -0.00226 0.00690 0.00025
N12 5 0.362426 0.473247 0.322722 11.00000 0.02484 0.02100 =
0.02328 0.00017 0.00605 -0.00057
C1 1 0.557810 0.215277 0.506610 11.00000 0.03513 0.02625 =
0.02570 0.00644 0.00349 0.00024
AFIX 43
H1 2 0.606931 0.178016 0.543545 11.00000 -1.20000
AFIX 0
C2 1 0.481822 0.250251 0.533927 11.00000 0.03919 0.03451 =
0.02402 0.00516 0.00870 -0.00377
AFIX 43
H2 2 0.469002 0.241928 0.591869 11.00000 -1.20000
AFIX 0
C3 1 0.428038 0.301091 0.455441 11.00000 0.02997 0.03101 =
0.02712 0.00260 0.00972 -0.00085
AFIX 43
H3 2 0.371505 0.332987 0.452730 11.00000 -1.20000
AFIX 0
C4 1 0.569989 0.100244 0.226777 11.00000 0.04002 0.02698 =
0.04429 -0.00136 0.01405 0.00803
AFIX 43
H4 2 0.618660 0.059869 0.257882 11.00000 -1.20000
AFIX 0
C5 1 0.501271 0.088358 0.138324 11.00000 0.04544 0.02880 =
0.04522 -0.01074 0.01515 0.00114
AFIX 43
H5 2 0.493999 0.039610 0.097809 11.00000 -1.20000
AFIX 0
C6 1 0.444869 0.165396 0.122662 11.00000 0.03846 0.03014 =
0.03054 -0.00408 0.01046 -0.00201
AFIX 43
H6 2 0.392047 0.176565 0.067891 11.00000 -1.20000
AFIX 0
C7 1 0.751619 0.341379 0.364255 11.00000 0.02179 0.04791 =
0.03182 -0.00408 0.00548 0.00304
AFIX 43
H7 2 0.805407 0.305797 0.394806 11.00000 -1.20000
AFIX 0
C8 1 0.755493 0.429361 0.343494 11.00000 0.02784 0.04799 =
0.03670 -0.00143 0.00820 -0.00899
AFIX 43
H8 2 0.811043 0.465299 0.356996 11.00000 -1.20000
AFIX 0
C9 1 0.657724 0.453505 0.297539 11.00000 0.03100 0.03234 =
0.02931 0.00059 0.00667 -0.00633
AFIX 43
H9 2 0.637266 0.510063 0.274611 11.00000 -1.20000
AFIX 0
C10 1 0.116512 0.514519 0.091521 11.00000 0.02502 0.02722 =
0.03632 -0.00385 0.00106 0.00288
AFIX 43
H10 2 0.060060 0.537959 0.101119 11.00000 -1.20000
AFIX 0
C11 1 0.146619 0.528095 0.011662 11.00000 0.03179 0.02913 =
0.03291 0.00537 -0.00116 0.00222
AFIX 43
H11 2 0.115626 0.561672 -0.042589 11.00000 -1.20000
AFIX 0
C12 1 0.233869 0.480159 0.030698 11.00000 0.03020 0.02813 =
0.02611 0.00409 0.00331 -0.00282
AFIX 43
H12 2 0.271551 0.476424 -0.010818 11.00000 -1.20000
AFIX 0
C13 1 0.138548 0.266455 0.283825 11.00000 0.03559 0.03741 =
0.03543 -0.00572 0.01791 -0.01409
AFIX 43
H13 2 0.081261 0.278538 0.299025 11.00000 -1.20000
AFIX 0
C14 1 0.180467 0.183765 0.285131 11.00000 0.04733 0.02734 =
0.03447 -0.00172 0.01594 -0.01441
AFIX 43
H14 2 0.158026 0.129919 0.301250 11.00000 -1.20000
AFIX 0
C15 1 0.263479 0.198735 0.257080 11.00000 0.04028 0.01989 =
0.02833 0.00026 0.00896 -0.00384
AFIX 43
H15 2 0.306810 0.154735 0.251063 11.00000 -1.20000
AFIX 0
C16 1 0.267366 0.521118 0.406864 11.00000 0.03436 0.02678 =
0.02764 -0.00299 0.01235 0.00361
AFIX 43
H16 2 0.212371 0.530217 0.426923 11.00000 -1.20000
AFIX 0
C17 1 0.359756 0.554865 0.450657 11.00000 0.03715 0.02827 =
0.02488 -0.00437 0.00638 0.00164
AFIX 43
H17 2 0.379973 0.590446 0.505159 11.00000 -1.20000
AFIX 0
C18 1 0.416281 0.523940 0.395297 11.00000 0.02680 0.02804 =
0.02568 0.00052 0.00354 -0.00188
AFIX 43
H18 2 0.482689 0.536721 0.407041 11.00000 -1.20000
AFIX 0
C19 1 0.457663 0.422644 0.029013 11.00000 0.02041 0.02149 =
0.02307 0.00211 0.00694 0.00027
C20 1 0.472227 0.421843 -0.060504 11.00000 0.02685 0.02177 =
0.02293 -0.00096 0.00956 -0.00147
C21 1 0.516111 0.493809 -0.092135 11.00000 0.02106 0.02114 =
0.02111 0.00223 0.00657 0.00085
B1 3 0.615950 0.225212 0.355639 11.00000 0.03104 0.02932 =
0.02843 0.00247 0.00648 0.00688
AFIX 13
H1A 2 0.670391 0.186596 0.390812 11.00000 -1.20000
AFIX 0
B2 3 0.182448 0.428229 0.252236 11.00000 0.02497 0.02927 =
0.02860 -0.00503 0.00958 -0.00242
AFIX 13
H2A 2 0.120136 0.444321 0.262830 11.00000 -1.20000
AFIX 0
O3 6 0.354911 0.188465 0.682806 11.00000 0.05372 0.09344 =
0.05431 -0.00044 0.01987 -0.00949
C22 1 0.278559 0.224735 0.633654 11.00000 0.05628 0.06642 =
0.04605 -0.01322 0.02844 -0.01457
C23 1 0.186182 0.172834 0.592418 11.00000 0.05566 0.07261 =
0.05633 -0.01083 0.02209 -0.01804
AFIX 137
H23A 2 0.172821 0.167142 0.524237 11.00000 -1.50000
H23B 2 0.132398 0.202949 0.605296 11.00000 -1.50000
H23C 2 0.193853 0.114995 0.621171 11.00000 -1.50000
AFIX 0
C24 1 0.273730 0.320067 0.613635 11.00000 0.07857 0.06072 =
0.10302 -0.02137 0.05011 -0.01259
AFIX 137
H24A 2 0.248050 0.350267 0.658453 11.00000 -1.50000
H24B 2 0.231396 0.330516 0.549403 11.00000 -1.50000
H24C 2 0.338581 0.341896 0.619927 11.00000 -1.50000
AFIX 0
HKLF 4
REM 1-Y-2Me2CO_a.res in P2(1)/n
REM R1 = 0.0338 for 5362 Fo > 4sig(Fo) and 0.0433 for all 6302 data
REM 390 parameters refined using 0 restraints
END
WGHT 0.0410 1.9408
REM Highest difference peak 0.830, deepest hole -0.551, 1-sigma level 0.076
Q1 1 0.4626 0.3646 0.1804 11.00000 0.05 0.83
Q2 1 0.3628 0.3713 0.2610 11.00000 0.05 0.82
Q3 1 0.4436 0.2942 0.1966 11.00000 0.05 0.60
Q4 1 0.3802 0.3373 0.1910 11.00000 0.05 0.58
Q5 1 0.3805 0.4419 0.2367 11.00000 0.05 0.45
Q6 1 0.0858 0.3990 0.2785 11.00000 0.05 0.43
Q7 1 0.4550 0.4395 0.2229 11.00000 0.05 0.39
Q8 1 0.4866 0.4611 -0.0813 11.00000 0.05 0.37
Q9 1 0.4398 0.4020 -0.1348 11.00000 0.05 0.36
Q10 1 0.3697 0.3010 0.2171 11.00000 0.05 0.34
;
_shelx_res_checksum 33374
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.443
_oxdiff_exptl_absorpt_empirical_full_min 0.724
# start Validation Reply Form
_vrf_PLAT369_1-y-2me2co
;
PROBLEM: Long C(sp2)-C(sp2) Bond C19 - C21_a .. 1.54 Ang.
RESPONSE: Bond has similar observed mean bond length to that of
similar bonds in -C(=O)-C(=O)- systems.
;
# 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_5-y-meoh
_database_code_depnum_ccdc_archive 'CCDC 1566112'
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_audit_creation_date 2017-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'C63.34 H90.69 B6 N24 O20 Y4, 10(C H4 O), 2(Cl)'
_chemical_formula_sum 'C73.35 H130.69 B6 Cl2 N24 O30 Y4'
_chemical_formula_weight 2320.24
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 13.1868(3)
_cell_length_b 21.4815(4)
_cell_length_c 19.6434(4)
_cell_angle_alpha 90
_cell_angle_beta 101.2134(18)
_cell_angle_gamma 90
_cell_volume 5458.21(19)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 23979
_cell_measurement_temperature 130.01(10)
_cell_measurement_theta_max 77.2420
_cell_measurement_theta_min 3.9600
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.880
_exptl_absorpt_correction_T_max 0.944
_exptl_absorpt_correction_T_min 0.681
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'intense purple'
_exptl_crystal_colour_modifier intense
_exptl_crystal_colour_primary purple
_exptl_crystal_density_diffrn 1.412
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2398
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 -6 6 0.1326
3 9 8 0.2004
-1 -1 -12 0.1143
-1 1 13 0.1556
8 1 -1 0.0359
-8 -1 1 0.0359
6 -6 -9 0.2093
_exptl_crystal_size_max 0.89
_exptl_crystal_size_mid 0.278
_exptl_crystal_size_min 0.072
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.6050 -6.4260 5.8643 -0.5349 -0.1594 -0.8297
3.1412 8.6133 7.7887 0.5389 0.1592 -0.8272
-0.7458 -0.7094 -12.2334 -0.2622 0.4836 0.8351
-0.6108 0.5007 12.6518 0.3223 -0.5940 -0.7371
8.4674 1.3703 -1.1870 -0.3411 0.6266 -0.7008
-8.4674 -1.3703 1.1870 0.3411 -0.6266 0.7008
5.8548 -6.4311 -8.7781 -0.8513 0.5211 0.0609
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0731
_diffrn_reflns_av_unetI/netI 0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 60720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 77.592
_diffrn_reflns_theta_min 3.417
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 130.01(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -43.00 -13.00 1.00 1.45 -- -40.81 -57.00 -30.00 30
2 \w -50.00 35.00 1.00 1.45 -- -40.81 38.00-150.00 85
3 \w -36.00 70.00 1.00 1.45 -- 40.81 -77.00-120.00 106
4 \w 36.00 98.00 1.00 1.45 -- 40.81-125.00-180.00 62
5 \w 54.00 90.00 1.00 12.50 -- 113.00 -30.00-150.00 36
6 \w 103.00 133.00 1.00 12.50 -- 113.00 15.00-120.00 30
7 \w 140.00 173.00 1.00 12.50 -- 113.00 15.00-120.00 33
8 \w 143.00 178.00 1.00 12.50 -- 113.00 45.00 -30.00 35
9 \w 152.00 177.00 1.00 12.50 -- 113.00 111.00 -30.00 25
10 \w 105.00 156.00 1.00 12.50 -- 113.00 30.00 120.00 51
11 \w 110.00 136.00 1.00 12.50 -- 113.00 -77.00 150.00 26
12 \w 88.00 116.00 1.00 12.50 -- 113.00-111.00 150.00 28
13 \w 75.00 142.00 1.00 12.50 -- 113.00 -77.00 60.00 67
14 \w 112.00 138.00 1.00 12.50 -- 113.00 -61.00 -30.00 26
15 \w 96.00 121.00 1.00 12.50 -- 113.00 -77.00 -60.00 25
16 \w 82.00 114.00 1.00 12.50 -- 113.00-111.00 -60.00 32
17 \w 79.00 115.00 1.00 12.50 -- 113.00-111.00-120.00 36
18 \w 89.00 114.00 1.00 12.50 -- 113.00-111.00-180.00 25
19 \w 63.00 97.00 1.00 12.50 -- 113.00-111.00 -90.00 34
20 \w 58.00 112.00 1.00 12.50 -- 113.00-111.00 0.00 54
21 \w 71.00 97.00 1.00 12.50 -- 113.00 -45.00 30.00 26
22 \w 58.00 116.00 1.00 12.50 -- 113.00-111.00 60.00 58
23 \w 56.00 93.00 1.00 12.50 -- 113.00 -77.00 150.00 37
24 \w 48.00 96.00 1.00 12.50 -- 113.00 -94.00 60.00 48
25 \w 52.00 78.00 1.00 12.50 -- 113.00 -61.00 -30.00 26
26 \w 45.00 97.00 1.00 12.50 -- 113.00 -45.00 -60.00 52
27 \w 85.00 155.00 1.00 12.50 -- 113.00 30.00 -90.00 70
28 \w 89.00 176.00 1.00 12.50 -- 113.00 77.00 -60.00 87
29 \w 48.00 74.00 1.00 12.50 -- 113.00 -77.00 60.00 26
30 \w 41.00 91.00 1.00 12.50 -- 113.00 -30.00 0.00 50
31 \w 42.00 68.00 1.00 12.50 -- 113.00-111.00-120.00 26
32 \w 35.00 67.00 1.00 12.50 -- 113.00-111.00-180.00 32
33 \w 39.00 132.00 1.00 12.50 -- 113.00 -61.00-120.00 93
34 \w 36.00 71.00 1.00 12.50 -- 113.00 -30.00 -30.00 35
35 \w 35.00 172.00 1.00 12.50 -- 113.00 -15.00-120.00 137
36 \w 47.00 74.00 1.00 12.50 -- 113.00-111.00 150.00 27
37 \w 36.00 74.00 1.00 12.50 -- 113.00 -94.00 150.00 38
38 \w 43.00 99.00 1.00 12.50 -- 113.00 -45.00 150.00 56
39 \w -50.00 32.00 1.00 1.45 -- -40.81 38.00 120.00 82
40 \w -105.00 -16.00 1.00 1.45 -- -40.81 -57.00 -60.00 89
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0472401000
_diffrn_orient_matrix_UB_12 0.0610054000
_diffrn_orient_matrix_UB_13 0.0207786000
_diffrn_orient_matrix_UB_21 0.0616245000
_diffrn_orient_matrix_UB_22 0.0370946000
_diffrn_orient_matrix_UB_23 -0.0454396000
_diffrn_orient_matrix_UB_31 -0.0904242000
_diffrn_orient_matrix_UB_32 -0.0066666000
_diffrn_orient_matrix_UB_33 -0.0623633000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 10142
_reflns_number_total 11486
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_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 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 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 1.371
_refine_diff_density_min -1.457
_refine_diff_density_rms 0.142
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 688
_refine_ls_number_reflns 11486
_refine_ls_number_restraints 12
_refine_ls_R_factor_all 0.0624
_refine_ls_R_factor_gt 0.0558
_refine_ls_restrained_S_all 1.065
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+8.2208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1444
_refine_ls_wR_factor_ref 0.1502
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Shared sites
{O10A, O10B}
3. Restrained distances
O10A-H10C
0.85 with sigma of 0.01
O10B-H10B
0.82 with sigma of 0.001
H10A-H10B
1.34 with sigma of 0.001
Y2-H10B
2.85 with sigma of 0.001
O9-H9
0.85 with sigma of 0.01
O15A-C37A
1.46 with sigma of 0.02
C37B-O15B
1.4 with sigma of 0.001
Y2-H10C
2.902118 with sigma of 0.02
C32-H10C
1.891083 with sigma of 0.02
C31-H9
1.872335 with sigma of 0.02
Y1-H9
2.858143 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O10A) = Uanis(O10B)
Uanis(C37A) = Uanis(O15B)
Uanis(O15A) = Uanis(C37A)
Uanis(O11) = Uanis(O15B) = Uanis(O15A)
Uanis(O15B) = Uanis(C37B)
Uanis(C33) = Uanis(C37A) = Uanis(C37B)
5. Others
1*[Sof(Cl1A)]+1*[Sof(Cl1B)]+1*[Sof(Cl1C)]=1 with esd of 0.001
Sof(O10B)=Sof(H10A)=Sof(H10B)=Sof(O12A)=Sof(H12A)=Sof(C34A)=Sof(H34A)=
Sof(H34B)=Sof(H34C)=1-FVAR(1)
Sof(O12B)=Sof(H12B)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(O10A)=
Sof(H10C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
Sof(O15B)=Sof(H15B)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(2)
Sof(O15A)=Sof(H15A)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(2)
Fixed X: H10A(0.8348)
Fixed Y: H10A(0.68752)
Fixed Z: H10A(0.34091)
6.a Ternary CH refined with riding coordinates:
B1(H1A), B2(H2A)
6.b Aromatic/amide H refined with riding coordinates:
C11(H11), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
C9(H9A), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
C18(H18)
6.c Idealised Me refined with riding coordinates:
C37B(H37D,H37E,H37F)
6.d Idealised Me refined as rotating group:
C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,
H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
C34A(H34A,H34B,H34C), C33(H33A,H33B,H33C), C37A(H37A,H37B,H37C), C36(H36A,H36B,
H36C), C35(H35A,H35B,H35C), C34B(H34D,H34E,H34F), C32(H32A,H32B,H32C)
6.e Idealised tetrahedral OH refined as rotating group:
O12A(H12A), O11(H11A), O15A(H15A), O14(H14A), O13(H13A), O12B(H12B),
O10A(H10C), O15B(H15B)
;
_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
Y1 Y 0.65884(2) 0.41141(2) 0.74175(2) 0.02248(10) Uani 1 1 d D . . . .
Y2 Y 0.71902(2) 0.69630(2) 0.44972(2) 0.02221(10) Uani 1 1 d D . . . .
O1 O 0.60088(19) 0.50458(11) 0.69280(12) 0.0267(5) Uani 1 1 d . . . . .
O2 O 0.76805(19) 0.45253(12) 0.67010(12) 0.0267(5) Uani 1 1 d . . . . .
O3 O 0.6386(2) 0.66397(12) 0.53771(12) 0.0280(5) Uani 1 1 d . . . . .
O4 O 0.79964(19) 0.60912(12) 0.50809(12) 0.0273(5) Uani 1 1 d . . . . .
O5 O 0.49538(19) 0.36669(12) 0.71809(12) 0.0269(5) Uani 1 1 d . . . . .
O6 O 0.57436(18) 0.37655(12) 0.62904(11) 0.0257(5) Uani 1 1 d . . . . .
O8 O 0.44456(19) 0.29223(12) 0.62106(12) 0.0270(5) Uani 1 1 d . . . . .
O7 O 0.38316(19) 0.38813(11) 0.60472(12) 0.0262(5) Uani 1 1 d . . . . .
O9 O 0.7594(2) 0.32699(12) 0.72313(12) 0.0315(5) Uani 1 1 d D . . . .
H9 H 0.758(3) 0.3130(19) 0.6824(8) 0.047 Uiso 1 1 d DR . . . .
N1 N 0.8095(2) 0.44982(14) 0.89703(15) 0.0274(6) Uani 1 1 d . . . . .
N2 N 0.8080(2) 0.44762(14) 0.82714(14) 0.0270(6) Uani 1 1 d . . . . .
N3 N 0.6213(3) 0.47154(15) 0.89642(15) 0.0302(6) Uani 1 1 d . . . . .
N4 N 0.5835(2) 0.47200(15) 0.82634(15) 0.0303(6) Uani 1 1 d . . . . .
N5 N 0.6896(3) 0.36275(15) 0.91204(15) 0.0304(6) Uani 1 1 d . . . . .
N6 N 0.6651(3) 0.34192(15) 0.84515(15) 0.0304(6) Uani 1 1 d . . . . .
N7 N 0.9057(3) 0.79878(15) 0.51771(16) 0.0316(6) Uani 1 1 d . . . . .
N8 N 0.8825(2) 0.73715(15) 0.51279(15) 0.0295(6) Uani 1 1 d . . . . .
N9 N 0.7286(3) 0.84199(15) 0.52081(15) 0.0323(6) Uani 1 1 d . . . . .
N10 N 0.6709(3) 0.78882(15) 0.51078(16) 0.0316(6) Uani 1 1 d . . . . .
N11 N 0.7903(3) 0.84246(15) 0.40934(16) 0.0314(6) Uani 1 1 d . . . . .
N12 N 0.7466(2) 0.78914(15) 0.38057(15) 0.0291(6) Uani 1 1 d . . . . .
C11 C 1.0456(3) 0.7489(2) 0.5701(2) 0.0408(9) Uani 1 1 d . . . . .
H11 H 1.113457 0.739791 0.594551 0.049 Uiso 1 1 calc R . . . .
C1 C 0.9031(3) 0.46769(18) 0.93054(19) 0.0328(7) Uani 1 1 d . . . . .
H1 H 0.923018 0.472962 0.979326 0.039 Uiso 1 1 calc R . . . .
C2 C 0.9659(3) 0.4772(2) 0.8831(2) 0.0359(8) Uani 1 1 d . . . . .
H2 H 1.036360 0.489767 0.891985 0.043 Uiso 1 1 calc R . . . .
C3 C 0.9027(3) 0.46437(18) 0.81923(19) 0.0318(7) Uani 1 1 d . . . . .
H3 H 0.923977 0.467119 0.775826 0.038 Uiso 1 1 calc R . . . .
C4 C 0.5654(3) 0.5101(2) 0.9282(2) 0.0369(8) Uani 1 1 d . . . . .
H4 H 0.577009 0.517655 0.976775 0.044 Uiso 1 1 calc R . . . .
C5 C 0.4886(4) 0.5368(2) 0.8797(2) 0.0413(9) Uani 1 1 d . . . . .
H5 H 0.437254 0.565666 0.887229 0.050 Uiso 1 1 calc R . . . .
C6 C 0.5033(3) 0.5119(2) 0.8167(2) 0.0365(8) Uani 1 1 d . . . . .
H6 H 0.462107 0.521749 0.772804 0.044 Uiso 1 1 calc R . . . .
C7 C 0.6896(3) 0.3150(2) 0.95654(19) 0.0345(8) Uani 1 1 d . . . . .
H7 H 0.704643 0.317896 1.005733 0.041 Uiso 1 1 calc R . . . .
C8 C 0.6639(3) 0.26107(19) 0.9186(2) 0.0361(8) Uani 1 1 d . . . . .
H8 H 0.657376 0.220177 0.935664 0.043 Uiso 1 1 calc R . . . .
C9 C 0.6498(3) 0.28034(18) 0.8497(2) 0.0335(7) Uani 1 1 d . . . . .
H9A H 0.631703 0.253390 0.810932 0.040 Uiso 1 1 calc R . . . .
C27 C 0.4164(3) 0.3539(2) 0.75699(19) 0.0355(8) Uani 1 1 d . . . . .
H27A H 0.433483 0.315607 0.783839 0.053 Uiso 1 1 calc GR . . . .
H27B H 0.349912 0.348825 0.725084 0.053 Uiso 1 1 calc GR . . . .
H27C H 0.411887 0.388629 0.788645 0.053 Uiso 1 1 calc GR . . . .
C10 C 1.0033(3) 0.8064(2) 0.5520(2) 0.0396(9) Uani 1 1 d . . . . .
H10 H 1.037600 0.845141 0.562118 0.047 Uiso 1 1 calc R . . . .
C12 C 0.9673(3) 0.7071(2) 0.5448(2) 0.0337(7) Uani 1 1 d . . . . .
H12 H 0.972984 0.663192 0.549625 0.040 Uiso 1 1 calc R . . . .
C13 C 0.6804(4) 0.88469(19) 0.55314(19) 0.0394(9) Uani 1 1 d . . . . .
H13 H 0.705460 0.925304 0.566141 0.047 Uiso 1 1 calc R . . . .
C14 C 0.5888(4) 0.8599(2) 0.5643(2) 0.0410(9) Uani 1 1 d . . . . .
H14 H 0.538171 0.879304 0.585536 0.049 Uiso 1 1 calc R . . . .
C15 C 0.5871(3) 0.79974(19) 0.5374(2) 0.0359(8) Uani 1 1 d . . . . .
H15 H 0.533379 0.770425 0.538039 0.043 Uiso 1 1 calc R . . . .
C16 C 0.7790(4) 0.88770(19) 0.3614(2) 0.0407(9) Uani 1 1 d . . . . .
H16 H 0.802924 0.929301 0.369133 0.049 Uiso 1 1 calc R . . . .
C17 C 0.7271(4) 0.8640(2) 0.2994(2) 0.0420(9) Uani 1 1 d . . . . .
H17 H 0.708143 0.885075 0.256285 0.050 Uiso 1 1 calc R . . . .
C18 C 0.7088(3) 0.80265(19) 0.3139(2) 0.0348(8) Uani 1 1 d . . . . .
H18 H 0.673894 0.773735 0.280832 0.042 Uiso 1 1 calc R . . . .
C19 C 0.6445(3) 0.53297(15) 0.64958(16) 0.0236(6) Uani 1 1 d . . . . .
C20 C 0.7425(3) 0.50139(16) 0.63580(16) 0.0241(6) Uani 1 1 d . . . . .
C21 C 0.6079(3) 0.58881(16) 0.61767(17) 0.0253(6) Uani 1 1 d . . . . .
C22 C 0.7972(3) 0.52650(16) 0.58744(17) 0.0270(6) Uani 1 1 d . . . . .
C23 C 0.6631(3) 0.61404(16) 0.57017(16) 0.0241(6) Uani 1 1 d . . . . .
C24 C 0.7593(3) 0.58165(16) 0.55359(16) 0.0237(6) Uani 1 1 d . . . . .
C25 C 0.5150(3) 0.62110(19) 0.6348(2) 0.0345(8) Uani 1 1 d . . . . .
H25A H 0.452582 0.606722 0.603196 0.052 Uiso 1 1 calc GR . . . .
H25B H 0.522273 0.666177 0.629727 0.052 Uiso 1 1 calc GR . . . .
H25C H 0.509586 0.611487 0.682756 0.052 Uiso 1 1 calc GR . . . .
C26 C 0.8926(3) 0.4956(2) 0.5726(2) 0.0401(9) Uani 1 1 d . . . . .
H26A H 0.950804 0.503736 0.610856 0.060 Uiso 1 1 calc GR . . . .
H26B H 0.908291 0.512234 0.529364 0.060 Uiso 1 1 calc GR . . . .
H26C H 0.880966 0.450604 0.567881 0.060 Uiso 1 1 calc GR . . . .
C28 C 0.5894(3) 0.3797(2) 0.55905(18) 0.0355(8) Uani 1 1 d . . . . .
H28A H 0.558831 0.418237 0.537510 0.053 Uiso 1 1 calc GR . . . .
H28B H 0.556017 0.343854 0.533002 0.053 Uiso 1 1 calc GR . . . .
H28C H 0.663546 0.379147 0.558609 0.053 Uiso 1 1 calc GR . . . .
C29 C 0.3763(3) 0.45437(18) 0.6096(2) 0.0395(9) Uani 1 1 d . . . . .
H29A H 0.433559 0.473617 0.592052 0.059 Uiso 1 1 calc GR . . . .
H29B H 0.380280 0.466308 0.658188 0.059 Uiso 1 1 calc GR . . . .
H29C H 0.310446 0.468583 0.581868 0.059 Uiso 1 1 calc GR . . . .
C30 C 0.5162(3) 0.2417(2) 0.6412(2) 0.0404(9) Uani 1 1 d . . . . .
H30A H 0.482484 0.202169 0.625660 0.061 Uiso 1 1 calc GR . . . .
H30B H 0.538088 0.241282 0.691801 0.061 Uiso 1 1 calc GR . . . .
H30C H 0.576771 0.247439 0.619760 0.061 Uiso 1 1 calc GR . . . .
C31 C 0.8516(4) 0.3044(3) 0.7664(3) 0.0524(12) Uani 1 1 d D . . . .
H31A H 0.850928 0.258826 0.766367 0.079 Uiso 1 1 calc GR . . . .
H31B H 0.855376 0.319698 0.813825 0.079 Uiso 1 1 calc GR . . . .
H31C H 0.911757 0.319313 0.748668 0.079 Uiso 1 1 calc GR . . . .
B1 B 0.7145(3) 0.4314(2) 0.92879(19) 0.0315(8) Uani 1 1 d . . . . .
H1A H 0.730673 0.437663 0.980210 0.038 Uiso 1 1 calc R . . . .
B2 B 0.8254(3) 0.8497(2) 0.4888(2) 0.0325(8) Uani 1 1 d . . . . .
H2A H 0.856126 0.891896 0.499915 0.039 Uiso 1 1 calc R . . . .
B3 B 0.4746(3) 0.35601(18) 0.64247(18) 0.0248(7) Uani 1 1 d . . . . .
O10B O 0.8200(2) 0.66288(13) 0.36938(13) 0.0319(5) Uani 0.328(8) 1 d D . P A 2
H10A H 0.834800 0.687520 0.340910 0.048 Uiso 0.328(8) 1 d DR . P A 2
H10B H 0.8082(7) 0.62858(8) 0.3513(4) 0.048 Uiso 0.328(8) 1 d DR . P A 2
O12A O 0.8250(18) 0.5483(7) 0.3079(11) 0.097(7) Uani 0.328(8) 1 d . . P A 2
H12A H 0.859510 0.520593 0.332292 0.146 Uiso 0.328(8) 1 calc GR . P A 2
C34A C 0.854(3) 0.5513(14) 0.2435(17) 0.120(14) Uani 0.328(8) 1 d . . P A 2
H34A H 0.793750 0.560052 0.207348 0.181 Uiso 0.328(8) 1 calc GR . P A 2
H34B H 0.884827 0.511409 0.233755 0.181 Uiso 0.328(8) 1 calc GR . P A 2
H34C H 0.905623 0.584506 0.244204 0.181 Uiso 0.328(8) 1 calc GR . P A 2
Cl1B Cl 0.7853(15) 0.3659(11) 0.1529(7) 0.122(5) Uani 0.35(2) 1 d . . P B 4
O11 O 0.7727(4) 0.2752(3) 0.6056(3) 0.0882(11) Uani 1 1 d . . . . .
H11A H 0.774693 0.239826 0.624073 0.132 Uiso 1 1 calc GR . . . .
C33 C 0.8677(6) 0.2872(5) 0.5848(4) 0.0882(11) Uani 1 1 d . . . . .
H33A H 0.862796 0.326413 0.559004 0.132 Uiso 1 1 calc GR . . . .
H33B H 0.883037 0.253158 0.555164 0.132 Uiso 1 1 calc GR . . . .
H33C H 0.922972 0.290184 0.625998 0.132 Uiso 1 1 calc GR . . . .
O15A O 0.2174(8) 0.5980(6) 0.6402(5) 0.0882(11) Uani 0.576(9) 1 d D . P C 1
H15A H 0.255814 0.609210 0.612994 0.132 Uiso 0.576(9) 1 calc GR . P C 1
C37A C 0.2783(11) 0.5719(8) 0.7005(6) 0.0882(11) Uani 0.576(9) 1 d D . P C 1
H37A H 0.351700 0.578009 0.699573 0.132 Uiso 0.576(9) 1 calc GR . P C 1
H37B H 0.263744 0.527211 0.702113 0.132 Uiso 0.576(9) 1 calc GR . P C 1
H37C H 0.261875 0.592201 0.741676 0.132 Uiso 0.576(9) 1 calc GR . P C 1
O14 O 1.0024(4) 0.8272(2) 0.2658(4) 0.0878(17) Uani 1 1 d . . . . .
H14A H 1.065652 0.832813 0.281414 0.132 Uiso 1 1 calc GR . . . .
C36 C 0.9615(6) 0.8791(3) 0.2273(5) 0.079(2) Uani 1 1 d . . . . .
H36A H 1.004994 0.889594 0.193815 0.119 Uiso 1 1 calc GR . . . .
H36B H 0.959526 0.914414 0.258619 0.119 Uiso 1 1 calc GR . . . .
H36C H 0.891249 0.869717 0.202518 0.119 Uiso 1 1 calc GR . . . .
O13 O 0.8906(3) 0.72145(17) 0.26744(18) 0.0501(8) Uani 1 1 d . . . . .
H13A H 0.924880 0.754622 0.273476 0.075 Uiso 1 1 calc GR . . . .
C35 C 0.8404(6) 0.7170(4) 0.1973(3) 0.0720(18) Uani 1 1 d . . . . .
H35A H 0.892167 0.713977 0.167834 0.108 Uiso 1 1 calc GR . . . .
H35B H 0.797610 0.754033 0.184497 0.108 Uiso 1 1 calc GR . . . .
H35C H 0.796502 0.679785 0.190993 0.108 Uiso 1 1 calc GR . . . .
O12B O 0.7928(4) 0.4922(2) 0.1254(3) 0.0512(14) Uani 0.672(8) 1 d . . P A 1
H12B H 0.786329 0.453311 0.126318 0.077 Uiso 0.672(8) 1 calc GR . P A 1
C34B C 0.8036(7) 0.5160(4) 0.1932(5) 0.060(2) Uani 0.672(8) 1 d . . P A 1
H34D H 0.835630 0.557279 0.195347 0.090 Uiso 0.672(8) 1 calc GR . P A 1
H34E H 0.847306 0.487980 0.225767 0.090 Uiso 0.672(8) 1 calc GR . P A 1
H34F H 0.735331 0.519256 0.205625 0.090 Uiso 0.672(8) 1 calc GR . P A 1
O10A O 0.8200(2) 0.66288(13) 0.36938(13) 0.0319(5) Uani 0.672(8) 1 d D . P A 1
H10C H 0.781722 0.671132 0.331058 0.048 Uiso 0.672(8) 1 calc DGR . P A 1
C32 C 0.8712(6) 0.6046(3) 0.3645(4) 0.0520(19) Uani 0.672(8) 1 d D . P A 1
H32A H 0.905885 0.591339 0.410942 0.078 Uiso 0.672(8) 1 calc GR . P A 1
H32B H 0.922412 0.609562 0.334858 0.078 Uiso 0.672(8) 1 calc GR . P A 1
H32C H 0.820180 0.573218 0.344440 0.078 Uiso 0.672(8) 1 calc GR . P A 1
Cl1A Cl 0.7636(4) 0.35329(16) 0.1614(4) 0.0645(15) Uani 0.51(2) 1 d . . P D 1
Cl1C Cl 0.2259(11) 0.6799(6) 0.7442(7) 0.080(4) Uani 0.139(6) 1 d . . P E 3
O15B O 0.3214(9) 0.6216(8) 0.7182(6) 0.0882(11) Uani 0.424(9) 1 d D . P C -1
H15B H 0.310363 0.645063 0.750192 0.132 Uiso 0.424(9) 1 calc GR . P C -1
C37B C 0.2301(11) 0.6144(12) 0.6689(9) 0.0882(11) Uani 0.424(9) 1 d D . P C -1
H37D H 0.228510 0.645028 0.631714 0.132 Uiso 0.424(9) 1 calc R . P C -1
H37E H 0.170471 0.620744 0.691006 0.132 Uiso 0.424(9) 1 calc R . P C -1
H37F H 0.227554 0.572309 0.649277 0.132 Uiso 0.424(9) 1 calc R . P C -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
Y1 0.02613(15) 0.02388(15) 0.01630(14) 0.00115(9) 0.00135(10) -0.00236(10)
Y2 0.02439(15) 0.02334(15) 0.01778(14) 0.00239(9) 0.00136(10) -0.00120(9)
O1 0.0316(12) 0.0269(11) 0.0224(10) 0.0036(9) 0.0070(9) -0.0004(9)
O2 0.0285(11) 0.0288(12) 0.0226(10) 0.0049(9) 0.0044(9) 0.0001(9)
O3 0.0327(12) 0.0290(12) 0.0227(11) 0.0057(9) 0.0062(9) 0.0031(10)
O4 0.0271(11) 0.0296(12) 0.0251(11) 0.0051(9) 0.0051(9) -0.0004(9)
O5 0.0266(11) 0.0343(12) 0.0189(10) 0.0001(9) 0.0025(8) -0.0055(10)
O6 0.0275(11) 0.0314(12) 0.0177(10) 0.0006(9) 0.0032(8) -0.0025(9)
O8 0.0267(11) 0.0280(12) 0.0239(11) 0.0013(9) -0.0014(9) 0.0004(9)
O7 0.0271(11) 0.0253(11) 0.0250(11) 0.0003(9) 0.0024(9) -0.0009(9)
O9 0.0382(14) 0.0324(13) 0.0224(11) -0.0002(10) 0.0021(10) 0.0053(11)
N1 0.0331(15) 0.0262(13) 0.0207(13) 0.0005(10) 0.0001(11) -0.0022(11)
N2 0.0326(15) 0.0275(13) 0.0194(12) -0.0009(10) 0.0015(10) -0.0030(11)
N3 0.0367(16) 0.0328(15) 0.0211(13) -0.0031(11) 0.0055(11) -0.0038(12)
N4 0.0350(15) 0.0343(15) 0.0208(13) 0.0002(11) 0.0033(11) -0.0009(12)
N5 0.0366(16) 0.0335(15) 0.0194(12) 0.0022(11) 0.0017(11) -0.0042(12)
N6 0.0380(16) 0.0299(15) 0.0217(13) 0.0019(11) 0.0018(11) -0.0057(12)
N7 0.0343(16) 0.0320(15) 0.0263(14) -0.0002(11) 0.0007(12) -0.0065(12)
N8 0.0293(14) 0.0303(15) 0.0271(13) 0.0019(11) 0.0010(11) -0.0022(12)
N9 0.0445(18) 0.0272(14) 0.0233(13) -0.0011(11) 0.0017(12) -0.0018(13)
N10 0.0353(16) 0.0309(15) 0.0289(14) 0.0006(12) 0.0070(12) -0.0002(12)
N11 0.0361(16) 0.0273(14) 0.0294(14) 0.0028(12) 0.0030(12) -0.0036(12)
N12 0.0336(15) 0.0284(14) 0.0241(13) 0.0027(11) 0.0025(11) -0.0021(12)
C11 0.0292(18) 0.049(2) 0.040(2) -0.0023(18) -0.0029(15) -0.0031(17)
C1 0.0355(18) 0.0322(17) 0.0260(16) -0.0014(13) -0.0053(13) -0.0009(14)
C2 0.0267(17) 0.041(2) 0.0369(19) -0.0016(16) -0.0019(14) -0.0034(15)
C3 0.0307(17) 0.0342(18) 0.0294(17) -0.0001(14) 0.0030(13) -0.0012(14)
C4 0.043(2) 0.042(2) 0.0287(17) -0.0106(15) 0.0150(15) -0.0067(17)
C5 0.044(2) 0.043(2) 0.042(2) -0.0061(17) 0.0195(17) 0.0050(18)
C6 0.040(2) 0.040(2) 0.0304(18) 0.0008(15) 0.0094(15) 0.0021(16)
C7 0.0348(18) 0.043(2) 0.0243(16) 0.0101(15) 0.0014(13) -0.0027(16)
C8 0.0343(18) 0.0361(19) 0.0373(19) 0.0121(16) 0.0050(14) -0.0020(15)
C9 0.0374(19) 0.0286(17) 0.0331(18) 0.0028(14) 0.0030(14) -0.0036(14)
C27 0.0361(19) 0.048(2) 0.0244(15) -0.0016(15) 0.0104(14) -0.0080(16)
C10 0.034(2) 0.043(2) 0.038(2) 0.0008(16) -0.0024(15) -0.0093(16)
C12 0.0293(17) 0.0385(19) 0.0315(17) 0.0040(15) 0.0015(14) -0.0002(15)
C13 0.058(2) 0.0328(18) 0.0238(16) -0.0036(14) -0.0016(16) 0.0124(18)
C14 0.055(2) 0.040(2) 0.0294(17) 0.0002(16) 0.0121(16) 0.0153(18)
C15 0.043(2) 0.0367(19) 0.0295(17) 0.0059(14) 0.0107(15) 0.0076(16)
C16 0.052(2) 0.0300(18) 0.038(2) 0.0092(16) 0.0043(17) -0.0074(17)
C17 0.051(2) 0.042(2) 0.0303(18) 0.0143(16) 0.0012(16) -0.0025(18)
C18 0.043(2) 0.0344(19) 0.0256(17) 0.0045(14) 0.0024(14) -0.0024(15)
C19 0.0274(15) 0.0254(15) 0.0168(13) -0.0006(11) 0.0017(11) -0.0045(12)
C20 0.0259(15) 0.0247(15) 0.0196(14) 0.0015(11) -0.0007(11) -0.0010(12)
C21 0.0273(16) 0.0271(16) 0.0210(14) 0.0034(12) 0.0035(12) 0.0024(12)
C22 0.0284(16) 0.0275(16) 0.0243(14) 0.0055(13) 0.0030(12) 0.0019(13)
C23 0.0271(15) 0.0248(15) 0.0191(13) 0.0002(12) 0.0012(11) -0.0003(12)
C24 0.0258(15) 0.0256(15) 0.0188(13) 0.0006(11) 0.0018(11) -0.0017(12)
C25 0.0377(19) 0.0359(18) 0.0322(17) 0.0069(15) 0.0123(14) 0.0078(15)
C26 0.0353(19) 0.040(2) 0.049(2) 0.0176(18) 0.0175(16) 0.0098(16)
C28 0.0395(19) 0.048(2) 0.0190(15) -0.0001(14) 0.0057(13) -0.0075(16)
C29 0.039(2) 0.0264(17) 0.047(2) -0.0036(16) -0.0051(16) 0.0018(15)
C30 0.038(2) 0.0354(19) 0.042(2) 0.0005(16) -0.0063(16) 0.0060(16)
C31 0.051(3) 0.054(3) 0.048(2) -0.002(2) -0.002(2) 0.016(2)
B1 0.040(2) 0.035(2) 0.0182(16) -0.0025(15) 0.0027(14) -0.0060(17)
B2 0.037(2) 0.0293(19) 0.0290(18) 0.0010(15) 0.0005(15) -0.0064(16)
B3 0.0248(17) 0.0312(18) 0.0175(15) -0.0007(13) 0.0019(12) -0.0029(14)
O10B 0.0364(13) 0.0333(13) 0.0276(12) 0.0014(10) 0.0099(10) 0.0011(11)
O12A 0.153(19) 0.049(7) 0.110(13) -0.006(8) 0.075(14) -0.010(9)
C34A 0.20(4) 0.079(16) 0.11(2) -0.003(16) 0.11(3) 0.00(2)
Cl1B 0.098(8) 0.177(12) 0.073(4) 0.002(6) -0.028(5) 0.038(7)
O11 0.089(2) 0.113(3) 0.066(2) -0.0154(19) 0.0223(17) 0.015(2)
C33 0.089(2) 0.113(3) 0.066(2) -0.0154(19) 0.0223(17) 0.015(2)
O15A 0.089(2) 0.113(3) 0.066(2) -0.0154(19) 0.0223(17) 0.015(2)
C37A 0.089(2) 0.113(3) 0.066(2) -0.0154(19) 0.0223(17) 0.015(2)
O14 0.063(3) 0.051(2) 0.140(5) 0.021(3) -0.002(3) -0.004(2)
C36 0.075(4) 0.057(3) 0.111(6) 0.023(4) 0.033(4) 0.012(3)
O13 0.056(2) 0.0521(19) 0.0474(17) 0.0035(15) 0.0222(15) -0.0046(15)
C35 0.088(4) 0.088(4) 0.046(3) -0.007(3) 0.029(3) -0.025(4)
O12B 0.056(3) 0.041(3) 0.057(3) -0.001(2) 0.013(2) -0.004(2)
C34B 0.067(5) 0.055(4) 0.058(5) -0.002(4) 0.012(4) 0.013(4)
O10A 0.0364(13) 0.0333(13) 0.0276(12) 0.0014(10) 0.0099(10) 0.0011(11)
C32 0.072(5) 0.038(3) 0.057(4) 0.013(3) 0.041(4) 0.016(3)
Cl1A 0.0524(19) 0.031(2) 0.103(3) 0.0079(13) -0.0030(17) 0.0011(11)
Cl1C 0.091(9) 0.066(7) 0.087(8) 0.001(6) 0.031(6) -0.006(6)
O15B 0.089(2) 0.113(3) 0.066(2) -0.0154(19) 0.0223(17) 0.015(2)
C37B 0.089(2) 0.113(3) 0.066(2) -0.0154(19) 0.0223(17) 0.015(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 O1 2.287(2) . ?
Y1 O2 2.371(2) . ?
Y1 O5 2.323(2) . ?
Y1 O6 2.397(2) . ?
Y1 O9 2.317(3) . ?
Y1 N2 2.451(3) . ?
Y1 N4 2.467(3) . ?
Y1 N6 2.509(3) . ?
Y2 O3 2.304(2) . ?
Y2 O4 2.341(2) . ?
Y2 O8 2.341(2) 3_666 ?
Y2 O7 2.385(2) 3_666 ?
Y2 N8 2.431(3) . ?
Y2 N10 2.467(3) . ?
Y2 N12 2.479(3) . ?
Y2 B3 3.043(4) 3_666 ?
Y2 O10B 2.366(3) . ?
Y2 O10A 2.366(3) . ?
O1 C19 1.270(4) . ?
O2 C20 1.257(4) . ?
O3 C23 1.258(4) . ?
O4 C24 1.271(4) . ?
O5 C27 1.433(4) . ?
O5 B3 1.475(4) . ?
O6 C28 1.428(4) . ?
O6 B3 1.459(4) . ?
O8 C30 1.442(5) . ?
O8 B3 1.465(4) . ?
O7 C29 1.430(4) . ?
O7 B3 1.460(4) . ?
O9 H9 0.852(9) . ?
O9 C31 1.425(5) . ?
N1 N2 1.370(4) . ?
N1 C1 1.337(5) . ?
N1 B1 1.556(5) . ?
N2 C3 1.336(5) . ?
N3 N4 1.370(4) . ?
N3 C4 1.341(5) . ?
N3 B1 1.533(5) . ?
N4 C6 1.345(5) . ?
N5 N6 1.366(4) . ?
N5 C7 1.348(5) . ?
N5 B1 1.533(5) . ?
N6 C9 1.344(5) . ?
N7 N8 1.358(5) . ?
N7 C10 1.342(5) . ?
N7 B2 1.551(5) . ?
N8 C12 1.337(5) . ?
N9 N10 1.365(5) . ?
N9 C13 1.343(5) . ?
N9 B2 1.539(6) . ?
N10 C15 1.332(5) . ?
N11 N12 1.355(5) . ?
N11 C16 1.341(5) . ?
N11 B2 1.547(5) . ?
N12 C18 1.340(5) . ?
C11 H11 0.9500 . ?
C11 C10 1.372(7) . ?
C11 C12 1.385(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.377(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.393(5) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.375(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.396(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.384(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.392(5) . ?
C9 H9A 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C10 H10 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.377(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.394(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.374(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.379(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.530(5) . ?
C19 C21 1.395(5) . ?
C20 C22 1.407(5) . ?
C21 C23 1.400(5) . ?
C21 C25 1.502(5) . ?
C22 C24 1.402(5) . ?
C22 C26 1.500(5) . ?
C23 C24 1.536(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
B1 H1A 1.0000 . ?
B2 H2A 1.0000 . ?
O10B H10A 0.820(3) . ?
O10B H10B 0.8199(10) . ?
O12A H12A 0.8400 . ?
O12A C34A 1.40(3) . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
O11 H11A 0.8400 . ?
O11 C33 1.414(10) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O15A H15A 0.8400 . ?
O15A C37A 1.412(14) . ?
O15A C37B 0.656(16) . ?
C37A H37A 0.9800 . ?
C37A H37B 0.9800 . ?
C37A H37C 0.9800 . ?
C37A O15B 1.23(2) . ?
C37A C37B 1.21(3) . ?
O14 H14A 0.8400 . ?
O14 C36 1.396(8) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O13 H13A 0.8400 . ?
O13 C35 1.410(7) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
O12B H12B 0.8400 . ?
O12B C34B 1.407(10) . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 0.9800 . ?
O10A H10C 0.8400 . ?
O10A C32 1.433(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O15B H15B 0.8400 . ?
O15B C37B 1.3998(10) . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
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
O1 Y1 O2 67.44(9) . . ?
O1 Y1 O5 93.24(9) . . ?
O1 Y1 O6 80.08(8) . . ?
O1 Y1 O9 140.66(9) . . ?
O1 Y1 N2 99.68(9) . . ?
O1 Y1 N4 71.09(9) . . ?
O1 Y1 N6 144.77(10) . . ?
O2 Y1 O6 78.17(8) . . ?
O2 Y1 N2 77.79(9) . . ?
O2 Y1 N4 125.02(10) . . ?
O2 Y1 N6 140.70(10) . . ?
O5 Y1 O2 133.03(8) . . ?
O5 Y1 O6 55.90(8) . . ?
O5 Y1 N2 149.14(9) . . ?
O5 Y1 N4 82.73(10) . . ?
O5 Y1 N6 78.41(9) . . ?
O6 Y1 N2 153.96(9) . . ?
O6 Y1 N4 127.69(9) . . ?
O6 Y1 N6 119.88(9) . . ?
O9 Y1 O2 76.45(9) . . ?
O9 Y1 O5 100.49(10) . . ?
O9 Y1 O6 77.71(9) . . ?
O9 Y1 N2 87.05(10) . . ?
O9 Y1 N4 146.84(9) . . ?
O9 Y1 N6 74.48(10) . . ?
N2 Y1 N4 75.30(10) . . ?
N2 Y1 N6 74.88(10) . . ?
N4 Y1 N6 73.91(11) . . ?
O3 Y2 O4 67.84(9) . . ?
O3 Y2 O8 88.39(9) . 3_666 ?
O3 Y2 O7 78.74(9) . 3_666 ?
O3 Y2 N8 102.62(10) . . ?
O3 Y2 N10 71.27(10) . . ?
O3 Y2 N12 142.34(10) . . ?
O3 Y2 B3 83.10(9) . 3_666 ?
O3 Y2 O10B 144.09(9) . . ?
O3 Y2 O10A 144.09(9) . . ?
O4 Y2 O8 130.80(9) . 3_666 ?
O4 Y2 O7 76.96(9) . 3_666 ?
O4 Y2 N8 76.46(10) . . ?
O4 Y2 N10 122.80(10) . . ?
O4 Y2 N12 144.19(10) . . ?
O4 Y2 B3 104.16(10) . 3_666 ?
O4 Y2 O10B 79.80(9) . . ?
O4 Y2 O10A 79.80(9) . . ?
O8 Y2 O7 55.86(8) 3_666 3_666 ?
O8 Y2 N8 152.59(10) 3_666 . ?
O8 Y2 N10 84.82(10) 3_666 . ?
O8 Y2 N12 78.83(9) 3_666 . ?
O8 Y2 B3 27.87(10) 3_666 3_666 ?
O8 Y2 O10B 102.07(9) 3_666 . ?
O8 Y2 O10A 102.07(9) 3_666 . ?
O7 Y2 N8 150.51(10) 3_666 . ?
O7 Y2 N10 130.87(10) 3_666 . ?
O7 Y2 N12 119.75(9) 3_666 . ?
O7 Y2 B3 27.99(9) 3_666 3_666 ?
N8 Y2 N10 75.39(11) . . ?
N8 Y2 N12 77.22(10) . . ?
N8 Y2 B3 173.92(10) . 3_666 ?
N10 Y2 N12 72.39(11) . . ?
N10 Y2 B3 108.76(11) . 3_666 ?
N12 Y2 B3 99.58(10) . 3_666 ?
O10B Y2 N8 83.74(10) . . ?
O10B Y2 N10 143.13(10) . . ?
O10B Y2 N12 73.56(10) . . ?
O10B Y2 B3 90.40(10) . 3_666 ?
O10A Y2 O7 79.19(9) . 3_666 ?
O10A Y2 N8 83.74(10) . . ?
O10A Y2 N10 143.13(10) . . ?
O10A Y2 N12 73.56(10) . . ?
O10A Y2 B3 90.40(10) . 3_666 ?
C19 O1 Y1 122.9(2) . . ?
C20 O2 Y1 119.9(2) . . ?
C23 O3 Y2 121.8(2) . . ?
C24 O4 Y2 120.2(2) . . ?
C27 O5 Y1 135.6(2) . . ?
C27 O5 B3 119.7(3) . . ?
B3 O5 Y1 104.44(19) . . ?
C28 O6 Y1 138.4(2) . . ?
C28 O6 B3 119.1(3) . . ?
B3 O6 Y1 101.59(18) . . ?
C30 O8 Y2 136.1(2) . 3_666 ?
C30 O8 B3 119.9(3) . . ?
B3 O8 Y2 103.80(19) . 3_666 ?
C29 O7 Y2 138.5(2) . 3_666 ?
C29 O7 B3 119.5(3) . . ?
B3 O7 Y2 101.95(19) . 3_666 ?
Y1 O9 H9 121.3(15) . . ?
C31 O9 Y1 128.3(3) . . ?
C31 O9 H9 107.2(15) . . ?
N2 N1 B1 122.5(3) . . ?
C1 N1 N2 109.6(3) . . ?
C1 N1 B1 127.9(3) . . ?
N1 N2 Y1 123.3(2) . . ?
C3 N2 Y1 130.5(2) . . ?
C3 N2 N1 106.0(3) . . ?
N4 N3 B1 121.8(3) . . ?
C4 N3 N4 109.7(3) . . ?
C4 N3 B1 128.5(3) . . ?
N3 N4 Y1 123.9(2) . . ?
C6 N4 Y1 130.5(2) . . ?
C6 N4 N3 105.6(3) . . ?
N6 N5 B1 121.5(3) . . ?
C7 N5 N6 110.2(3) . . ?
C7 N5 B1 128.3(3) . . ?
N5 N6 Y1 123.2(2) . . ?
C9 N6 Y1 131.2(2) . . ?
C9 N6 N5 105.6(3) . . ?
N8 N7 B2 122.2(3) . . ?
C10 N7 N8 109.6(3) . . ?
C10 N7 B2 128.2(3) . . ?
N7 N8 Y2 123.6(2) . . ?
C12 N8 Y2 130.0(3) . . ?
C12 N8 N7 106.3(3) . . ?
N10 N9 B2 120.9(3) . . ?
C13 N9 N10 109.8(4) . . ?
C13 N9 B2 128.8(4) . . ?
N9 N10 Y2 123.8(2) . . ?
C15 N10 Y2 130.1(3) . . ?
C15 N10 N9 106.1(3) . . ?
N12 N11 B2 121.7(3) . . ?
C16 N11 N12 109.9(3) . . ?
C16 N11 B2 127.3(3) . . ?
N11 N12 Y2 123.2(2) . . ?
C18 N12 Y2 130.1(3) . . ?
C18 N12 N11 105.8(3) . . ?
C10 C11 H11 127.7 . . ?
C10 C11 C12 104.7(4) . . ?
C12 C11 H11 127.7 . . ?
N1 C1 H1 125.4 . . ?
N1 C1 C2 109.2(3) . . ?
C2 C1 H1 125.4 . . ?
C1 C2 H2 127.9 . . ?
C1 C2 C3 104.2(3) . . ?
C3 C2 H2 127.9 . . ?
N2 C3 C2 111.0(3) . . ?
N2 C3 H3 124.5 . . ?
C2 C3 H3 124.5 . . ?
N3 C4 H4 125.3 . . ?
N3 C4 C5 109.4(3) . . ?
C5 C4 H4 125.3 . . ?
C4 C5 H5 128.0 . . ?
C4 C5 C6 104.1(4) . . ?
C6 C5 H5 128.0 . . ?
N4 C6 C5 111.2(4) . . ?
N4 C6 H6 124.4 . . ?
C5 C6 H6 124.4 . . ?
N5 C7 H7 125.7 . . ?
N5 C7 C8 108.6(3) . . ?
C8 C7 H7 125.7 . . ?
C7 C8 H8 127.9 . . ?
C7 C8 C9 104.3(3) . . ?
C9 C8 H8 127.9 . . ?
N6 C9 C8 111.4(4) . . ?
N6 C9 H9A 124.3 . . ?
C8 C9 H9A 124.3 . . ?
O5 C27 H27A 109.5 . . ?
O5 C27 H27B 109.5 . . ?
O5 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C10 C11 108.8(4) . . ?
N7 C10 H10 125.6 . . ?
C11 C10 H10 125.6 . . ?
N8 C12 C11 110.7(4) . . ?
N8 C12 H12 124.7 . . ?
C11 C12 H12 124.7 . . ?
N9 C13 H13 125.6 . . ?
N9 C13 C14 108.7(4) . . ?
C14 C13 H13 125.6 . . ?
C13 C14 H14 127.8 . . ?
C13 C14 C15 104.4(4) . . ?
C15 C14 H14 127.8 . . ?
N10 C15 C14 111.0(4) . . ?
N10 C15 H15 124.5 . . ?
C14 C15 H15 124.5 . . ?
N11 C16 H16 125.6 . . ?
N11 C16 C17 108.8(4) . . ?
C17 C16 H16 125.6 . . ?
C16 C17 H17 127.8 . . ?
C16 C17 C18 104.4(3) . . ?
C18 C17 H17 127.8 . . ?
N12 C18 C17 111.2(4) . . ?
N12 C18 H18 124.4 . . ?
C17 C18 H18 124.4 . . ?
O1 C19 C20 114.4(3) . . ?
O1 C19 C21 123.4(3) . . ?
C21 C19 C20 122.1(3) . . ?
O2 C20 C19 115.0(3) . . ?
O2 C20 C22 124.3(3) . . ?
C22 C20 C19 120.7(3) . . ?
C19 C21 C23 116.9(3) . . ?
C19 C21 C25 121.5(3) . . ?
C23 C21 C25 121.6(3) . . ?
C20 C22 C26 121.4(3) . . ?
C24 C22 C20 117.5(3) . . ?
C24 C22 C26 121.1(3) . . ?
O3 C23 C21 123.5(3) . . ?
O3 C23 C24 114.9(3) . . ?
C21 C23 C24 121.6(3) . . ?
O4 C24 C22 124.5(3) . . ?
O4 C24 C23 114.5(3) . . ?
C22 C24 C23 121.0(3) . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O6 C28 H28A 109.5 . . ?
O6 C28 H28B 109.5 . . ?
O6 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O7 C29 H29A 109.5 . . ?
O7 C29 H29B 109.5 . . ?
O7 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O8 C30 H30A 109.5 . . ?
O8 C30 H30B 109.5 . . ?
O8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O9 C31 H31A 109.5 . . ?
O9 C31 H31B 109.5 . . ?
O9 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N1 B1 H1A 109.9 . . ?
N3 B1 N1 109.5(3) . . ?
N3 B1 H1A 109.9 . . ?
N5 B1 N1 108.3(3) . . ?
N5 B1 N3 109.3(3) . . ?
N5 B1 H1A 109.9 . . ?
N7 B2 H2A 109.9 . . ?
N9 B2 N7 109.6(3) . . ?
N9 B2 N11 107.0(3) . . ?
N9 B2 H2A 109.9 . . ?
N11 B2 N7 110.4(3) . . ?
N11 B2 H2A 109.9 . . ?
O5 B3 Y2 128.8(2) . 3_666 ?
O6 B3 Y2 133.3(2) . 3_666 ?
O6 B3 O5 97.9(2) . . ?
O6 B3 O8 115.7(3) . . ?
O6 B3 O7 116.7(3) . . ?
O8 B3 Y2 48.33(14) . 3_666 ?
O8 B3 O5 114.9(3) . . ?
O7 B3 Y2 50.05(15) . 3_666 ?
O7 B3 O5 114.3(3) . . ?
O7 B3 O8 98.4(2) . . ?
Y2 O10B H10A 119.9(2) . . ?
Y2 O10B H10B 118.5(3) . . ?
H10A O10B H10B 109.5(3) . . ?
C34A O12A H12A 109.5 . . ?
O12A C34A H34A 109.5 . . ?
O12A C34A H34B 109.5 . . ?
O12A C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C33 O11 H11A 109.5 . . ?
O11 C33 H33A 109.5 . . ?
O11 C33 H33B 109.5 . . ?
O11 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C37A O15A H15A 109.5 . . ?
C37B O15A H15A 107.9 . . ?
C37B O15A C37A 59(2) . . ?
O15A C37A H37A 109.5 . . ?
O15A C37A H37B 109.5 . . ?
O15A C37A H37C 109.5 . . ?
H37A C37A H37B 109.5 . . ?
H37A C37A H37C 109.5 . . ?
H37B C37A H37C 109.5 . . ?
O15B C37A O15A 92.8(13) . . ?
O15B C37A H37A 58.9 . . ?
O15B C37A H37B 157.7 . . ?
O15B C37A H37C 62.8 . . ?
C37B C37A O15A 27.7(9) . . ?
C37B C37A H37A 108.0 . . ?
C37B C37A H37B 131.8 . . ?
C37B C37A H37C 84.8 . . ?
C37B C37A O15B 70.0(12) . . ?
C36 O14 H14A 109.5 . . ?
O14 C36 H36A 109.5 . . ?
O14 C36 H36B 109.5 . . ?
O14 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 O13 H13A 109.5 . . ?
O13 C35 H35A 109.5 . . ?
O13 C35 H35B 109.5 . . ?
O13 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34B O12B H12B 109.5 . . ?
O12B C34B H34D 109.5 . . ?
O12B C34B H34E 109.5 . . ?
O12B C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
Y2 O10A H10C 102.4 . . ?
C32 O10A Y2 130.0(3) . . ?
C32 O10A H10C 109.5 . . ?
O10A C32 H32A 109.5 . . ?
O10A C32 H32B 109.5 . . ?
O10A C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C37A O15B H15B 126.7 . . ?
C37A O15B C37B 54.5(13) . . ?
C37B O15B H15B 109.5 . . ?
O15A C37B C37A 93(3) . . ?
O15A C37B O15B 134(2) . . ?
O15A C37B H37D 75.9 . . ?
O15A C37B H37E 111.2 . . ?
O15A C37B H37F 35.6 . . ?
C37A C37B O15B 55.5(11) . . ?
C37A C37B H37D 145.2 . . ?
C37A C37B H37E 105.3 . . ?
C37A C37B H37F 58.8 . . ?
O15B C37B H37D 109.5 . . ?
O15B C37B H37E 109.5 . . ?
O15B C37B H37F 109.5 . . ?
H37D C37B H37E 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
_shelx_res_file
;
TITL 5-Y-MeOH_a.res in P2(1)/c
5-y-meoh.res
created by SHELXL-2016/6 at 17:19:19 on 21-Jun-2017
REM Old TITL 5-Y-MeOH in P21/c #14
REM SHELXT solution in P2(1)/c
REM R1 0.103, Rweak 0.030, Alpha 0.046, Orientation as input
REM Formula found by SHELXT: C46 B N10 O13 Y2
CELL 1.54184 13.186849 21.481474 19.643393 90 101.2134 90
ZERR 2 0.000291 0.000418 0.000352 0 0.0018 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H B Cl N O Y
UNIT 146.69 261.38 12 4 48 60 8
DFIX 0.85 0.01 O10A H10C
DFIX 0.82 0.001 O10B H10B
DFIX 1.34 0.001 H10A H10B
DFIX 2.85 0.001 Y2 H10B
DFIX 0.85 0.01 O9 H9
DFIX 1.46 O15A C37A
DFIX 1.4 0.001 C37B O15B
DANG 2.902118 0.02 Y2 H10C
DANG 1.891083 0.02 C32 H10C
DANG 1.872335 0.02 C31 H9
DANG 2.858143 0.02 Y1 H9
EADP O10A O10B
EADP C37A O15B
EADP O15A C37A
EADP O11 O15B O15A
EADP O15B C37B
EADP C33 C37A C37B
EXYZ O10A O10B
SUMP 1 0.001 1 4 1 5 1 6
L.S. 10
PLAN 10
TEMP -143
FREE Y1 B3
FREE B3 Y2
BOND $H
LIST 6
fmap 2
acta
OMIT 6 20 6
OMIT 10 16 5
OMIT 5 21 9
OMIT -11 14 4
OMIT 0 1 2
OMIT -5 9 16
REM
REM
REM
WGHT 0.082600 8.220800
FVAR 0.25174 0.67236 0.57600 0.50543 0.35487 0.13931
Y1 7 0.658845 0.411409 0.741747 11.00000 0.02613 0.02388 =
0.01630 0.00115 0.00135 -0.00236
Y2 7 0.719018 0.696303 0.449725 11.00000 0.02439 0.02334 =
0.01778 0.00239 0.00136 -0.00120
O1 6 0.600885 0.504577 0.692802 11.00000 0.03158 0.02691 =
0.02239 0.00358 0.00698 -0.00043
O2 6 0.768049 0.452531 0.670105 11.00000 0.02853 0.02876 =
0.02257 0.00487 0.00444 0.00006
O3 6 0.638606 0.663967 0.537708 11.00000 0.03269 0.02897 =
0.02272 0.00572 0.00624 0.00309
O4 6 0.799642 0.609119 0.508091 11.00000 0.02708 0.02962 =
0.02510 0.00514 0.00508 -0.00044
O5 6 0.495383 0.366693 0.718091 11.00000 0.02656 0.03433 =
0.01891 0.00012 0.00252 -0.00546
O6 6 0.574356 0.376550 0.629043 11.00000 0.02752 0.03143 =
0.01774 0.00059 0.00319 -0.00249
O8 6 0.444559 0.292227 0.621059 11.00000 0.02666 0.02799 =
0.02386 0.00127 -0.00144 0.00037
O7 6 0.383158 0.388127 0.604720 11.00000 0.02712 0.02532 =
0.02496 0.00026 0.00242 -0.00089
O9 6 0.759394 0.326989 0.723126 11.00000 0.03821 0.03238 =
0.02237 -0.00020 0.00211 0.00526
H9 2 0.758421 0.313007 0.682429 11.00000 -1.50000
N1 5 0.809509 0.449819 0.897035 11.00000 0.03314 0.02621 =
0.02066 0.00053 0.00013 -0.00224
N2 5 0.808044 0.447624 0.827135 11.00000 0.03262 0.02749 =
0.01937 -0.00094 0.00153 -0.00297
N3 5 0.621346 0.471538 0.896422 11.00000 0.03672 0.03281 =
0.02105 -0.00312 0.00546 -0.00375
N4 5 0.583518 0.472005 0.826337 11.00000 0.03497 0.03434 =
0.02085 0.00024 0.00328 -0.00090
N5 5 0.689598 0.362749 0.912039 11.00000 0.03664 0.03350 =
0.01943 0.00216 0.00167 -0.00417
N6 5 0.665109 0.341920 0.845150 11.00000 0.03804 0.02993 =
0.02170 0.00194 0.00185 -0.00571
N7 5 0.905695 0.798776 0.517710 11.00000 0.03431 0.03205 =
0.02628 -0.00025 0.00069 -0.00646
N8 5 0.882479 0.737148 0.512785 11.00000 0.02933 0.03034 =
0.02715 0.00187 0.00097 -0.00223
N9 5 0.728553 0.841989 0.520813 11.00000 0.04454 0.02725 =
0.02326 -0.00105 0.00173 -0.00178
N10 5 0.670932 0.788816 0.510782 11.00000 0.03530 0.03093 =
0.02885 0.00061 0.00701 -0.00021
N11 5 0.790278 0.842459 0.409339 11.00000 0.03608 0.02730 =
0.02936 0.00276 0.00300 -0.00356
N12 5 0.746609 0.789135 0.380570 11.00000 0.03358 0.02844 =
0.02409 0.00272 0.00251 -0.00208
C11 1 1.045589 0.748899 0.570120 11.00000 0.02924 0.04921 =
0.04005 -0.00228 -0.00290 -0.00307
AFIX 43
H11 2 1.113457 0.739791 0.594551 11.00000 -1.20000
AFIX 0
C1 1 0.903053 0.467688 0.930537 11.00000 0.03552 0.03222 =
0.02604 -0.00139 -0.00533 -0.00090
AFIX 43
H1 2 0.923018 0.472962 0.979326 11.00000 -1.20000
AFIX 0
C2 1 0.965923 0.477246 0.883127 11.00000 0.02672 0.04064 =
0.03695 -0.00157 -0.00186 -0.00337
AFIX 43
H2 2 1.036360 0.489767 0.891985 11.00000 -1.20000
AFIX 0
C3 1 0.902680 0.464367 0.819232 11.00000 0.03072 0.03425 =
0.02936 -0.00011 0.00295 -0.00121
AFIX 43
H3 2 0.923977 0.467119 0.775826 11.00000 -1.20000
AFIX 0
C4 1 0.565382 0.510052 0.928234 11.00000 0.04312 0.04212 =
0.02866 -0.01061 0.01504 -0.00671
AFIX 43
H4 2 0.577009 0.517655 0.976775 11.00000 -1.20000
AFIX 0
C5 1 0.488555 0.536828 0.879671 11.00000 0.04387 0.04294 =
0.04151 -0.00611 0.01954 0.00505
AFIX 43
H5 2 0.437254 0.565666 0.887229 11.00000 -1.20000
AFIX 0
C6 1 0.503327 0.511869 0.816726 11.00000 0.04028 0.03989 =
0.03042 0.00075 0.00937 0.00208
AFIX 43
H6 2 0.462107 0.521749 0.772804 11.00000 -1.20000
AFIX 0
C7 1 0.689565 0.315003 0.956539 11.00000 0.03479 0.04264 =
0.02434 0.01013 0.00142 -0.00268
AFIX 43
H7 2 0.704643 0.317896 1.005733 11.00000 -1.20000
AFIX 0
C8 1 0.663902 0.261067 0.918600 11.00000 0.03432 0.03606 =
0.03725 0.01210 0.00499 -0.00204
AFIX 43
H8 2 0.657376 0.220177 0.935664 11.00000 -1.20000
AFIX 0
C9 1 0.649818 0.280340 0.849739 11.00000 0.03739 0.02857 =
0.03306 0.00283 0.00299 -0.00360
AFIX 43
H9A 2 0.631703 0.253390 0.810932 11.00000 -1.20000
AFIX 0
C27 1 0.416431 0.353931 0.756987 11.00000 0.03614 0.04790 =
0.02443 -0.00163 0.01042 -0.00796
AFIX 137
H27A 2 0.433483 0.315607 0.783839 11.00000 -1.50000
H27B 2 0.349912 0.348825 0.725084 11.00000 -1.50000
H27C 2 0.411887 0.388629 0.788645 11.00000 -1.50000
AFIX 0
C10 1 1.003347 0.806361 0.552020 11.00000 0.03440 0.04267 =
0.03786 0.00076 -0.00237 -0.00933
AFIX 43
H10 2 1.037600 0.845141 0.562118 11.00000 -1.20000
AFIX 0
C12 1 0.967260 0.707127 0.544843 11.00000 0.02927 0.03845 =
0.03154 0.00400 0.00154 -0.00021
AFIX 43
H12 2 0.972984 0.663192 0.549625 11.00000 -1.20000
AFIX 0
C13 1 0.680426 0.884693 0.553139 11.00000 0.05775 0.03276 =
0.02378 -0.00365 -0.00159 0.01243
AFIX 43
H13 2 0.705460 0.925304 0.566141 11.00000 -1.20000
AFIX 0
C14 1 0.588807 0.859858 0.564309 11.00000 0.05487 0.04040 =
0.02940 0.00023 0.01214 0.01533
AFIX 43
H14 2 0.538171 0.879304 0.585536 11.00000 -1.20000
AFIX 0
C15 1 0.587142 0.799736 0.537433 11.00000 0.04297 0.03666 =
0.02954 0.00588 0.01066 0.00764
AFIX 43
H15 2 0.533379 0.770425 0.538039 11.00000 -1.20000
AFIX 0
C16 1 0.778994 0.887699 0.361447 11.00000 0.05209 0.02996 =
0.03821 0.00921 0.00430 -0.00739
AFIX 43
H16 2 0.802924 0.929301 0.369133 11.00000 -1.20000
AFIX 0
C17 1 0.727104 0.863984 0.299393 11.00000 0.05124 0.04181 =
0.03026 0.01427 0.00117 -0.00248
AFIX 43
H17 2 0.708143 0.885075 0.256285 11.00000 -1.20000
AFIX 0
C18 1 0.708790 0.802652 0.313864 11.00000 0.04256 0.03440 =
0.02563 0.00451 0.00238 -0.00245
AFIX 43
H18 2 0.673894 0.773735 0.280832 11.00000 -1.20000
AFIX 0
C19 1 0.644511 0.532973 0.649581 11.00000 0.02740 0.02538 =
0.01684 -0.00063 0.00175 -0.00454
C20 1 0.742548 0.501391 0.635803 11.00000 0.02588 0.02473 =
0.01963 0.00147 -0.00067 -0.00097
C21 1 0.607899 0.588807 0.617670 11.00000 0.02735 0.02706 =
0.02096 0.00345 0.00354 0.00240
C22 1 0.797216 0.526502 0.587435 11.00000 0.02844 0.02752 =
0.02428 0.00545 0.00297 0.00190
C23 1 0.663128 0.614036 0.570173 11.00000 0.02715 0.02476 =
0.01910 0.00020 0.00124 -0.00029
C24 1 0.759265 0.581648 0.553587 11.00000 0.02583 0.02557 =
0.01875 0.00060 0.00184 -0.00168
C25 1 0.515016 0.621104 0.634828 11.00000 0.03769 0.03587 =
0.03217 0.00693 0.01231 0.00778
AFIX 137
H25A 2 0.452582 0.606722 0.603196 11.00000 -1.50000
H25B 2 0.522273 0.666177 0.629727 11.00000 -1.50000
H25C 2 0.509586 0.611487 0.682756 11.00000 -1.50000
AFIX 0
C26 1 0.892585 0.495590 0.572598 11.00000 0.03530 0.03957 =
0.04913 0.01758 0.01752 0.00981
AFIX 137
H26A 2 0.950804 0.503736 0.610856 11.00000 -1.50000
H26B 2 0.908291 0.512234 0.529364 11.00000 -1.50000
H26C 2 0.880966 0.450604 0.567881 11.00000 -1.50000
AFIX 0
C28 1 0.589365 0.379694 0.559049 11.00000 0.03945 0.04812 =
0.01898 -0.00010 0.00569 -0.00748
AFIX 137
H28A 2 0.558831 0.418237 0.537510 11.00000 -1.50000
H28B 2 0.556017 0.343854 0.533002 11.00000 -1.50000
H28C 2 0.663546 0.379147 0.558609 11.00000 -1.50000
AFIX 0
C29 1 0.376323 0.454373 0.609590 11.00000 0.03948 0.02645 =
0.04707 -0.00359 -0.00508 0.00181
AFIX 137
H29A 2 0.433559 0.473617 0.592052 11.00000 -1.50000
H29B 2 0.380280 0.466308 0.658188 11.00000 -1.50000
H29C 2 0.310446 0.468583 0.581868 11.00000 -1.50000
AFIX 0
C30 1 0.516219 0.241732 0.641183 11.00000 0.03796 0.03538 =
0.04220 0.00054 -0.00631 0.00596
AFIX 137
H30A 2 0.482484 0.202169 0.625660 11.00000 -1.50000
H30B 2 0.538088 0.241282 0.691801 11.00000 -1.50000
H30C 2 0.576771 0.247439 0.619760 11.00000 -1.50000
AFIX 0
C31 1 0.851565 0.304445 0.766375 11.00000 0.05128 0.05354 =
0.04772 -0.00211 -0.00203 0.01636
AFIX 137
H31A 2 0.850928 0.258826 0.766367 11.00000 -1.50000
H31B 2 0.855376 0.319698 0.813825 11.00000 -1.50000
H31C 2 0.911757 0.319313 0.748668 11.00000 -1.50000
AFIX 0
B1 3 0.714459 0.431432 0.928786 11.00000 0.03976 0.03539 =
0.01821 -0.00254 0.00274 -0.00598
AFIX 13
H1A 2 0.730673 0.437663 0.980210 11.00000 -1.20000
AFIX 0
B2 3 0.825422 0.849674 0.488774 11.00000 0.03694 0.02929 =
0.02902 0.00103 0.00048 -0.00635
AFIX 13
H2A 2 0.856126 0.891896 0.499915 11.00000 -1.20000
AFIX 0
B3 3 0.474590 0.356010 0.642471 11.00000 0.02484 0.03116 =
0.01754 -0.00066 0.00187 -0.00291
PART 2
O10B 6 0.820042 0.662880 0.369383 -21.00000 0.03640 0.03331 =
0.02759 0.00142 0.00989 0.00106
H10A 2 10.834800 10.687520 10.340910 -21.00000 -1.50000
H10B 2 0.808170 0.628579 0.351276 -21.00000 -1.50000
O12A 6 0.824984 0.548292 0.307932 -21.00000 0.15323 0.04897 =
0.10956 -0.00632 0.07530 -0.00954
AFIX 147
H12A 2 0.859510 0.520593 0.332292 -21.00000 -1.50000
AFIX 0
C34A 1 0.854494 0.551288 0.243511 -21.00000 0.20024 0.07945 =
0.11221 -0.00293 0.10565 0.00379
AFIX 137
H34A 2 0.793750 0.560052 0.207348 -21.00000 -1.50000
H34B 2 0.884827 0.511409 0.233755 -21.00000 -1.50000
H34C 2 0.905623 0.584506 0.244204 -21.00000 -1.50000
AFIX 0
PART 0
PART 4
CL1B 4 0.785311 0.365947 0.152895 51.00000 0.09823 0.17725 =
0.07332 0.00154 -0.02757 0.03761
PART 0
O11 6 0.772660 0.275183 0.605591 11.00000 0.08860 0.11328 =
0.06558 -0.01538 0.02225 0.01505
AFIX 147
H11A 2 0.774693 0.239826 0.624073 11.00000 -1.50000
AFIX 0
C33 1 0.867658 0.287153 0.584847 11.00000 0.08860 0.11328 =
0.06558 -0.01538 0.02225 0.01505
AFIX 137
H33A 2 0.862796 0.326413 0.559004 11.00000 -1.50000
H33B 2 0.883037 0.253158 0.555164 11.00000 -1.50000
H33C 2 0.922972 0.290184 0.625998 11.00000 -1.50000
AFIX 0
PART 1
O15A 6 0.217443 0.598020 0.640242 31.00000 0.08860 0.11328 =
0.06558 -0.01538 0.02225 0.01505
AFIX 147
H15A 2 0.255814 0.609210 0.612994 31.00000 -1.50000
AFIX 0
C37A 1 0.278345 0.571861 0.700507 31.00000 0.08860 0.11328 =
0.06558 -0.01538 0.02225 0.01505
AFIX 137
H37A 2 0.351700 0.578009 0.699573 31.00000 -1.50000
H37B 2 0.263744 0.527211 0.702113 31.00000 -1.50000
H37C 2 0.261875 0.592201 0.741676 31.00000 -1.50000
AFIX 0
PART 0
O14 6 1.002359 0.827160 0.265849 11.00000 0.06345 0.05109 =
0.13998 0.02059 -0.00245 -0.00420
AFIX 147
H14A 2 1.065652 0.832813 0.281414 11.00000 -1.50000
AFIX 0
C36 1 0.961487 0.879090 0.227331 11.00000 0.07468 0.05736 =
0.11124 0.02253 0.03349 0.01230
AFIX 137
H36A 2 1.004994 0.889594 0.193815 11.00000 -1.50000
H36B 2 0.959526 0.914414 0.258619 11.00000 -1.50000
H36C 2 0.891249 0.869717 0.202518 11.00000 -1.50000
AFIX 0
O13 6 0.890575 0.721451 0.267440 11.00000 0.05567 0.05214 =
0.04741 0.00346 0.02218 -0.00457
AFIX 147
H13A 2 0.924880 0.754622 0.273476 11.00000 -1.50000
AFIX 0
C35 1 0.840386 0.716970 0.197345 11.00000 0.08834 0.08773 =
0.04632 -0.00745 0.02894 -0.02530
AFIX 137
H35A 2 0.892167 0.713977 0.167834 11.00000 -1.50000
H35B 2 0.797610 0.754033 0.184497 11.00000 -1.50000
H35C 2 0.796502 0.679785 0.190993 11.00000 -1.50000
AFIX 0
PART 1
O12B 6 0.792806 0.492187 0.125422 21.00000 0.05588 0.04083 =
0.05749 -0.00148 0.01274 -0.00443
AFIX 147
H12B 2 0.786329 0.453311 0.126318 21.00000 -1.50000
AFIX 0
C34B 1 0.803586 0.515981 0.193180 21.00000 0.06733 0.05473 =
0.05830 -0.00154 0.01165 0.01266
AFIX 137
H34D 2 0.835630 0.557279 0.195347 21.00000 -1.50000
H34E 2 0.847306 0.487980 0.225767 21.00000 -1.50000
H34F 2 0.735331 0.519256 0.205625 21.00000 -1.50000
AFIX 0
O10A 6 0.820042 0.662880 0.369383 21.00000 0.03640 0.03331 =
0.02759 0.00142 0.00989 0.00106
AFIX 147
H10C 2 0.781722 0.671132 0.331058 21.00000 -1.50000
AFIX 0
C32 1 0.871171 0.604648 0.364522 21.00000 0.07237 0.03832 =
0.05685 0.01299 0.04090 0.01597
AFIX 137
H32A 2 0.905885 0.591339 0.410942 21.00000 -1.50000
H32B 2 0.922412 0.609562 0.334858 21.00000 -1.50000
H32C 2 0.820180 0.573218 0.344440 21.00000 -1.50000
AFIX 0
CL1A 4 0.763606 0.353289 0.161426 41.00000 0.05244 0.03132 =
0.10252 0.00790 -0.00298 0.00114
PART 0
PART 3
CL1C 4 0.225906 0.679942 0.744170 61.00000 0.09080 0.06601 =
0.08736 0.00141 0.03064 -0.00580
PART 0
PART -1
O15B 6 0.321416 0.621557 0.718245 -31.00000 0.08860 0.11328 =
0.06558 -0.01538 0.02225 0.01505
AFIX 147
H15B 2 0.310363 0.645063 0.750192 -31.00000 -1.50000
AFIX 0
C37B 1 0.230145 0.614371 0.668858 -31.00000 0.08860 0.11328 =
0.06558 -0.01538 0.02225 0.01505
AFIX 133
H37D 2 0.228510 0.645028 0.631714 -31.00000 -1.50000
H37E 2 0.170471 0.620744 0.691006 -31.00000 -1.50000
H37F 2 0.227554 0.572309 0.649277 -31.00000 -1.50000
AFIX 0
HKLF 4
REM 5-Y-MeOH_a.res in P2(1)/c
REM R1 = 0.0558 for 10142 Fo > 4sig(Fo) and 0.0624 for all 11486 data
REM 688 parameters refined using 12 restraints
END
WGHT 0.0825 8.2272
REM Highest difference peak 1.371, deepest hole -1.457, 1-sigma level 0.142
Q1 1 0.5638 0.4072 0.7402 11.00000 0.05 1.37
Q2 1 0.7463 0.4094 0.7444 11.00000 0.05 1.29
Q3 1 0.8098 0.6947 0.4527 11.00000 0.05 1.19
Q4 1 0.6281 0.6949 0.4462 11.00000 0.05 1.18
Q5 1 0.4454 0.3034 0.5521 11.00000 0.05 1.02
Q6 1 0.8893 0.6965 0.4517 11.00000 0.05 1.01
Q7 1 0.4977 0.4105 0.7430 11.00000 0.05 0.97
Q8 1 0.8275 0.4116 0.7445 11.00000 0.05 0.93
Q9 1 0.7790 0.6624 0.4224 11.00000 0.05 0.91
Q10 1 0.6863 0.3775 0.7718 11.00000 0.05 0.90
;
_shelx_res_checksum 11190
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.756
_oxdiff_exptl_absorpt_empirical_full_min 0.543
# start Validation Reply Form
_vrf_PLAT417_5-y-meoh
;
PROBLEM: Short Inter D-H..H-D H9 .. H11A .. 2.00 Ang.
RESPONSE: Those hydrogen atoms are involved in a H-bond network including a Cl
atom disordered over 3 positions. Those hydrogens are therefore poorly resolved.
;
_vrf_PLAT420_5-y-meoh
;
PROBLEM: D-H Without Acceptor >O15A -- >H15A ... Please Check
RESPONSE: those atoms are on a disordered methanol molecule.
;
# 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_3-ydcm
_database_code_depnum_ccdc_archive 'CCDC 1566110'
_audit_update_record
;
2017-08-02 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_audit_creation_date 2017-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C44 H46 B4 N24 O4 Y2'
_chemical_formula_sum 'C44 H46 B4 N24 O4 Y2'
_chemical_formula_weight 1196.11
_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'
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'
Y Y -2.7962 3.5667 '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 148
_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'
'-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 49.226(7)
_cell_length_b 49.226(7)
_cell_length_c 13.220(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 27743(10)
_cell_formula_units_Z 18
_cell_measurement_reflns_used 2714
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 32.089
_cell_measurement_theta_min 0.407
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.931
_exptl_absorpt_correction_T_max 0.4342
_exptl_absorpt_correction_T_min 0.2940
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1181 before and 0.0897 after correction.
The Ratio of minimum to maximum transmission is 0.6771.
The \l/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'light purple'
_exptl_crystal_density_diffrn 1.289
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 10944
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.005
_exptl_crystal_size_min 0.005
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1746
_diffrn_reflns_av_unetI/netI 0.0806
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max 72
_diffrn_reflns_limit_h_min -72
_diffrn_reflns_limit_k_max 70
_diffrn_reflns_limit_k_min -71
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 260816
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 31.854
_diffrn_reflns_theta_min 0.827
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type 'ADSC Quantum 210r'
_diffrn_measurement_method 'Phi Scan'
_diffrn_radiation_monochromator 'Silicon Double Crystal'
_diffrn_radiation_type Synchrotron
_diffrn_radiation_wavelength 0.7108
_diffrn_source 'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 11662
_reflns_number_total 19276
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_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 'XDS (Kabsch, 1993)'
_computing_data_collection 'BluIce (McPhillips, 2002)'
_computing_data_reduction 'XDS (Kabsch, 1993)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max 0.433
_refine_diff_density_min -1.667
_refine_diff_density_rms 0.104
_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 705
_refine_ls_number_reflns 19276
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1118
_refine_ls_R_factor_gt 0.0576
_refine_ls_restrained_S_all 1.035
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+15.6478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1335
_refine_ls_wR_factor_ref 0.1547
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
B1(H1), B2(H2), B3(H3), B4(H4)
2.b Aromatic/amide H refined with riding coordinates:
C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
2.c Idealised Me refined as rotating group:
C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_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
Y1 Y 0.36981(2) 0.55716(2) 0.39207(2) 0.02745(7) Uani 1 1 d . . . . .
Y2 Y 0.56331(2) 0.64241(2) 0.52879(2) 0.03269(8) Uani 1 1 d . . . . .
O1 O 0.41890(5) 0.57182(5) 0.33027(16) 0.0315(4) Uani 1 1 d . . . . .
O2 O 0.40625(5) 0.57113(5) 0.52281(15) 0.0302(4) Uani 1 1 d . . . . .
O3 O 0.52611(5) 0.61974(6) 0.40272(17) 0.0372(5) Uani 1 1 d . . . . .
O4 O 0.51357(5) 0.61673(5) 0.59563(16) 0.0348(5) Uani 1 1 d . . . . .
N1 N 0.33693(6) 0.59341(6) 0.52050(19) 0.0319(5) Uani 1 1 d . . . . .
N2 N 0.34489(6) 0.57057(6) 0.52850(19) 0.0335(5) Uani 1 1 d . . . . .
N3 N 0.38434(6) 0.63317(6) 0.42181(19) 0.0306(5) Uani 1 1 d . . . . .
N4 N 0.39926(6) 0.61708(6) 0.39393(19) 0.0300(5) Uani 1 1 d . . . . .
N5 N 0.33376(6) 0.59930(6) 0.33202(19) 0.0306(5) Uani 1 1 d . . . . .
N6 N 0.33862(6) 0.57578(6) 0.29778(19) 0.0305(5) Uani 1 1 d . . . . .
N7 N 0.35325(7) 0.48092(6) 0.3876(2) 0.0386(6) Uani 1 1 d . . . . .
N8 N 0.36913(7) 0.50820(6) 0.4427(2) 0.0366(6) Uani 1 1 d . . . . .
N9 N 0.30494(7) 0.48387(7) 0.3517(2) 0.0382(6) Uani 1 1 d . . . . .
N10 N 0.31378(6) 0.51299(6) 0.3903(2) 0.0352(6) Uani 1 1 d . . . . .
N11 N 0.34549(7) 0.49844(6) 0.2156(2) 0.0373(6) Uani 1 1 d . . . . .
N12 N 0.36335(6) 0.53013(6) 0.2294(2) 0.0331(5) Uani 1 1 d . . . . .
N13 N 0.56295(7) 0.71216(7) 0.4991(2) 0.0388(6) Uani 1 1 d . . . . .
N14 N 0.54408(6) 0.68160(7) 0.5270(2) 0.0370(6) Uani 1 1 d . . . . .
N15 N 0.61567(7) 0.72108(7) 0.5489(2) 0.0418(7) Uani 1 1 d . . . . .
N16 N 0.60511(6) 0.69316(7) 0.5983(2) 0.0392(6) Uani 1 1 d . . . . .
N17 N 0.59692(7) 0.70521(7) 0.3688(2) 0.0430(7) Uani 1 1 d . . . . .
N18 N 0.58742(7) 0.67407(7) 0.3764(2) 0.0404(6) Uani 1 1 d . . . . .
N19 N 0.56865(7) 0.57641(7) 0.5709(2) 0.0449(7) Uani 1 1 d . . . . .
N20 N 0.55261(6) 0.58704(7) 0.5146(2) 0.0417(6) Uani 1 1 d . . . . .
N21 N 0.62109(7) 0.62503(7) 0.5821(2) 0.0422(7) Uani 1 1 d . . . . .
N22 N 0.61459(7) 0.64295(7) 0.5189(2) 0.0402(6) Uani 1 1 d . . . . .
N23 N 0.58221(7) 0.60997(7) 0.7266(2) 0.0418(6) Uani 1 1 d . . . . .
N24 N 0.56827(6) 0.62703(7) 0.7013(2) 0.0383(6) Uani 1 1 d . . . . .
C5 C 0.31793(8) 0.59062(9) 0.5996(2) 0.0377(7) Uani 1 1 d . . . . .
H5 H 0.309341 0.603825 0.611782 0.045 Uiso 1 1 calc R . . . .
C6 C 0.31321(8) 0.56591(9) 0.6582(2) 0.0426(8) Uani 1 1 d . . . . .
H6 H 0.300768 0.558346 0.717656 0.051 Uiso 1 1 calc R . . . .
C7 C 0.33058(8) 0.55416(8) 0.6121(2) 0.0376(7) Uani 1 1 d . . . . .
H7 H 0.332132 0.536836 0.636548 0.045 Uiso 1 1 calc R . . . .
C8 C 0.40527(8) 0.66410(7) 0.4289(2) 0.0351(7) Uani 1 1 d . . . . .
H8 H 0.400563 0.679978 0.446934 0.042 Uiso 1 1 calc R . . . .
C9 C 0.43466(8) 0.66885(8) 0.4056(2) 0.0375(7) Uani 1 1 d . . . . .
H9 H 0.453943 0.688158 0.404208 0.045 Uiso 1 1 calc R . . . .
C10 C 0.42968(7) 0.63903(7) 0.3844(2) 0.0333(6) Uani 1 1 d . . . . .
H10 H 0.445771 0.634700 0.365675 0.040 Uiso 1 1 calc R . . . .
C11 C 0.31495(7) 0.60331(9) 0.2665(2) 0.0362(7) Uani 1 1 d . . . . .
H11 H 0.308298 0.618315 0.273116 0.043 Uiso 1 1 calc R . . . .
C12 C 0.30702(7) 0.58209(8) 0.1887(2) 0.0369(7) Uani 1 1 d . . . . .
H12 H 0.294049 0.579434 0.132093 0.044 Uiso 1 1 calc R . . . .
C13 C 0.32220(7) 0.56533(8) 0.2113(2) 0.0336(6) Uani 1 1 d . . . . .
H13 H 0.321093 0.548812 0.171102 0.040 Uiso 1 1 calc R . . . .
C14 C 0.36092(10) 0.45984(8) 0.4234(3) 0.0482(9) Uani 1 1 d . . . . .
H14 H 0.353278 0.439264 0.397646 0.058 Uiso 1 1 calc R . . . .
C15 C 0.38140(10) 0.47282(9) 0.5024(3) 0.0482(9) Uani 1 1 d . . . . .
H15 H 0.390509 0.463369 0.542189 0.058 Uiso 1 1 calc R . . . .
C16 C 0.38590(8) 0.50296(9) 0.5115(3) 0.0410(7) Uani 1 1 d . . . . .
H16 H 0.399174 0.517893 0.560218 0.049 Uiso 1 1 calc R . . . .
C17 C 0.27339(8) 0.46661(9) 0.3482(3) 0.0458(9) Uani 1 1 d . . . . .
H17 H 0.261545 0.445652 0.324335 0.055 Uiso 1 1 calc R . . . .
C18 C 0.26119(8) 0.48451(9) 0.3853(3) 0.0455(9) Uani 1 1 d . . . . .
H18 H 0.239712 0.478585 0.392064 0.055 Uiso 1 1 calc R . . . .
C19 C 0.28710(7) 0.51295(9) 0.4103(2) 0.0388(7) Uani 1 1 d . . . . .
H19 H 0.286110 0.530231 0.438084 0.047 Uiso 1 1 calc R . . . .
C20 C 0.34634(8) 0.49134(8) 0.1174(3) 0.0414(8) Uani 1 1 d . . . . .
H20 H 0.335862 0.470853 0.089132 0.050 Uiso 1 1 calc R . . . .
C21 C 0.36488(9) 0.51866(9) 0.0649(3) 0.0434(8) Uani 1 1 d . . . . .
H21 H 0.369683 0.520953 -0.005241 0.052 Uiso 1 1 calc R . . . .
C22 C 0.37501(8) 0.54222(8) 0.1378(2) 0.0372(7) Uani 1 1 d . . . . .
H22 H 0.388374 0.563932 0.124510 0.045 Uiso 1 1 calc R . . . .
C23 C 0.54878(8) 0.72886(8) 0.5187(3) 0.0406(8) Uani 1 1 d . . . . .
H23 H 0.557459 0.750681 0.506652 0.049 Uiso 1 1 calc R . . . .
C24 C 0.51963(9) 0.70918(9) 0.5590(3) 0.0424(8) Uani 1 1 d . . . . .
H24 H 0.504236 0.714268 0.579772 0.051 Uiso 1 1 calc R . . . .
C25 C 0.51788(8) 0.68015(8) 0.5624(3) 0.0385(7) Uani 1 1 d . . . . .
H25 H 0.500243 0.661519 0.586769 0.046 Uiso 1 1 calc R . . . .
C26 C 0.64296(9) 0.74280(9) 0.5891(3) 0.0519(9) Uani 1 1 d . . . . .
H26 H 0.654833 0.764027 0.567747 0.062 Uiso 1 1 calc R . . . .
C27 C 0.65101(9) 0.72957(9) 0.6658(3) 0.0522(10) Uani 1 1 d . . . . .
H27 H 0.669104 0.739390 0.707649 0.063 Uiso 1 1 calc R . . . .
C28 C 0.62674(8) 0.69844(9) 0.6691(3) 0.0445(8) Uani 1 1 d . . . . .
H28 H 0.625686 0.683106 0.715040 0.053 Uiso 1 1 calc R . . . .
C29 C 0.60547(9) 0.71510(10) 0.2727(3) 0.0522(10) Uani 1 1 d . . . . .
H29 H 0.612802 0.735818 0.248757 0.063 Uiso 1 1 calc R . . . .
C30 C 0.60180(9) 0.69013(11) 0.2153(3) 0.0547(10) Uani 1 1 d . . . . .
H30 H 0.605980 0.689987 0.145158 0.066 Uiso 1 1 calc R . . . .
C31 C 0.59054(9) 0.66504(10) 0.2833(3) 0.0482(9) Uani 1 1 d . . . . .
H31 H 0.585745 0.644381 0.266035 0.058 Uiso 1 1 calc R . . . .
C32 C 0.55819(10) 0.54581(9) 0.5486(3) 0.0547(10) Uani 1 1 d . . . . .
H32 H 0.565650 0.533110 0.577600 0.066 Uiso 1 1 calc R . . . .
C33 C 0.53497(10) 0.53638(9) 0.4770(4) 0.0574(11) Uani 1 1 d . . . . .
H33 H 0.523328 0.516236 0.446891 0.069 Uiso 1 1 calc R . . . .
C34 C 0.53217(9) 0.56277(9) 0.4582(3) 0.0503(9) Uani 1 1 d . . . . .
H34 H 0.517767 0.563420 0.411771 0.060 Uiso 1 1 calc R . . . .
C35 C 0.65216(8) 0.63554(9) 0.5806(3) 0.0475(9) Uani 1 1 d . . . . .
H35 H 0.662471 0.626908 0.618327 0.057 Uiso 1 1 calc R . . . .
C36 C 0.66657(8) 0.66065(9) 0.5161(3) 0.0483(9) Uani 1 1 d . . . . .
H36 H 0.688264 0.672711 0.500384 0.058 Uiso 1 1 calc R . . . .
C37 C 0.64220(8) 0.66448(9) 0.4789(3) 0.0446(8) Uani 1 1 d . . . . .
H37 H 0.644741 0.680141 0.431709 0.054 Uiso 1 1 calc R . . . .
C38 C 0.57861(9) 0.60340(9) 0.8256(3) 0.0496(9) Uani 1 1 d . . . . .
H38 H 0.586247 0.591785 0.860969 0.060 Uiso 1 1 calc R . . . .
C39 C 0.56215(9) 0.61616(10) 0.8673(3) 0.0517(9) Uani 1 1 d . . . . .
H39 H 0.556203 0.615336 0.936068 0.062 Uiso 1 1 calc R . . . .
C40 C 0.55594(9) 0.63065(9) 0.7870(3) 0.0440(8) Uani 1 1 d . . . . .
H40 H 0.544595 0.641530 0.792452 0.053 Uiso 1 1 calc R . . . .
C41 C 0.44230(7) 0.58170(7) 0.3893(2) 0.0308(6) Uani 1 1 d . . . . .
C42 C 0.43503(7) 0.58164(7) 0.5015(2) 0.0301(6) Uani 1 1 d . . . . .
C43 C 0.47291(7) 0.59324(8) 0.3539(2) 0.0333(6) Uani 1 1 d . . . . .
C44 C 0.45916(7) 0.59284(7) 0.5732(2) 0.0314(6) Uani 1 1 d . . . . .
C45 C 0.49704(7) 0.60626(7) 0.4248(2) 0.0329(6) Uani 1 1 d . . . . .
C46 C 0.48978(7) 0.60502(7) 0.5377(2) 0.0317(6) Uani 1 1 d . . . . .
C47 C 0.47899(8) 0.59372(9) 0.2419(2) 0.0418(8) Uani 1 1 d . . . . .
H47A H 0.466636 0.572445 0.214526 0.063 Uiso 1 1 calc GR . . . .
H47B H 0.501345 0.601421 0.230449 0.063 Uiso 1 1 calc GR . . . .
H47C H 0.472941 0.607597 0.207937 0.063 Uiso 1 1 calc GR . . . .
C48 C 0.45283(8) 0.59285(8) 0.6846(2) 0.0372(7) Uani 1 1 d . . . . .
H48A H 0.432820 0.592300 0.694308 0.056 Uiso 1 1 calc GR . . . .
H48B H 0.469746 0.611887 0.715692 0.056 Uiso 1 1 calc GR . . . .
H48C H 0.451787 0.574360 0.716349 0.056 Uiso 1 1 calc GR . . . .
B1 B 0.34823(8) 0.61685(9) 0.4318(3) 0.0327(7) Uani 1 1 d . . . . .
H1 H 0.341837 0.632950 0.443558 0.039 Uiso 1 1 calc R . . . .
B2 B 0.32927(9) 0.47645(9) 0.3060(3) 0.0394(8) Uani 1 1 d . . . . .
H2 H 0.318421 0.454192 0.282124 0.047 Uiso 1 1 calc R . . . .
B3 B 0.59687(9) 0.72450(10) 0.4615(3) 0.0429(9) Uani 1 1 d . . . . .
H3 H 0.606482 0.747099 0.442239 0.051 Uiso 1 1 calc R . . . .
B4 B 0.59548(10) 0.59766(10) 0.6429(3) 0.0456(9) Uani 1 1 d . . . . .
H4 H 0.604385 0.585350 0.674624 0.055 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Y1 0.02592(14) 0.03020(14) 0.02731(14) 0.00142(10) -0.00014(10) 0.01484(11)
Y2 0.02661(14) 0.03421(16) 0.03791(17) -0.00167(12) -0.00137(11) 0.01570(12)
O1 0.0301(11) 0.0374(11) 0.0299(11) 0.0011(8) -0.0004(8) 0.0190(9)
O2 0.0253(10) 0.0351(11) 0.0306(11) 0.0018(8) 0.0014(8) 0.0154(9)
O3 0.0249(10) 0.0470(13) 0.0373(12) -0.0026(10) 0.0022(9) 0.0162(10)
O4 0.0296(11) 0.0391(12) 0.0359(12) -0.0016(9) -0.0040(9) 0.0173(10)
N1 0.0324(13) 0.0456(15) 0.0249(13) -0.0026(10) -0.0023(9) 0.0248(12)
N2 0.0324(13) 0.0429(15) 0.0295(13) 0.0010(11) 0.0001(10) 0.0220(12)
N3 0.0331(13) 0.0333(13) 0.0290(13) -0.0012(10) -0.0037(10) 0.0194(11)
N4 0.0285(12) 0.0340(13) 0.0318(13) 0.0009(10) -0.0003(10) 0.0189(11)
N5 0.0297(12) 0.0393(14) 0.0274(13) 0.0009(10) -0.0015(9) 0.0208(11)
N6 0.0303(12) 0.0330(13) 0.0284(13) 0.0001(10) -0.0002(9) 0.0161(11)
N7 0.0422(15) 0.0317(14) 0.0414(16) 0.0041(11) 0.0023(12) 0.0181(12)
N8 0.0385(14) 0.0344(14) 0.0402(15) 0.0014(11) -0.0006(11) 0.0206(12)
N9 0.0365(14) 0.0369(14) 0.0325(14) 0.0032(11) 0.0019(11) 0.0117(12)
N10 0.0349(14) 0.0369(14) 0.0325(14) 0.0027(11) 0.0018(10) 0.0170(12)
N11 0.0419(15) 0.0323(14) 0.0351(15) -0.0016(11) 0.0036(11) 0.0165(12)
N12 0.0307(13) 0.0312(13) 0.0338(14) 0.0003(10) 0.0028(10) 0.0129(11)
N13 0.0357(14) 0.0364(14) 0.0457(17) 0.0003(12) -0.0041(12) 0.0190(12)
N14 0.0324(13) 0.0391(15) 0.0401(15) -0.0015(11) -0.0023(11) 0.0183(12)
N15 0.0337(14) 0.0320(14) 0.0547(19) -0.0020(12) -0.0064(12) 0.0126(12)
N16 0.0336(14) 0.0369(15) 0.0483(17) -0.0062(12) -0.0080(12) 0.0184(12)
N17 0.0320(14) 0.0452(16) 0.0482(18) 0.0067(13) 0.0022(12) 0.0166(13)
N18 0.0338(14) 0.0410(15) 0.0457(17) 0.0001(12) 0.0031(12) 0.0181(12)
N19 0.0415(16) 0.0349(15) 0.060(2) 0.0035(13) 0.0046(14) 0.0206(13)
N20 0.0289(13) 0.0435(16) 0.0528(18) -0.0039(13) 0.0015(12) 0.0182(12)
N21 0.0327(14) 0.0443(16) 0.0527(18) -0.0014(13) -0.0022(12) 0.0215(13)
N22 0.0348(14) 0.0356(14) 0.0504(17) -0.0007(12) -0.0012(12) 0.0176(12)
N23 0.0384(15) 0.0439(16) 0.0481(17) 0.0036(13) -0.0015(12) 0.0243(13)
N24 0.0322(14) 0.0403(15) 0.0457(17) -0.0003(12) -0.0033(11) 0.0207(12)
C5 0.0366(17) 0.052(2) 0.0290(16) -0.0057(13) -0.0004(12) 0.0254(15)
C6 0.0386(18) 0.061(2) 0.0258(16) -0.0006(14) 0.0040(13) 0.0232(17)
C7 0.0377(17) 0.0435(18) 0.0287(16) 0.0055(13) 0.0022(12) 0.0181(14)
C8 0.0443(18) 0.0331(16) 0.0317(16) 0.0001(12) -0.0051(13) 0.0222(14)
C9 0.0364(17) 0.0341(16) 0.0359(17) 0.0040(13) -0.0025(13) 0.0131(14)
C10 0.0299(15) 0.0337(15) 0.0345(16) 0.0052(12) 0.0008(12) 0.0145(13)
C11 0.0319(15) 0.058(2) 0.0282(16) 0.0057(13) 0.0010(12) 0.0294(15)
C12 0.0318(15) 0.054(2) 0.0273(16) 0.0021(13) -0.0019(12) 0.0231(15)
C13 0.0319(15) 0.0394(17) 0.0257(15) 0.0016(12) -0.0013(11) 0.0150(13)
C14 0.058(2) 0.0339(17) 0.056(2) 0.0089(15) 0.0061(18) 0.0259(17)
C15 0.058(2) 0.047(2) 0.051(2) 0.0134(16) 0.0064(17) 0.0352(19)
C16 0.0463(19) 0.0439(19) 0.0404(19) 0.0077(14) 0.0026(14) 0.0283(16)
C17 0.0339(17) 0.049(2) 0.0346(18) 0.0046(15) 0.0008(13) 0.0061(15)
C18 0.0310(16) 0.063(2) 0.0307(17) 0.0076(15) 0.0017(13) 0.0152(16)
C19 0.0295(15) 0.0497(19) 0.0327(17) 0.0079(14) 0.0036(12) 0.0164(14)
C20 0.0462(19) 0.0415(18) 0.0380(19) -0.0074(14) 0.0017(14) 0.0232(16)
C21 0.053(2) 0.048(2) 0.0345(18) -0.0024(14) 0.0053(15) 0.0294(17)
C22 0.0359(16) 0.0376(17) 0.0343(17) 0.0046(13) 0.0071(13) 0.0156(14)
C23 0.0436(19) 0.0379(17) 0.047(2) -0.0060(14) -0.0100(15) 0.0255(15)
C24 0.0463(19) 0.050(2) 0.0413(19) -0.0051(15) -0.0010(15) 0.0317(17)
C25 0.0394(17) 0.0429(18) 0.0394(18) -0.0040(14) 0.0012(13) 0.0253(15)
C26 0.0379(19) 0.042(2) 0.070(3) -0.0074(18) -0.0117(17) 0.0153(16)
C27 0.0381(19) 0.051(2) 0.067(3) -0.0159(19) -0.0186(17) 0.0221(17)
C28 0.0389(18) 0.0458(19) 0.053(2) -0.0113(16) -0.0133(15) 0.0243(16)
C29 0.0390(19) 0.061(2) 0.054(2) 0.0192(19) 0.0107(16) 0.0237(18)
C30 0.044(2) 0.072(3) 0.047(2) 0.0086(19) 0.0088(16) 0.028(2)
C31 0.0380(18) 0.060(2) 0.047(2) -0.0003(17) 0.0064(15) 0.0247(18)
C32 0.053(2) 0.0356(19) 0.077(3) 0.0019(18) 0.012(2) 0.0239(18)
C33 0.048(2) 0.038(2) 0.077(3) -0.0103(19) 0.007(2) 0.0142(17)
C34 0.0361(18) 0.043(2) 0.067(3) -0.0140(18) 0.0004(17) 0.0164(16)
C35 0.0321(17) 0.053(2) 0.062(2) -0.0071(18) -0.0056(16) 0.0253(16)
C36 0.0276(16) 0.050(2) 0.063(2) -0.0100(18) -0.0018(15) 0.0167(15)
C37 0.0335(17) 0.0417(19) 0.056(2) -0.0012(16) 0.0052(15) 0.0171(15)
C38 0.051(2) 0.052(2) 0.049(2) 0.0087(17) -0.0033(17) 0.0281(19)
C39 0.051(2) 0.060(2) 0.048(2) 0.0072(18) 0.0042(17) 0.030(2)
C40 0.0428(19) 0.051(2) 0.043(2) -0.0018(15) -0.0047(15) 0.0274(17)
C41 0.0335(15) 0.0353(15) 0.0282(15) 0.0018(11) -0.0004(11) 0.0205(13)
C42 0.0313(14) 0.0313(14) 0.0310(15) 0.0037(11) 0.0021(11) 0.0181(12)
C43 0.0318(15) 0.0396(16) 0.0316(16) -0.0013(12) 0.0028(12) 0.0201(13)
C44 0.0296(14) 0.0376(16) 0.0279(15) 0.0008(12) -0.0016(11) 0.0174(13)
C45 0.0296(15) 0.0371(16) 0.0335(16) -0.0004(12) 0.0013(12) 0.0179(13)
C46 0.0315(15) 0.0339(15) 0.0313(16) 0.0001(12) 0.0000(11) 0.0175(13)
C47 0.0315(16) 0.056(2) 0.0320(17) -0.0033(14) 0.0034(12) 0.0179(15)
C48 0.0333(16) 0.0464(18) 0.0297(16) 0.0002(13) -0.0003(12) 0.0182(14)
B1 0.0355(18) 0.0425(19) 0.0288(18) -0.0019(14) -0.0039(13) 0.0261(16)
B2 0.044(2) 0.0297(17) 0.037(2) 0.0021(14) 0.0015(15) 0.0126(16)
B3 0.038(2) 0.0359(19) 0.053(2) 0.0029(17) -0.0031(17) 0.0172(17)
B4 0.042(2) 0.045(2) 0.054(3) -0.0004(18) -0.0057(18) 0.0252(19)
_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
Y1 O1 2.298(2) . ?
Y1 O2 2.333(2) . ?
Y1 N2 2.450(3) . ?
Y1 N4 2.555(3) . ?
Y1 N6 2.482(3) . ?
Y1 N8 2.485(3) . ?
Y1 N10 2.518(3) . ?
Y1 N12 2.464(3) . ?
Y2 O3 2.309(2) . ?
Y2 O4 2.298(2) . ?
Y2 N14 2.539(3) . ?
Y2 N16 2.486(3) . ?
Y2 N18 2.459(3) . ?
Y2 N20 2.511(3) . ?
Y2 N22 2.514(3) . ?
Y2 N24 2.453(3) . ?
O1 C41 1.270(4) . ?
O2 C42 1.273(4) . ?
O3 C45 1.274(4) . ?
O4 C46 1.271(4) . ?
N1 N2 1.367(4) . ?
N1 C5 1.363(4) . ?
N1 B1 1.541(4) . ?
N2 C7 1.342(4) . ?
N3 N4 1.373(3) . ?
N3 C8 1.349(4) . ?
N3 B1 1.547(4) . ?
N4 C10 1.345(4) . ?
N5 N6 1.371(3) . ?
N5 C11 1.352(4) . ?
N5 B1 1.542(4) . ?
N6 C13 1.345(4) . ?
N7 N8 1.376(4) . ?
N7 C14 1.355(4) . ?
N7 B2 1.532(5) . ?
N8 C16 1.337(4) . ?
N9 N10 1.372(4) . ?
N9 C17 1.347(4) . ?
N9 B2 1.540(5) . ?
N10 C19 1.339(4) . ?
N11 N12 1.367(4) . ?
N11 C20 1.351(4) . ?
N11 B2 1.540(5) . ?
N12 C22 1.345(4) . ?
N13 N14 1.365(4) . ?
N13 C23 1.342(4) . ?
N13 B3 1.547(5) . ?
N14 C25 1.340(4) . ?
N15 N16 1.368(4) . ?
N15 C26 1.340(4) . ?
N15 B3 1.542(5) . ?
N16 C28 1.342(4) . ?
N17 N18 1.364(4) . ?
N17 C29 1.350(5) . ?
N17 B3 1.550(5) . ?
N18 C31 1.342(5) . ?
N19 N20 1.366(4) . ?
N19 C32 1.358(5) . ?
N19 B4 1.538(5) . ?
N20 C34 1.339(5) . ?
N21 N22 1.365(4) . ?
N21 C35 1.347(4) . ?
N21 B4 1.534(5) . ?
N22 C37 1.345(4) . ?
N23 N24 1.366(4) . ?
N23 C38 1.338(5) . ?
N23 B4 1.553(5) . ?
N24 C40 1.339(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.361(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.390(5) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.380(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(5) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.376(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.394(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.368(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.392(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C17 C18 1.381(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.382(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C20 C21 1.377(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.394(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.375(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.389(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C26 C27 1.366(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.395(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C29 C30 1.378(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.399(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C32 C33 1.373(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.396(6) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C35 C36 1.371(6) . ?
C36 H36 0.9500 . ?
C36 C37 1.394(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C38 C39 1.365(6) . ?
C39 H39 0.9500 . ?
C39 C40 1.395(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.526(4) . ?
C41 C43 1.398(4) . ?
C42 C44 1.399(4) . ?
C43 C45 1.393(4) . ?
C43 C47 1.508(4) . ?
C44 C46 1.396(4) . ?
C44 C48 1.506(4) . ?
C45 C46 1.528(4) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
B1 H1 1.0000 . ?
B2 H2 1.0000 . ?
B3 H3 1.0000 . ?
B4 H4 1.0000 . ?
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
O1 Y1 O2 68.79(7) . . ?
O1 Y1 N2 140.03(8) . . ?
O1 Y1 N4 74.95(8) . . ?
O1 Y1 N6 116.93(8) . . ?
O1 Y1 N8 84.41(8) . . ?
O1 Y1 N10 142.52(8) . . ?
O1 Y1 N12 72.00(8) . . ?
O2 Y1 N2 77.88(8) . . ?
O2 Y1 N4 75.15(8) . . ?
O2 Y1 N6 142.15(8) . . ?
O2 Y1 N8 73.86(8) . . ?
O2 Y1 N10 127.62(8) . . ?
O2 Y1 N12 132.71(8) . . ?
N2 Y1 N4 75.72(9) . . ?
N2 Y1 N6 77.56(8) . . ?
N2 Y1 N8 107.30(9) . . ?
N2 Y1 N10 76.10(9) . . ?
N2 Y1 N12 147.24(9) . . ?
N6 Y1 N4 71.16(8) . . ?
N6 Y1 N8 141.50(9) . . ?
N6 Y1 N10 72.62(9) . . ?
N8 Y1 N4 147.33(9) . . ?
N8 Y1 N10 71.78(9) . . ?
N10 Y1 N4 137.84(8) . . ?
N12 Y1 N4 118.51(8) . . ?
N12 Y1 N6 79.89(9) . . ?
N12 Y1 N8 77.05(9) . . ?
N12 Y1 N10 74.67(9) . . ?
O3 Y2 N14 81.57(9) . . ?
O3 Y2 N16 144.14(9) . . ?
O3 Y2 N18 74.32(9) . . ?
O3 Y2 N20 74.70(9) . . ?
O3 Y2 N22 121.13(9) . . ?
O3 Y2 N24 134.34(9) . . ?
O4 Y2 O3 69.03(8) . . ?
O4 Y2 N14 73.86(9) . . ?
O4 Y2 N16 121.98(9) . . ?
O4 Y2 N18 135.04(9) . . ?
O4 Y2 N20 81.03(9) . . ?
O4 Y2 N22 144.47(9) . . ?
O4 Y2 N24 73.48(8) . . ?
N16 Y2 N14 71.07(9) . . ?
N16 Y2 N20 137.52(9) . . ?
N16 Y2 N22 71.73(9) . . ?
N18 Y2 N14 75.86(9) . . ?
N18 Y2 N16 76.79(10) . . ?
N18 Y2 N20 113.54(10) . . ?
N18 Y2 N22 77.70(10) . . ?
N20 Y2 N14 150.28(9) . . ?
N20 Y2 N22 70.87(9) . . ?
N22 Y2 N14 138.19(9) . . ?
N24 Y2 N14 112.07(9) . . ?
N24 Y2 N16 78.84(10) . . ?
N24 Y2 N18 150.04(10) . . ?
N24 Y2 N20 74.56(10) . . ?
N24 Y2 N22 78.31(9) . . ?
C41 O1 Y1 120.81(19) . . ?
C42 O2 Y1 119.41(18) . . ?
C45 O3 Y2 119.9(2) . . ?
C46 O4 Y2 120.3(2) . . ?
N2 N1 B1 122.0(2) . . ?
C5 N1 N2 108.8(3) . . ?
C5 N1 B1 129.2(3) . . ?
N1 N2 Y1 123.54(18) . . ?
C7 N2 Y1 128.8(2) . . ?
C7 N2 N1 106.2(3) . . ?
N4 N3 B1 122.0(2) . . ?
C8 N3 N4 110.0(3) . . ?
C8 N3 B1 127.7(3) . . ?
N3 N4 Y1 120.70(18) . . ?
C10 N4 Y1 133.5(2) . . ?
C10 N4 N3 105.3(2) . . ?
N6 N5 B1 121.9(2) . . ?
C11 N5 N6 109.5(3) . . ?
C11 N5 B1 128.6(3) . . ?
N5 N6 Y1 123.20(18) . . ?
C13 N6 Y1 130.6(2) . . ?
C13 N6 N5 106.2(2) . . ?
N8 N7 B2 122.3(3) . . ?
C14 N7 N8 108.8(3) . . ?
C14 N7 B2 128.7(3) . . ?
N7 N8 Y1 122.0(2) . . ?
C16 N8 Y1 131.3(2) . . ?
C16 N8 N7 106.0(3) . . ?
N10 N9 B2 121.1(3) . . ?
C17 N9 N10 109.6(3) . . ?
C17 N9 B2 128.7(3) . . ?
N9 N10 Y1 123.0(2) . . ?
C19 N10 Y1 130.5(2) . . ?
C19 N10 N9 105.9(3) . . ?
N12 N11 B2 120.7(3) . . ?
C20 N11 N12 109.7(3) . . ?
C20 N11 B2 129.5(3) . . ?
N11 N12 Y1 124.62(19) . . ?
C22 N12 Y1 129.5(2) . . ?
C22 N12 N11 105.9(3) . . ?
N14 N13 B3 121.7(3) . . ?
C23 N13 N14 110.3(3) . . ?
C23 N13 B3 127.7(3) . . ?
N13 N14 Y2 122.2(2) . . ?
C25 N14 Y2 132.1(2) . . ?
C25 N14 N13 105.0(3) . . ?
N16 N15 B3 121.3(3) . . ?
C26 N15 N16 109.8(3) . . ?
C26 N15 B3 128.9(3) . . ?
N15 N16 Y2 122.7(2) . . ?
C28 N16 Y2 129.1(2) . . ?
C28 N16 N15 105.8(3) . . ?
N18 N17 B3 121.7(3) . . ?
C29 N17 N18 110.1(3) . . ?
C29 N17 B3 128.2(3) . . ?
N17 N18 Y2 123.9(2) . . ?
C31 N18 Y2 129.8(3) . . ?
C31 N18 N17 105.9(3) . . ?
N20 N19 B4 122.8(3) . . ?
C32 N19 N20 109.6(3) . . ?
C32 N19 B4 127.5(3) . . ?
N19 N20 Y2 121.8(2) . . ?
C34 N20 Y2 131.8(3) . . ?
C34 N20 N19 106.4(3) . . ?
N22 N21 B4 122.2(3) . . ?
C35 N21 N22 109.3(3) . . ?
C35 N21 B4 128.4(3) . . ?
N21 N22 Y2 121.3(2) . . ?
C37 N22 Y2 130.0(2) . . ?
C37 N22 N21 106.2(3) . . ?
N24 N23 B4 120.3(3) . . ?
C38 N23 N24 110.0(3) . . ?
C38 N23 B4 129.3(3) . . ?
N23 N24 Y2 125.1(2) . . ?
C40 N24 Y2 128.6(2) . . ?
C40 N24 N23 106.0(3) . . ?
N1 C5 H5 125.4 . . ?
C6 C5 N1 109.2(3) . . ?
C6 C5 H5 125.4 . . ?
C5 C6 H6 127.6 . . ?
C5 C6 C7 104.8(3) . . ?
C7 C6 H6 127.6 . . ?
N2 C7 C6 111.0(3) . . ?
N2 C7 H7 124.5 . . ?
C6 C7 H7 124.5 . . ?
N3 C8 H8 125.7 . . ?
N3 C8 C9 108.7(3) . . ?
C9 C8 H8 125.7 . . ?
C8 C9 H9 127.8 . . ?
C8 C9 C10 104.5(3) . . ?
C10 C9 H9 127.8 . . ?
N4 C10 C9 111.5(3) . . ?
N4 C10 H10 124.2 . . ?
C9 C10 H10 124.2 . . ?
N5 C11 H11 125.6 . . ?
N5 C11 C12 108.8(3) . . ?
C12 C11 H11 125.6 . . ?
C11 C12 H12 127.6 . . ?
C11 C12 C13 104.9(3) . . ?
C13 C12 H12 127.6 . . ?
N6 C13 C12 110.7(3) . . ?
N6 C13 H13 124.7 . . ?
C12 C13 H13 124.7 . . ?
N7 C14 H14 125.3 . . ?
N7 C14 C15 109.4(3) . . ?
C15 C14 H14 125.3 . . ?
C14 C15 H15 127.7 . . ?
C14 C15 C16 104.5(3) . . ?
C16 C15 H15 127.7 . . ?
N8 C16 C15 111.3(3) . . ?
N8 C16 H16 124.4 . . ?
C15 C16 H16 124.4 . . ?
N9 C17 H17 125.7 . . ?
N9 C17 C18 108.5(3) . . ?
C18 C17 H17 125.7 . . ?
C17 C18 H18 127.6 . . ?
C17 C18 C19 104.8(3) . . ?
C19 C18 H18 127.6 . . ?
N10 C19 C18 111.2(3) . . ?
N10 C19 H19 124.4 . . ?
C18 C19 H19 124.4 . . ?
N11 C20 H20 125.6 . . ?
N11 C20 C21 108.8(3) . . ?
C21 C20 H20 125.6 . . ?
C20 C21 H21 127.7 . . ?
C20 C21 C22 104.6(3) . . ?
C22 C21 H21 127.7 . . ?
N12 C22 C21 111.0(3) . . ?
N12 C22 H22 124.5 . . ?
C21 C22 H22 124.5 . . ?
N13 C23 H23 125.6 . . ?
N13 C23 C24 108.8(3) . . ?
C24 C23 H23 125.6 . . ?
C23 C24 H24 127.9 . . ?
C23 C24 C25 104.1(3) . . ?
C25 C24 H24 127.9 . . ?
N14 C25 C24 111.8(3) . . ?
N14 C25 H25 124.1 . . ?
C24 C25 H25 124.1 . . ?
N15 C26 H26 125.4 . . ?
N15 C26 C27 109.2(4) . . ?
C27 C26 H26 125.4 . . ?
C26 C27 H27 127.7 . . ?
C26 C27 C28 104.7(3) . . ?
C28 C27 H27 127.7 . . ?
N16 C28 C27 110.6(3) . . ?
N16 C28 H28 124.7 . . ?
C27 C28 H28 124.7 . . ?
N17 C29 H29 125.7 . . ?
N17 C29 C30 108.6(4) . . ?
C30 C29 H29 125.7 . . ?
C29 C30 H30 127.8 . . ?
C29 C30 C31 104.5(4) . . ?
C31 C30 H30 127.8 . . ?
N18 C31 C30 110.9(4) . . ?
N18 C31 H31 124.5 . . ?
C30 C31 H31 124.5 . . ?
N19 C32 H32 125.8 . . ?
N19 C32 C33 108.3(4) . . ?
C33 C32 H32 125.8 . . ?
C32 C33 H33 127.4 . . ?
C32 C33 C34 105.2(4) . . ?
C34 C33 H33 127.4 . . ?
N20 C34 C33 110.5(4) . . ?
N20 C34 H34 124.7 . . ?
C33 C34 H34 124.7 . . ?
N21 C35 H35 125.3 . . ?
N21 C35 C36 109.4(3) . . ?
C36 C35 H35 125.3 . . ?
C35 C36 H36 127.8 . . ?
C35 C36 C37 104.4(3) . . ?
C37 C36 H36 127.8 . . ?
N22 C37 C36 110.7(3) . . ?
N22 C37 H37 124.7 . . ?
C36 C37 H37 124.7 . . ?
N23 C38 H38 125.6 . . ?
N23 C38 C39 108.7(3) . . ?
C39 C38 H38 125.6 . . ?
C38 C39 H39 127.5 . . ?
C38 C39 C40 105.1(4) . . ?
C40 C39 H39 127.5 . . ?
N24 C40 C39 110.2(3) . . ?
N24 C40 H40 124.9 . . ?
C39 C40 H40 124.9 . . ?
O1 C41 C42 115.4(3) . . ?
O1 C41 C43 122.5(3) . . ?
C43 C41 C42 122.0(3) . . ?
O2 C42 C41 115.4(3) . . ?
O2 C42 C44 124.3(3) . . ?
C44 C42 C41 120.3(3) . . ?
C41 C43 C47 120.0(3) . . ?
C45 C43 C41 117.3(3) . . ?
C45 C43 C47 122.5(3) . . ?
C42 C44 C48 121.8(3) . . ?
C46 C44 C42 117.6(3) . . ?
C46 C44 C48 120.5(3) . . ?
O3 C45 C43 124.2(3) . . ?
O3 C45 C46 115.1(3) . . ?
C43 C45 C46 120.7(3) . . ?
O4 C46 C44 123.0(3) . . ?
O4 C46 C45 115.2(3) . . ?
C44 C46 C45 121.7(3) . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N1 B1 N3 110.1(2) . . ?
N1 B1 N5 109.8(3) . . ?
N1 B1 H1 109.7 . . ?
N3 B1 H1 109.7 . . ?
N5 B1 N3 107.8(2) . . ?
N5 B1 H1 109.7 . . ?
N7 B2 N9 108.9(3) . . ?
N7 B2 N11 110.7(3) . . ?
N7 B2 H2 109.3 . . ?
N9 B2 N11 109.2(3) . . ?
N9 B2 H2 109.3 . . ?
N11 B2 H2 109.3 . . ?
N13 B3 N17 110.2(3) . . ?
N13 B3 H3 109.6 . . ?
N15 B3 N13 107.8(3) . . ?
N15 B3 N17 109.9(3) . . ?
N15 B3 H3 109.6 . . ?
N17 B3 H3 109.6 . . ?
N19 B4 N23 108.7(3) . . ?
N19 B4 H4 109.6 . . ?
N21 B4 N19 108.8(3) . . ?
N21 B4 N23 110.6(3) . . ?
N21 B4 H4 109.6 . . ?
N23 B4 H4 109.6 . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 43.2 4.0 ?
2 0.000 0.000 0.500 12.3 0.0 ?
3 0.167 0.333 -0.604 671.3 85.4 ?
4 0.000 0.500 -0.398 671.3 85.4 ?
5 -0.167 0.667 -0.930 671.3 85.4 ?
6 0.167 0.833 -0.741 671.3 85.4 ?
7 0.333 0.167 -0.608 671.3 85.4 ?
8 0.333 0.667 0.667 43.2 4.0 ?
9 0.333 0.667 0.167 12.3 0.0 ?
10 0.500 0.000 -0.938 671.3 85.4 ?
11 0.500 0.500 -0.075 671.3 85.4 ?
12 0.667 0.833 -0.942 671.3 85.4 ?
13 0.667 0.333 0.333 43.2 4.0 ?
14 0.667 0.333 0.833 12.3 0.0 ?
15 0.833 0.167 -0.408 671.3 85.4 ?
_shelx_res_file
;
TITL 3-Y-1,2CH2Cl2_a.res in R-3
3-ydcm.res
created by SHELXL-2016/6 at 17:18:44 on 19-Jun-2017
REM Old TITL 3-Y-1,2CH2Cl2 in R-3 #148
REM SHELXT solution in R-3
REM R1 0.110, Rweak 0.016, Alpha 0.059, Orientation as input
REM Formula found by SHELXT: C61 N11 O4 Y2
CELL 0.71073 49.2258 49.2258 13.22 90 90 120
ZERR 18 0.007 0.007 0.0026 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SFAC C H B N O Y
UNIT 792 828 72 432 72 36
L.S. 4
PLAN 10
TEMP -173(2)
BOND $H
LIST 6
fmap 2
acta 52
ABIN
REM
REM
REM
WGHT 0.077400 15.647800
FVAR 0.08526
Y1 6 0.369814 0.557159 0.392070 11.00000 0.02592 0.03020 =
0.02731 0.00142 -0.00014 0.01484
Y2 6 0.563315 0.642413 0.528786 11.00000 0.02661 0.03421 =
0.03791 -0.00167 -0.00137 0.01570
O1 5 0.418900 0.571824 0.330266 11.00000 0.03008 0.03740 =
0.02993 0.00107 -0.00039 0.01898
O2 5 0.406253 0.571132 0.522807 11.00000 0.02530 0.03512 =
0.03062 0.00180 0.00139 0.01544
O3 5 0.526107 0.619741 0.402719 11.00000 0.02493 0.04702 =
0.03726 -0.00259 0.00222 0.01619
O4 5 0.513575 0.616731 0.595631 11.00000 0.02958 0.03909 =
0.03590 -0.00158 -0.00397 0.01727
N1 4 0.336934 0.593412 0.520503 11.00000 0.03240 0.04557 =
0.02489 -0.00256 -0.00234 0.02477
N2 4 0.344889 0.570569 0.528505 11.00000 0.03237 0.04289 =
0.02950 0.00105 0.00009 0.02198
N3 4 0.384336 0.633171 0.421810 11.00000 0.03315 0.03332 =
0.02901 -0.00121 -0.00374 0.01937
N4 4 0.399257 0.617076 0.393930 11.00000 0.02846 0.03404 =
0.03181 0.00089 -0.00031 0.01885
N5 4 0.333757 0.599297 0.332023 11.00000 0.02973 0.03934 =
0.02742 0.00085 -0.00153 0.02079
N6 4 0.338621 0.575782 0.297780 11.00000 0.03029 0.03305 =
0.02842 0.00008 -0.00020 0.01609
N7 4 0.353247 0.480925 0.387647 11.00000 0.04219 0.03168 =
0.04138 0.00412 0.00235 0.01808
N8 4 0.369135 0.508197 0.442680 11.00000 0.03850 0.03435 =
0.04023 0.00145 -0.00056 0.02060
N9 4 0.304937 0.483866 0.351651 11.00000 0.03651 0.03687 =
0.03252 0.00321 0.00192 0.01174
N10 4 0.313778 0.512988 0.390262 11.00000 0.03486 0.03693 =
0.03247 0.00265 0.00181 0.01702
N11 4 0.345494 0.498441 0.215631 11.00000 0.04190 0.03229 =
0.03506 -0.00159 0.00364 0.01651
N12 4 0.363353 0.530134 0.229393 11.00000 0.03072 0.03123 =
0.03384 0.00033 0.00279 0.01287
N13 4 0.562945 0.712163 0.499142 11.00000 0.03571 0.03638 =
0.04571 0.00030 -0.00408 0.01903
N14 4 0.544076 0.681604 0.526967 11.00000 0.03238 0.03913 =
0.04015 -0.00151 -0.00230 0.01829
N15 4 0.615670 0.721083 0.548902 11.00000 0.03366 0.03198 =
0.05473 -0.00201 -0.00637 0.01263
N16 4 0.605110 0.693158 0.598310 11.00000 0.03358 0.03691 =
0.04829 -0.00624 -0.00799 0.01843
N17 4 0.596916 0.705209 0.368830 11.00000 0.03197 0.04522 =
0.04821 0.00673 0.00224 0.01660
N18 4 0.587416 0.674073 0.376353 11.00000 0.03378 0.04101 =
0.04568 0.00007 0.00309 0.01808
N19 4 0.568652 0.576408 0.570852 11.00000 0.04153 0.03488 =
0.06022 0.00346 0.00460 0.02062
N20 4 0.552612 0.587044 0.514557 11.00000 0.02887 0.04346 =
0.05282 -0.00389 0.00146 0.01816
N21 4 0.621090 0.625026 0.582141 11.00000 0.03266 0.04427 =
0.05268 -0.00140 -0.00225 0.02145
N22 4 0.614585 0.642951 0.518888 11.00000 0.03478 0.03561 =
0.05039 -0.00073 -0.00125 0.01764
N23 4 0.582212 0.609966 0.726587 11.00000 0.03843 0.04390 =
0.04808 0.00359 -0.00155 0.02428
N24 4 0.568269 0.627028 0.701286 11.00000 0.03222 0.04034 =
0.04570 -0.00026 -0.00334 0.02067
C5 1 0.317930 0.590617 0.599564 11.00000 0.03658 0.05184 =
0.02904 -0.00571 -0.00037 0.02542
AFIX 43
H5 2 0.309341 0.603825 0.611782 11.00000 -1.20000
AFIX 0
C6 1 0.313207 0.565906 0.658243 11.00000 0.03864 0.06100 =
0.02578 -0.00061 0.00398 0.02322
AFIX 43
H6 2 0.300768 0.558346 0.717656 11.00000 -1.20000
AFIX 0
C7 1 0.330585 0.554164 0.612130 11.00000 0.03773 0.04354 =
0.02866 0.00548 0.00217 0.01814
AFIX 43
H7 2 0.332132 0.536836 0.636548 11.00000 -1.20000
AFIX 0
C8 1 0.405272 0.664102 0.428883 11.00000 0.04433 0.03310 =
0.03166 0.00014 -0.00510 0.02217
AFIX 43
H8 2 0.400563 0.679978 0.446934 11.00000 -1.20000
AFIX 0
C9 1 0.434656 0.668855 0.405552 11.00000 0.03635 0.03407 =
0.03594 0.00396 -0.00246 0.01310
AFIX 43
H9 2 0.453943 0.688158 0.404208 11.00000 -1.20000
AFIX 0
C10 1 0.429685 0.639026 0.384444 11.00000 0.02992 0.03368 =
0.03453 0.00523 0.00078 0.01454
AFIX 43
H10 2 0.445771 0.634700 0.365675 11.00000 -1.20000
AFIX 0
C11 1 0.314948 0.603306 0.266514 11.00000 0.03192 0.05779 =
0.02824 0.00574 0.00102 0.02938
AFIX 43
H11 2 0.308298 0.618315 0.273116 11.00000 -1.20000
AFIX 0
C12 1 0.307023 0.582087 0.188749 11.00000 0.03177 0.05391 =
0.02734 0.00213 -0.00193 0.02307
AFIX 43
H12 2 0.294049 0.579434 0.132093 11.00000 -1.20000
AFIX 0
C13 1 0.322197 0.565334 0.211288 11.00000 0.03188 0.03944 =
0.02572 0.00165 -0.00132 0.01498
AFIX 43
H13 2 0.321093 0.548812 0.171102 11.00000 -1.20000
AFIX 0
C14 1 0.360923 0.459842 0.423409 11.00000 0.05832 0.03388 =
0.05630 0.00893 0.00615 0.02590
AFIX 43
H14 2 0.353278 0.439264 0.397646 11.00000 -1.20000
AFIX 0
C15 1 0.381400 0.472818 0.502411 11.00000 0.05823 0.04720 =
0.05101 0.01342 0.00637 0.03522
AFIX 43
H15 2 0.390509 0.463369 0.542189 11.00000 -1.20000
AFIX 0
C16 1 0.385900 0.502962 0.511455 11.00000 0.04628 0.04386 =
0.04043 0.00766 0.00261 0.02826
AFIX 43
H16 2 0.399174 0.517893 0.560218 11.00000 -1.20000
AFIX 0
C17 1 0.273394 0.466609 0.348222 11.00000 0.03388 0.04938 =
0.03456 0.00461 0.00075 0.00610
AFIX 43
H17 2 0.261545 0.445652 0.324335 11.00000 -1.20000
AFIX 0
C18 1 0.261189 0.484511 0.385268 11.00000 0.03104 0.06348 =
0.03066 0.00755 0.00166 0.01517
AFIX 43
H18 2 0.239712 0.478585 0.392064 11.00000 -1.20000
AFIX 0
C19 1 0.287103 0.512952 0.410286 11.00000 0.02954 0.04968 =
0.03270 0.00786 0.00361 0.01643
AFIX 43
H19 2 0.286110 0.530231 0.438084 11.00000 -1.20000
AFIX 0
C20 1 0.346340 0.491341 0.117384 11.00000 0.04618 0.04155 =
0.03800 -0.00740 0.00170 0.02316
AFIX 43
H20 2 0.335862 0.470853 0.089132 11.00000 -1.20000
AFIX 0
C21 1 0.364875 0.518665 0.064925 11.00000 0.05317 0.04809 =
0.03448 -0.00243 0.00529 0.02940
AFIX 43
H21 2 0.369683 0.520953 -0.005241 11.00000 -1.20000
AFIX 0
C22 1 0.375011 0.542225 0.137794 11.00000 0.03588 0.03763 =
0.03435 0.00463 0.00710 0.01562
AFIX 43
H22 2 0.388374 0.563932 0.124510 11.00000 -1.20000
AFIX 0
C23 1 0.548780 0.728863 0.518684 11.00000 0.04355 0.03785 =
0.04732 -0.00601 -0.00999 0.02551
AFIX 43
H23 2 0.557459 0.750681 0.506652 11.00000 -1.20000
AFIX 0
C24 1 0.519630 0.709176 0.558998 11.00000 0.04628 0.04972 =
0.04134 -0.00509 -0.00097 0.03166
AFIX 43
H24 2 0.504236 0.714268 0.579772 11.00000 -1.20000
AFIX 0
C25 1 0.517876 0.680147 0.562353 11.00000 0.03942 0.04290 =
0.03944 -0.00405 0.00118 0.02534
AFIX 43
H25 2 0.500243 0.661519 0.586769 11.00000 -1.20000
AFIX 0
C26 1 0.642961 0.742802 0.589133 11.00000 0.03793 0.04169 =
0.07007 -0.00742 -0.01172 0.01535
AFIX 43
H26 2 0.654833 0.764027 0.567747 11.00000 -1.20000
AFIX 0
C27 1 0.651005 0.729571 0.665823 11.00000 0.03809 0.05112 =
0.06708 -0.01590 -0.01858 0.02210
AFIX 43
H27 2 0.669104 0.739390 0.707649 11.00000 -1.20000
AFIX 0
C28 1 0.626743 0.698441 0.669076 11.00000 0.03890 0.04582 =
0.05300 -0.01132 -0.01332 0.02426
AFIX 43
H28 2 0.625686 0.683106 0.715040 11.00000 -1.20000
AFIX 0
C29 1 0.605475 0.715104 0.272729 11.00000 0.03899 0.06130 =
0.05440 0.01919 0.01070 0.02374
AFIX 43
H29 2 0.612802 0.735818 0.248757 11.00000 -1.20000
AFIX 0
C30 1 0.601804 0.690135 0.215253 11.00000 0.04409 0.07189 =
0.04711 0.00858 0.00876 0.02830
AFIX 43
H30 2 0.605980 0.689987 0.145158 11.00000 -1.20000
AFIX 0
C31 1 0.590540 0.665043 0.283337 11.00000 0.03803 0.06012 =
0.04679 -0.00033 0.00641 0.02474
AFIX 43
H31 2 0.585745 0.644381 0.266035 11.00000 -1.20000
AFIX 0
C32 1 0.558188 0.545814 0.548615 11.00000 0.05331 0.03562 =
0.07732 0.00191 0.01242 0.02393
AFIX 43
H32 2 0.565650 0.533110 0.577600 11.00000 -1.20000
AFIX 0
C33 1 0.534971 0.536382 0.477045 11.00000 0.04786 0.03784 =
0.07680 -0.01033 0.00735 0.01421
AFIX 43
H33 2 0.523328 0.516236 0.446891 11.00000 -1.20000
AFIX 0
C34 1 0.532168 0.562768 0.458162 11.00000 0.03608 0.04317 =
0.06713 -0.01402 0.00044 0.01638
AFIX 43
H34 2 0.517767 0.563420 0.411771 11.00000 -1.20000
AFIX 0
C35 1 0.652158 0.635540 0.580617 11.00000 0.03209 0.05324 =
0.06242 -0.00715 -0.00560 0.02535
AFIX 43
H35 2 0.662471 0.626908 0.618327 11.00000 -1.20000
AFIX 0
C36 1 0.666566 0.660648 0.516125 11.00000 0.02758 0.05032 =
0.06333 -0.00997 -0.00179 0.01669
AFIX 43
H36 2 0.688264 0.672711 0.500384 11.00000 -1.20000
AFIX 0
C37 1 0.642198 0.664478 0.478878 11.00000 0.03346 0.04169 =
0.05637 -0.00120 0.00522 0.01710
AFIX 43
H37 2 0.644741 0.680141 0.431709 11.00000 -1.20000
AFIX 0
C38 1 0.578609 0.603402 0.825567 11.00000 0.05114 0.05154 =
0.04934 0.00867 -0.00329 0.02810
AFIX 43
H38 2 0.586247 0.591785 0.860969 11.00000 -1.20000
AFIX 0
C39 1 0.562146 0.616156 0.867275 11.00000 0.05107 0.05966 =
0.04770 0.00725 0.00416 0.03026
AFIX 43
H39 2 0.556203 0.615336 0.936068 11.00000 -1.20000
AFIX 0
C40 1 0.555937 0.630652 0.787045 11.00000 0.04277 0.05136 =
0.04319 -0.00175 -0.00466 0.02744
AFIX 43
H40 2 0.544595 0.641530 0.792452 11.00000 -1.20000
AFIX 0
C41 1 0.442305 0.581695 0.389250 11.00000 0.03354 0.03530 =
0.02816 0.00179 -0.00039 0.02055
C42 1 0.435027 0.581643 0.501504 11.00000 0.03127 0.03129 =
0.03095 0.00367 0.00210 0.01812
C43 1 0.472906 0.593237 0.353855 11.00000 0.03176 0.03963 =
0.03155 -0.00133 0.00284 0.02006
C44 1 0.459160 0.592841 0.573165 11.00000 0.02959 0.03761 =
0.02787 0.00079 -0.00160 0.01744
C45 1 0.497036 0.606258 0.424803 11.00000 0.02965 0.03709 =
0.03349 -0.00037 0.00131 0.01785
C46 1 0.489780 0.605023 0.537665 11.00000 0.03150 0.03393 =
0.03128 0.00012 -0.00005 0.01747
C47 1 0.478990 0.593717 0.241891 11.00000 0.03150 0.05634 =
0.03202 -0.00335 0.00344 0.01788
AFIX 137
H47A 2 0.466636 0.572445 0.214526 11.00000 -1.50000
H47B 2 0.501345 0.601421 0.230449 11.00000 -1.50000
H47C 2 0.472941 0.607597 0.207937 11.00000 -1.50000
AFIX 0
C48 1 0.452825 0.592847 0.684609 11.00000 0.03326 0.04638 =
0.02966 0.00016 -0.00034 0.01820
AFIX 137
H48A 2 0.432820 0.592300 0.694308 11.00000 -1.50000
H48B 2 0.469746 0.611887 0.715692 11.00000 -1.50000
H48C 2 0.451787 0.574360 0.716349 11.00000 -1.50000
AFIX 0
B1 3 0.348226 0.616853 0.431815 11.00000 0.03547 0.04245 =
0.02882 -0.00194 -0.00389 0.02607
AFIX 13
H1 2 0.341837 0.632950 0.443558 11.00000 -1.20000
AFIX 0
B2 3 0.329272 0.476450 0.305976 11.00000 0.04363 0.02968 =
0.03735 0.00214 0.00154 0.01263
AFIX 13
H2 2 0.318421 0.454192 0.282124 11.00000 -1.20000
AFIX 0
B3 3 0.596870 0.724496 0.461461 11.00000 0.03805 0.03589 =
0.05288 0.00291 -0.00313 0.01719
AFIX 13
H3 2 0.606482 0.747099 0.442239 11.00000 -1.20000
AFIX 0
B4 3 0.595483 0.597656 0.642928 11.00000 0.04163 0.04529 =
0.05448 -0.00041 -0.00569 0.02521
AFIX 13
H4 2 0.604385 0.585350 0.674624 11.00000 -1.20000
AFIX 0
HKLF 4
REM 3-Y-1,2CH2Cl2_a.res in R-3
REM R1 = 0.0576 for 11662 Fo > 4sig(Fo) and 0.1118 for all 19276 data
REM 705 parameters refined using 0 restraints
END
WGHT 0.0774 15.6937
REM Highest difference peak 0.433, deepest hole -1.667, 1-sigma level 0.104
Q1 1 0.3803 0.5635 0.4863 11.00000 0.05 0.43
Q2 1 0.4005 0.5691 0.3845 11.00000 0.05 0.43
Q3 1 0.3717 0.5500 0.3638 11.00000 0.05 0.42
Q4 1 0.3701 0.5510 0.2968 11.00000 0.05 0.42
Q5 1 0.5595 0.6365 0.6260 11.00000 0.05 0.41
Q6 1 0.3383 0.4351 0.3744 11.00000 0.05 0.41
Q7 1 0.5881 0.6391 0.5353 11.00000 0.05 0.40
Q8 1 0.3839 0.5393 0.3976 11.00000 0.05 0.40
Q9 1 0.5358 0.6319 0.4828 11.00000 0.05 0.39
Q10 1 0.3404 0.5383 0.3957 11.00000 0.05 0.39
;
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58 5 -1 2.4328 0.0000
58 6 -2 9.1944 0.0000
58 6 1 -11.2086 0.0000
58 7 0 2.7951 0.0000
58 8 -1 20.1196 0.0000
59 1 -5 22.1895 0.0000
59 1 -2 4.4452 0.0000
59 1 1 8.4304 0.0000
59 2 -3 -13.6959 0.0000
59 2 0 11.8757 0.0000
59 3 -4 -11.7123 0.0000
59 3 -1 -24.2715 0.0000
59 4 -5 10.6545 0.0000
59 4 -2 -10.3983 0.0000
59 5 0 -1.3004 0.0000
59 6 -1 6.3126 0.0000
60 1 -4 -12.2305 0.0000
60 1 -1 -8.2596 0.0000
60 2 -5 9.9781 0.0000
60 2 -2 7.3785 0.0000
60 3 0 -13.3760 0.0000
60 4 -1 21.4555 0.0000
61 1 -3 -8.3653 0.0000
61 2 -1 13.1681 0.0000
61 3 -2 1.9124 0.0000
62 1 -2 -3.2716 0.0000
0 0 0 0.0 0.0
;
_shelx_fab_checksum 38513
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_RINTA01_3-ydcm
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Every attempt was made to acheive a better structure
collection, however the only crystals obtained were small and poorly
diffracting, and therefore collected at the synchrotron.
;
_vrf_PLAT369_3-ydcm
;
PROBLEM: Long C(sp2)-C(sp2) Bond C41 - C42 .. 1.53 Ang.
RESPONSE: Bond has similar observed mean bond length to that of
similar bonds in -C(=O)-C(=O)- systems.
;
_vrf_PLAT905_3-ydcm
;
PROBLEM: Negative K value in the Analysis of Variance ... -2.198 Report
RESPONSE: Due to a slight overestimation of the intensities of weak reflections.
;
# end Validation Reply Form