# Electronic Supplementary Material (ESI) for Chemical Science.
# 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).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_kz86m_0m
_database_code_depnum_ccdc_archive 'CCDC 1533271'
_audit_update_record
;
2017-02-17 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;
_audit_creation_date 2017-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number 2016/4
# start Validation Reply Form
_vrf_PLAT701_kz86m_0m
;
PROBLEM: Bond Calc 1.577(18), Rep 1.434(10), Dev.. 7.94 Sigma
RESPONSE: This is the result of disorder in the polyether chain.
;
_vrf_PLAT702_kz86m_0m
;
PROBLEM: Angle Calc 81.7(12), Rep 113.0(9), Dev.. 26.08 Sigma
RESPONSE: This is the result of disorder in the polyether chain.
;
# end Validation Reply Form
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C34 H50 O10, C25 H18 N2, 2(C H4 O)'
_chemical_formula_sum 'C61 H76 N2 O12'
_chemical_formula_weight 1029.23
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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 12.9848(10)
_cell_length_b 19.3820(15)
_cell_length_c 22.2953(17)
_cell_angle_alpha 90
_cell_angle_beta 99.8421(10)
_cell_angle_gamma 90
_cell_volume 5528.5(7)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9906
_cell_measurement_temperature 273(2)
_cell_measurement_theta_max 26.11
_cell_measurement_theta_min 2.24
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.085
_exptl_absorpt_correction_T_max 0.7359
_exptl_absorpt_correction_T_min 0.5429
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1057 before and 0.0908 after correction.
The Ratio of minimum to maximum transmission is 0.7377.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.237
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2208
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0882
_diffrn_reflns_av_unetI/netI 0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 51517
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.027
_diffrn_reflns_theta_max 25.027
_diffrn_reflns_theta_min 1.998
_diffrn_ambient_temperature 273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6800
_reflns_number_total 9760
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max 0.714
_refine_diff_density_min -0.295
_refine_diff_density_rms 0.048
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 717
_refine_ls_number_reflns 9760
_refine_ls_number_restraints 7
_refine_ls_R_factor_all 0.0890
_refine_ls_R_factor_gt 0.0561
_refine_ls_restrained_S_all 1.025
_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^)+(0.0597P)^2^+2.4887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1310
_refine_ls_wR_factor_ref 0.1490
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2. Same fragment restrains
{O7, O8A, C55A, C56A, C54A, C57} sigma for 1-2: 0.02, 1-3: 0.02
as
{O7, O8, C55, C56, C54, O8A}
3. Others
Sof(O8A)=Sof(C55A)=Sof(H55C)=Sof(H55D)=Sof(C56A)=Sof(H56C)=Sof(H56D)=
Sof(C54A)=Sof(H54C)=Sof(H54D)=Sof(H57C)=Sof(H57D)=1-FVAR(1)
Sof(O8)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C54)=
Sof(H54A)=Sof(H54B)=Sof(H57A)=Sof(H57B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
C39(H39A,H39B), C53(H53A,H53B), C48(H48A,H48B), C59(H59A,H59B), C52(H52A,
H52B), C41(H41A,H41B), C47(H47A,H47B), C46(H46A,H46B), C42(H42A,H42B),
C51(H51A,H51B), C38(H38A,H38B), C40(H40A,H40B), C50(H50A,H50B), C58(H58A,H58B),
C49(H49A,H49B), C45(H45A,H45B), C43(H43A,H43B), C44(H44A,H44B), C55(H55A,
H55B), C56(H56A,H56B), C54(H54A,H54B), C55A(H55C,H55D), C56A(H56C,H56D),
C54A(H54C,H54D), C57(H57A,H57B), C57(H57C,H57D)
4.b Aromatic/amide H refined with riding coordinates:
C35(H35), C33(H33), C37(H37), C29(H29), C27(H27), C31(H31), C15(H15),
C25(H25), C22(H22), C7(H7), C19(H19), C10(H10), C24(H24), C11(H11), C3(H3),
C23(H23), C16(H16), C21(H21), C18(H18), C4(H4), C17(H17), C5(H5), C6(H6),
N1(H1)
4.c Idealised Me refined as rotating group:
C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
4.d Idealised tetrahedral OH refined as rotating group:
O1S(H1S), O2S(H2S)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_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
C35 C 0.64723(19) 0.93630(12) 0.09422(11) 0.0287(6) Uani 1 1 d . . . . .
H35 H 0.643152 0.953650 0.132639 0.034 Uiso 1 1 calc R . . . .
C36 C 0.74277(19) 0.91936(12) 0.07910(11) 0.0289(6) Uani 1 1 d . . . . .
C28 C 0.49660(19) 0.62169(13) 0.19198(11) 0.0315(6) Uani 1 1 d . . . . .
C34 C 0.55679(19) 0.92709(12) 0.05117(11) 0.0290(6) Uani 1 1 d . . . . .
C33 C 0.56210(19) 0.90235(12) -0.00645(11) 0.0298(6) Uani 1 1 d . . . . .
H33 H 0.501325 0.895815 -0.034675 0.036 Uiso 1 1 calc R . . . .
C37 C 0.7493(2) 0.89573(12) 0.02067(11) 0.0314(6) Uani 1 1 d . . . . .
H37 H 0.814103 0.885668 0.010346 0.038 Uiso 1 1 calc R . . . .
C29 C 0.58203(19) 0.63519(12) 0.23623(11) 0.0322(6) Uani 1 1 d . . . . .
H29 H 0.576725 0.665741 0.267721 0.039 Uiso 1 1 calc R . . . .
C27 C 0.5051(2) 0.57504(13) 0.14547(11) 0.0346(6) Uani 1 1 d . . . . .
H27 H 0.447375 0.566306 0.115515 0.042 Uiso 1 1 calc R . . . .
C39 C 0.6933(2) 0.44093(13) 0.02253(12) 0.0370(6) Uani 1 1 d . . . . .
H39A H 0.628123 0.441350 -0.006205 0.044 Uiso 1 1 calc R . . . .
H39B H 0.701060 0.395864 0.041688 0.044 Uiso 1 1 calc R . . . .
C32 C 0.65910(19) 0.88734(12) -0.02181(11) 0.0301(6) Uani 1 1 d . . . . .
C31 C 0.6852(2) 0.55565(13) 0.18775(12) 0.0379(6) Uani 1 1 d . . . . .
H31 H 0.748549 0.533683 0.186784 0.045 Uiso 1 1 calc R . . . .
C53 C 0.36902(18) 0.92559(13) 0.03314(12) 0.0330(6) Uani 1 1 d . . . . .
H53A H 0.372889 0.878953 0.017901 0.040 Uiso 1 1 calc R . . . .
H53B H 0.355261 0.956733 -0.001358 0.040 Uiso 1 1 calc R . . . .
C26 C 0.5984(2) 0.54167(13) 0.14353(12) 0.0347(6) Uani 1 1 d . . . . .
C48 C 0.3847(2) 0.69273(14) 0.24123(11) 0.0366(6) Uani 1 1 d . . . . .
H48A H 0.428576 0.733531 0.244302 0.044 Uiso 1 1 calc R . . . .
H48B H 0.402762 0.666308 0.278495 0.044 Uiso 1 1 calc R . . . .
C59 C 0.8323(2) 0.94028(15) 0.18059(12) 0.0389(6) Uani 1 1 d . . . . .
H59A H 0.784622 0.909731 0.196768 0.047 Uiso 1 1 calc R . . . .
H59B H 0.807513 0.987254 0.182875 0.047 Uiso 1 1 calc R . . . .
C52 C 0.28389(19) 0.93068(13) 0.07000(12) 0.0360(6) Uani 1 1 d . . . . .
H52A H 0.283574 0.976382 0.087701 0.043 Uiso 1 1 calc R . . . .
H52B H 0.216729 0.923064 0.044238 0.043 Uiso 1 1 calc R . . . .
C41 C 0.7748(2) 0.52220(14) -0.04423(13) 0.0451(7) Uani 1 1 d . . . . .
H41A H 0.709249 0.522433 -0.072652 0.054 Uiso 1 1 calc R . . . .
H41B H 0.770950 0.558642 -0.014870 0.054 Uiso 1 1 calc R . . . .
C47 C 0.6625(2) 0.86402(14) -0.08645(12) 0.0377(6) Uani 1 1 d . . . . .
H47A H 0.607577 0.830327 -0.098326 0.045 Uiso 1 1 calc R . . . .
H47B H 0.647809 0.903371 -0.113439 0.045 Uiso 1 1 calc R . . . .
C30 C 0.6759(2) 0.60262(13) 0.23316(12) 0.0355(6) Uani 1 1 d . . . . .
C46 C 0.7719(2) 0.76447(13) -0.07547(13) 0.0373(6) Uani 1 1 d . . . . .
H46A H 0.721732 0.735652 -0.101358 0.045 Uiso 1 1 calc R . . . .
H46B H 0.759444 0.760196 -0.033958 0.045 Uiso 1 1 calc R . . . .
C42 C 0.8615(2) 0.53980(15) -0.07905(13) 0.0468(7) Uani 1 1 d . . . . .
H42A H 0.860146 0.507331 -0.112278 0.056 Uiso 1 1 calc R . . . .
H42B H 0.928281 0.535058 -0.052225 0.056 Uiso 1 1 calc R . . . .
C51 C 0.2166(2) 0.87673(14) 0.14985(14) 0.0419(7) Uani 1 1 d . . . . .
H51A H 0.154532 0.859980 0.123335 0.050 Uiso 1 1 calc R . . . .
H51B H 0.201772 0.922570 0.163618 0.050 Uiso 1 1 calc R . . . .
C38 C 0.6021(2) 0.48635(14) 0.09626(13) 0.0421(7) Uani 1 1 d . . . . .
H38A H 0.603108 0.441413 0.115506 0.051 Uiso 1 1 calc R . . . .
H38B H 0.539394 0.489123 0.065673 0.051 Uiso 1 1 calc R . . . .
C40 C 0.7835(2) 0.45408(13) -0.01070(13) 0.0426(7) Uani 1 1 d . . . . .
H40A H 0.786632 0.417065 -0.039618 0.051 Uiso 1 1 calc R . . . .
H40B H 0.848207 0.453431 0.018412 0.051 Uiso 1 1 calc R . . . .
C50 C 0.2425(2) 0.82996(14) 0.20327(12) 0.0394(7) Uani 1 1 d . . . . .
H50A H 0.309938 0.842495 0.226611 0.047 Uiso 1 1 calc R . . . .
H50B H 0.190402 0.834774 0.229415 0.047 Uiso 1 1 calc R . . . .
C58 C 0.9402(2) 0.93353(15) 0.21717(13) 0.0455(7) Uani 1 1 d . . . . .
H58A H 0.988054 0.960328 0.197490 0.055 Uiso 1 1 calc R . . . .
H58B H 0.940290 0.953507 0.257070 0.055 Uiso 1 1 calc R . . . .
C49 C 0.2717(2) 0.71297(15) 0.23182(12) 0.0396(7) Uani 1 1 d . . . . .
H49A H 0.228898 0.671986 0.223088 0.048 Uiso 1 1 calc R . . . .
H49B H 0.256195 0.733162 0.269077 0.048 Uiso 1 1 calc R . . . .
C45 C 0.8808(2) 0.74147(14) -0.07917(14) 0.0436(7) Uani 1 1 d . . . . .
H45A H 0.929995 0.771024 -0.053414 0.052 Uiso 1 1 calc R . . . .
H45B H 0.892560 0.746988 -0.120710 0.052 Uiso 1 1 calc R . . . .
C43 C 0.8515(2) 0.61346(14) -0.10481(13) 0.0461(7) Uani 1 1 d . . . . .
H43A H 0.883606 0.615370 -0.141000 0.055 Uiso 1 1 calc R . . . .
H43B H 0.778043 0.624613 -0.116742 0.055 Uiso 1 1 calc R . . . .
C44 C 0.9022(2) 0.66678(15) -0.05985(13) 0.0449(7) Uani 1 1 d . . . . .
H44A H 0.977131 0.659324 -0.052783 0.054 Uiso 1 1 calc R . . . .
H44B H 0.878106 0.659515 -0.021468 0.054 Uiso 1 1 calc R . . . .
O6 O 0.46560(12) 0.94363(8) 0.07132(7) 0.0314(4) Uani 1 1 d . . . . .
O5 O 0.30078(12) 0.88000(8) 0.11706(8) 0.0332(4) Uani 1 1 d . . . . .
O2 O 0.75959(14) 0.83452(9) -0.09471(8) 0.0382(4) Uani 1 1 d . . . . .
O4 O 0.24524(14) 0.76090(9) 0.18347(8) 0.0383(4) Uani 1 1 d . . . . .
O10 O 0.83590(12) 0.92262(9) 0.11861(8) 0.0339(4) Uani 1 1 d . . . . .
O1 O 0.69063(13) 0.49279(8) 0.06770(8) 0.0363(4) Uani 1 1 d . . . . .
O3 O 0.40045(13) 0.65180(9) 0.18987(8) 0.0373(4) Uani 1 1 d . . . . .
O9 O 0.97864(13) 0.86488(10) 0.22488(8) 0.0426(5) Uani 1 1 d . . . . .
O7 O 0.75424(14) 0.61955(10) 0.28073(10) 0.0550(6) Uani 1 1 d D . . . .
O8 O 0.9411(13) 0.7108(4) 0.3075(6) 0.040(2) Uani 0.575(9) 1 d D . P A 1
C55 C 0.9196(4) 0.6556(3) 0.2643(3) 0.0464(18) Uani 0.575(9) 1 d D . P A 1
H55A H 0.984873 0.637803 0.254910 0.056 Uiso 0.575(9) 1 calc R . P A 1
H55B H 0.878714 0.673081 0.226847 0.056 Uiso 0.575(9) 1 calc R . P A 1
C56 C 0.9935(8) 0.7670(5) 0.2854(5) 0.041(2) Uani 0.575(9) 1 d D . P A 1
H56A H 1.031181 0.750425 0.254283 0.049 Uiso 0.575(9) 1 calc R . P A 1
H56B H 1.044308 0.785446 0.318482 0.049 Uiso 0.575(9) 1 calc R . P A 1
C54 C 0.8613(5) 0.5989(3) 0.2886(3) 0.0399(18) Uani 0.575(9) 1 d D . P A 1
H54A H 0.868123 0.556433 0.266573 0.048 Uiso 0.575(9) 1 calc R . P A 1
H54B H 0.888594 0.591312 0.331322 0.048 Uiso 0.575(9) 1 calc R . P A 1
O8A O 0.9246(19) 0.7135(7) 0.3144(9) 0.048(5) Uani 0.425(9) 1 d D . P A 2
C55A C 0.9352(5) 0.6406(4) 0.3102(4) 0.045(2) Uani 0.425(9) 1 d D . P A 2
H55C H 0.924999 0.619459 0.348191 0.054 Uiso 0.425(9) 1 calc R . P A 2
H55D H 1.005367 0.629538 0.303719 0.054 Uiso 0.425(9) 1 calc R . P A 2
C56A C 0.9678(16) 0.7516(8) 0.2706(8) 0.088(6) Uani 0.425(9) 1 d D . P A 2
H56C H 0.955843 0.726524 0.232350 0.106 Uiso 0.425(9) 1 calc R . P A 2
H56D H 1.042740 0.755095 0.283817 0.106 Uiso 0.425(9) 1 calc R . P A 2
C54A C 0.8573(6) 0.6116(5) 0.2589(4) 0.041(3) Uani 0.425(9) 1 d D . P A 2
H54C H 0.871868 0.563520 0.251865 0.049 Uiso 0.425(9) 1 calc R . P A 2
H54D H 0.857710 0.637397 0.221682 0.049 Uiso 0.425(9) 1 calc R . P A 2
C57 C 0.9237(2) 0.82192(17) 0.26015(14) 0.0521(8) Uani 1 1 d D . . . .
H57A H 0.862160 0.802799 0.234835 0.063 Uiso 0.575(9) 1 calc R . P A 1
H57B H 0.901605 0.848394 0.292614 0.063 Uiso 0.575(9) 1 calc R . P A 1
H57C H 0.851686 0.818201 0.239825 0.063 Uiso 0.425(9) 1 calc R . P A 2
H57D H 0.923601 0.843765 0.299280 0.063 Uiso 0.425(9) 1 calc R . P A 2
C13 C 0.63505(17) 0.73952(11) 0.11058(10) 0.0223(5) Uani 1 1 d . . . . .
C1 C 0.58024(17) 0.80689(11) 0.17436(10) 0.0233(5) Uani 1 1 d . . . . .
C12 C 0.69590(17) 0.69773(11) 0.07866(10) 0.0243(5) Uani 1 1 d . . . . .
C14 C 0.36888(18) 0.74200(11) 0.00390(10) 0.0247(5) Uani 1 1 d . . . . .
C15 C 0.28524(18) 0.74039(12) 0.03558(11) 0.0304(6) Uani 1 1 d . . . . .
H15 H 0.296134 0.727226 0.076289 0.036 Uiso 1 1 calc R . . . .
C25 C 0.85599(19) 0.62361(12) 0.09673(11) 0.0301(6) Uani 1 1 d . . . . .
H25 H 0.813909 0.584650 0.089390 0.036 Uiso 1 1 calc R . . . .
C22 C 0.98289(19) 0.73781(14) 0.12006(11) 0.0349(6) Uani 1 1 d . . . . .
H22 H 1.025701 0.776338 0.128182 0.042 Uiso 1 1 calc R . . . .
C7 C 0.64410(19) 0.83534(13) 0.28192(11) 0.0330(6) Uani 1 1 d . . . . .
H7 H 0.687971 0.797186 0.283906 0.040 Uiso 1 1 calc R . . . .
C19 C 0.34971(19) 0.76191(12) -0.05706(11) 0.0294(6) Uani 1 1 d . . . . .
H19 H 0.404606 0.762553 -0.078931 0.035 Uiso 1 1 calc R . . . .
C9 C 0.47720(18) 0.72406(11) 0.03258(10) 0.0240(5) Uani 1 1 d . . . . .
C8 C 0.52853(17) 0.75135(11) 0.08795(10) 0.0220(5) Uani 1 1 d . . . . .
C10 C 0.53834(18) 0.68180(12) 0.00306(11) 0.0278(5) Uani 1 1 d . . . . .
H10 H 0.507952 0.661345 -0.033425 0.033 Uiso 1 1 calc R . . . .
C24 C 0.9635(2) 0.61666(13) 0.10758(12) 0.0356(6) Uani 1 1 d . . . . .
H24 H 0.993126 0.573012 0.107333 0.043 Uiso 1 1 calc R . . . .
C11 C 0.64300(19) 0.66846(12) 0.02534(11) 0.0289(6) Uani 1 1 d . . . . .
H11 H 0.679140 0.638685 0.003640 0.035 Uiso 1 1 calc R . . . .
C2 C 0.57698(17) 0.85049(12) 0.22795(10) 0.0257(5) Uani 1 1 d . . . . .
C3 C 0.51154(19) 0.90754(12) 0.22588(11) 0.0293(6) Uani 1 1 d . . . . .
H3 H 0.465867 0.918071 0.190204 0.035 Uiso 1 1 calc R . . . .
C20 C 0.81025(18) 0.68874(12) 0.09674(10) 0.0253(5) Uani 1 1 d . . . . .
C23 C 1.0271(2) 0.67361(14) 0.11872(12) 0.0369(6) Uani 1 1 d . . . . .
H23 H 1.099354 0.668654 0.125297 0.044 Uiso 1 1 calc R . . . .
C16 C 0.1860(2) 0.75833(15) 0.00659(13) 0.0410(7) Uani 1 1 d . . . . .
H16 H 0.130370 0.756561 0.027825 0.049 Uiso 1 1 calc R . . . .
C21 C 0.87575(19) 0.74587(12) 0.10951(11) 0.0299(6) Uani 1 1 d . . . . .
H21 H 0.846979 0.789661 0.110915 0.036 Uiso 1 1 calc R . . . .
C18 C 0.2512(2) 0.78064(14) -0.08553(12) 0.0398(7) Uani 1 1 d . . . . .
H18 H 0.239999 0.794457 -0.126068 0.048 Uiso 1 1 calc R . . . .
C4 C 0.5143(2) 0.94867(13) 0.27690(12) 0.0356(6) Uani 1 1 d . . . . .
H4 H 0.470344 0.986743 0.275352 0.043 Uiso 1 1 calc R . . . .
C17 C 0.1690(2) 0.77880(15) -0.05348(13) 0.0447(7) Uani 1 1 d . . . . .
H17 H 0.102235 0.791373 -0.072461 0.054 Uiso 1 1 calc R . . . .
C5 C 0.5815(2) 0.93364(14) 0.32975(12) 0.0410(7) Uani 1 1 d . . . . .
H5 H 0.583635 0.961871 0.363663 0.049 Uiso 1 1 calc R . . . .
C6 C 0.6460(2) 0.87669(15) 0.33265(12) 0.0421(7) Uani 1 1 d . . . . .
H6 H 0.690629 0.866125 0.368693 0.051 Uiso 1 1 calc R . . . .
N1 N 0.49601(14) 0.79484(9) 0.12987(8) 0.0221(4) Uani 1 1 d . . . . .
H1 H 0.434129 0.811337 0.128315 0.026 Uiso 1 1 calc R . . . .
N2 N 0.66542(14) 0.77434(9) 0.16488(8) 0.0240(4) Uani 1 1 d . . . . .
C1S C 0.9782(3) 0.9505(2) -0.0800(2) 0.0917(14) Uani 1 1 d . . . . .
H1SA H 1.008577 0.991265 -0.094103 0.138 Uiso 1 1 calc GR . . . .
H1SB H 1.032092 0.917152 -0.067047 0.138 Uiso 1 1 calc GR . . . .
H1SC H 0.944150 0.962133 -0.046333 0.138 Uiso 1 1 calc GR . . . .
O1S O 0.9056(2) 0.92299(16) -0.12679(11) 0.0885(9) Uani 1 1 d . . . . .
H1S H 0.866869 0.896434 -0.112600 0.133 Uiso 1 1 calc GR . . . .
C2S C 0.7754(4) 0.9878(2) -0.26900(18) 0.0908(13) Uani 1 1 d . . . . .
H2SA H 0.752194 0.959027 -0.303699 0.136 Uiso 1 1 calc GR . . . .
H2SB H 0.850443 0.989218 -0.261106 0.136 Uiso 1 1 calc GR . . . .
H2SC H 0.748569 1.033666 -0.277050 0.136 Uiso 1 1 calc GR . . . .
O2S O 0.7393(2) 0.96113(18) -0.21842(15) 0.1041(10) Uani 1 1 d . . . . .
H2S H 0.789225 0.951732 -0.191862 0.156 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
C35 0.0358(14) 0.0208(12) 0.0297(14) 0.0027(10) 0.0061(11) -0.0018(10)
C36 0.0327(14) 0.0215(12) 0.0321(14) 0.0032(10) 0.0041(11) -0.0053(10)
C28 0.0308(14) 0.0323(14) 0.0325(14) 0.0083(11) 0.0087(11) -0.0002(11)
C34 0.0315(14) 0.0187(12) 0.0375(15) 0.0073(11) 0.0080(11) -0.0025(10)
C33 0.0326(14) 0.0234(13) 0.0320(14) 0.0026(10) 0.0012(11) -0.0041(10)
C37 0.0336(14) 0.0248(13) 0.0368(15) 0.0039(11) 0.0087(12) 0.0000(11)
C29 0.0373(15) 0.0281(13) 0.0332(14) 0.0010(11) 0.0121(12) 0.0003(11)
C27 0.0371(15) 0.0364(15) 0.0305(14) 0.0048(12) 0.0062(12) -0.0037(12)
C39 0.0495(17) 0.0296(14) 0.0307(14) -0.0055(11) 0.0030(12) 0.0000(12)
C32 0.0366(15) 0.0190(12) 0.0343(14) 0.0022(10) 0.0049(12) -0.0028(10)
C31 0.0358(15) 0.0299(14) 0.0509(17) -0.0025(13) 0.0157(13) -0.0006(11)
C53 0.0311(14) 0.0258(13) 0.0399(15) 0.0053(11) -0.0006(12) -0.0025(11)
C26 0.0430(16) 0.0298(14) 0.0343(15) 0.0034(11) 0.0147(12) -0.0075(12)
C48 0.0387(15) 0.0429(16) 0.0297(14) 0.0037(12) 0.0097(12) 0.0041(12)
C59 0.0386(16) 0.0426(16) 0.0345(15) -0.0099(12) 0.0035(12) -0.0004(12)
C52 0.0308(14) 0.0272(14) 0.0482(17) 0.0051(12) 0.0019(12) 0.0010(11)
C41 0.0483(18) 0.0374(16) 0.0521(18) 0.0001(13) 0.0157(14) 0.0105(13)
C47 0.0396(16) 0.0348(15) 0.0381(15) -0.0015(12) 0.0052(12) -0.0006(12)
C30 0.0320(15) 0.0313(14) 0.0431(16) -0.0029(12) 0.0061(12) -0.0053(11)
C46 0.0404(16) 0.0300(14) 0.0432(16) -0.0014(12) 0.0121(13) -0.0059(12)
C42 0.0513(18) 0.0460(17) 0.0460(17) -0.0025(14) 0.0168(14) 0.0119(14)
C51 0.0313(15) 0.0314(15) 0.067(2) -0.0006(14) 0.0211(14) 0.0034(11)
C38 0.0476(17) 0.0353(15) 0.0459(17) -0.0068(13) 0.0153(14) -0.0081(13)
C40 0.0537(18) 0.0324(15) 0.0417(17) -0.0068(12) 0.0084(14) 0.0108(13)
C50 0.0393(15) 0.0407(16) 0.0430(16) -0.0069(13) 0.0206(13) -0.0065(12)
C58 0.0421(17) 0.0481(18) 0.0439(17) -0.0110(14) 0.0009(13) -0.0022(13)
C49 0.0384(16) 0.0454(16) 0.0366(15) 0.0075(13) 0.0110(12) 0.0063(13)
C45 0.0363(16) 0.0462(17) 0.0499(18) -0.0017(14) 0.0114(13) -0.0033(13)
C43 0.0533(18) 0.0480(18) 0.0405(16) 0.0006(14) 0.0179(14) 0.0128(14)
C44 0.0374(16) 0.0513(18) 0.0477(17) 0.0003(14) 0.0119(13) 0.0030(13)
O6 0.0287(9) 0.0285(9) 0.0368(10) 0.0027(8) 0.0049(8) -0.0012(7)
O5 0.0259(9) 0.0338(10) 0.0412(10) 0.0049(8) 0.0098(8) 0.0033(7)
O2 0.0417(11) 0.0339(10) 0.0416(11) -0.0005(8) 0.0147(8) -0.0043(8)
O4 0.0443(11) 0.0350(10) 0.0348(10) 0.0021(8) 0.0045(8) 0.0084(8)
O10 0.0290(9) 0.0389(10) 0.0332(10) -0.0031(8) 0.0037(8) -0.0044(8)
O1 0.0438(11) 0.0293(10) 0.0378(10) -0.0090(8) 0.0127(8) -0.0053(8)
O3 0.0353(10) 0.0424(11) 0.0341(10) -0.0008(8) 0.0060(8) 0.0050(8)
O9 0.0312(10) 0.0562(13) 0.0404(11) -0.0013(9) 0.0058(8) 0.0017(9)
O7 0.0305(11) 0.0567(13) 0.0742(15) -0.0257(11) -0.0010(10) 0.0040(9)
O8 0.036(4) 0.054(4) 0.029(4) 0.003(3) 0.004(4) 0.000(3)
C55 0.045(3) 0.053(4) 0.042(4) -0.004(3) 0.009(3) -0.001(3)
C56 0.020(3) 0.057(4) 0.043(5) 0.015(4) -0.004(3) -0.002(3)
C54 0.036(3) 0.041(3) 0.041(4) 0.009(3) 0.001(3) 0.006(2)
O8A 0.048(8) 0.066(7) 0.035(5) -0.019(4) 0.018(4) -0.020(5)
C55A 0.037(4) 0.066(6) 0.027(5) -0.003(4) -0.007(3) 0.007(4)
C56A 0.118(18) 0.099(12) 0.057(9) 0.003(8) 0.044(10) 0.008(9)
C54A 0.031(4) 0.047(6) 0.040(6) -0.003(5) -0.005(4) 0.015(4)
C57 0.0428(18) 0.064(2) 0.0531(19) -0.0065(16) 0.0175(15) 0.0007(15)
C13 0.0276(13) 0.0172(11) 0.0228(12) 0.0014(9) 0.0058(10) -0.0027(9)
C1 0.0263(13) 0.0223(12) 0.0216(12) 0.0026(10) 0.0053(10) -0.0033(10)
C12 0.0265(13) 0.0185(12) 0.0287(13) 0.0016(10) 0.0071(10) -0.0010(9)
C14 0.0276(13) 0.0210(12) 0.0250(12) -0.0038(10) 0.0032(10) -0.0053(10)
C15 0.0320(14) 0.0315(14) 0.0285(13) -0.0039(11) 0.0073(11) -0.0058(11)
C25 0.0297(14) 0.0254(13) 0.0362(14) -0.0008(11) 0.0084(11) -0.0005(10)
C22 0.0296(14) 0.0401(16) 0.0349(15) -0.0035(12) 0.0056(11) -0.0109(12)
C7 0.0323(14) 0.0374(15) 0.0286(14) -0.0045(11) 0.0032(11) -0.0006(11)
C19 0.0293(14) 0.0342(14) 0.0252(13) -0.0008(11) 0.0057(11) -0.0065(11)
C9 0.0283(13) 0.0197(12) 0.0244(13) 0.0017(10) 0.0053(10) -0.0032(10)
C8 0.0268(12) 0.0176(11) 0.0224(12) 0.0014(9) 0.0066(10) -0.0012(9)
C10 0.0297(14) 0.0273(13) 0.0260(13) -0.0067(10) 0.0033(10) -0.0047(10)
C24 0.0350(15) 0.0306(14) 0.0430(16) 0.0018(12) 0.0113(12) 0.0073(11)
C11 0.0360(15) 0.0218(12) 0.0309(14) -0.0054(10) 0.0110(11) 0.0014(10)
C2 0.0257(13) 0.0271(13) 0.0255(13) -0.0046(10) 0.0079(10) -0.0079(10)
C3 0.0285(13) 0.0293(13) 0.0319(14) -0.0022(11) 0.0096(11) -0.0029(10)
C20 0.0296(13) 0.0244(12) 0.0229(12) 0.0007(10) 0.0075(10) 0.0020(10)
C23 0.0251(14) 0.0495(17) 0.0364(15) 0.0021(13) 0.0063(11) 0.0008(12)
C16 0.0260(14) 0.0540(18) 0.0447(17) -0.0054(14) 0.0106(12) -0.0061(12)
C21 0.0332(14) 0.0249(13) 0.0326(14) -0.0012(11) 0.0082(11) -0.0024(10)
C18 0.0373(16) 0.0502(17) 0.0300(14) 0.0011(13) 0.0001(12) -0.0056(13)
C4 0.0388(15) 0.0302(14) 0.0419(16) -0.0103(12) 0.0187(13) -0.0059(11)
C17 0.0251(14) 0.0613(19) 0.0444(17) -0.0008(14) -0.0034(12) 0.0013(13)
C5 0.0452(17) 0.0476(17) 0.0334(15) -0.0181(13) 0.0157(13) -0.0113(14)
C6 0.0453(17) 0.0527(18) 0.0270(15) -0.0082(13) 0.0024(12) -0.0058(14)
N1 0.0202(10) 0.0231(10) 0.0234(10) -0.0018(8) 0.0053(8) 0.0012(8)
N2 0.0258(11) 0.0231(10) 0.0231(10) -0.0007(8) 0.0041(8) -0.0019(8)
C1S 0.085(3) 0.082(3) 0.102(3) 0.013(2) -0.003(2) -0.037(2)
O1S 0.105(2) 0.101(2) 0.0607(16) 0.0093(15) 0.0183(15) -0.0524(17)
C2S 0.112(3) 0.090(3) 0.065(3) -0.004(2) -0.001(2) 0.028(3)
O2S 0.121(3) 0.091(2) 0.105(3) -0.002(2) 0.032(2) 0.012(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
C35 C36 1.380(3) . ?
C35 C34 1.395(3) . ?
O8Ab C55A 1.425(13) . ?
O8Ab C56A 1.414(14) . ?
C55Ab C54A 1.500(10) . ?
C56Ab C57 1.482(17) . ?
C36 C37 1.397(3) . ?
C36 O10 1.370(3) . ?
C28 C29 1.378(3) . ?
C28 C27 1.394(4) . ?
C28 O3 1.372(3) . ?
C34 C33 1.384(3) . ?
C34 O6 1.374(3) . ?
C33 C32 1.391(3) . ?
C37 C32 1.384(3) . ?
C29 C30 1.385(3) . ?
C27 C26 1.381(4) . ?
C39 C40 1.511(4) . ?
C39 O1 1.427(3) . ?
C32 C47 1.518(3) . ?
C31 C26 1.391(4) . ?
C31 C30 1.382(4) . ?
C53 C52 1.489(3) . ?
C53 O6 1.433(3) . ?
C26 C38 1.510(4) . ?
C48 C49 1.499(3) . ?
C48 O3 1.436(3) . ?
C59 C58 1.502(4) . ?
C59 O10 1.432(3) . ?
C52 O5 1.427(3) . ?
C41 C42 1.512(4) . ?
C41 C40 1.512(4) . ?
C47 O2 1.424(3) . ?
C30 O7 1.378(3) . ?
C46 C45 1.498(4) . ?
C46 O2 1.425(3) . ?
C42 C43 1.536(4) . ?
C51 C50 1.489(4) . ?
C51 O5 1.417(3) . ?
C38 O1 1.412(3) . ?
C50 O4 1.412(3) . ?
C58 O9 1.421(3) . ?
C49 O4 1.420(3) . ?
C45 C44 1.522(4) . ?
C43 C44 1.510(4) . ?
O9 C57 1.418(3) . ?
O7 C54 1.428(6) . ?
O7 C54A 1.508(8) . ?
O8A C55 1.434(10) . ?
O8A C56 1.416(9) . ?
C55A C54 1.488(8) . ?
C56A C57 1.447(10) . ?
C13 C12 1.407(3) . ?
C13 C8 1.408(3) . ?
C13 N2 1.383(3) . ?
C1 C2 1.470(3) . ?
C1 N1 1.365(3) . ?
C1 N2 1.321(3) . ?
C12 C11 1.389(3) . ?
C12 C20 1.481(3) . ?
C14 C15 1.393(3) . ?
C14 C19 1.394(3) . ?
C14 C9 1.483(3) . ?
C15 C16 1.383(4) . ?
C25 C24 1.381(3) . ?
C25 C20 1.395(3) . ?
C22 C23 1.373(4) . ?
C22 C21 1.380(3) . ?
C7 C2 1.391(3) . ?
C7 C6 1.383(3) . ?
C19 C18 1.376(3) . ?
C9 C8 1.402(3) . ?
C9 C10 1.383(3) . ?
C8 N1 1.377(3) . ?
C10 C11 1.389(3) . ?
C24 C23 1.375(4) . ?
C2 C3 1.390(3) . ?
C3 C4 1.384(3) . ?
C20 C21 1.396(3) . ?
C16 C17 1.378(4) . ?
C18 C17 1.383(4) . ?
C4 C5 1.372(4) . ?
C5 C6 1.380(4) . ?
C1S O1S 1.388(4) . ?
C2S O2S 1.393(5) . ?
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
C36 C35 C34 119.2(2) . . ?
C55Ab C54Ab O7 103.7(6) . . ?
C56Ab O8Ab C55A 114.7(14) . . ?
O8Ab C55Ab C54A 111.1(10) . . ?
O8Ab C56Ab C57 113.6(16) . . ?
C35 C36 C37 120.4(2) . . ?
O10 C36 C35 124.3(2) . . ?
O10 C36 C37 115.3(2) . . ?
C29 C28 C27 120.0(2) . . ?
O3 C28 C29 124.1(2) . . ?
O3 C28 C27 115.9(2) . . ?
C33 C34 C35 120.9(2) . . ?
O6 C34 C35 114.6(2) . . ?
O6 C34 C33 124.5(2) . . ?
C34 C33 C32 119.4(2) . . ?
C32 C37 C36 119.8(2) . . ?
C28 C29 C30 119.1(2) . . ?
C26 C27 C28 120.5(2) . . ?
O1 C39 C40 110.0(2) . . ?
C33 C32 C47 118.1(2) . . ?
C37 C32 C33 120.2(2) . . ?
C37 C32 C47 121.7(2) . . ?
C30 C31 C26 119.1(2) . . ?
O6 C53 C52 108.2(2) . . ?
C27 C26 C31 119.7(2) . . ?
C27 C26 C38 119.1(2) . . ?
C31 C26 C38 121.0(2) . . ?
O3 C48 C49 107.6(2) . . ?
O10 C59 C58 108.8(2) . . ?
O5 C52 C53 109.0(2) . . ?
C42 C41 C40 116.8(2) . . ?
O2 C47 C32 114.3(2) . . ?
C31 C30 C29 121.6(2) . . ?
O7 C30 C29 113.2(2) . . ?
O7 C30 C31 125.1(2) . . ?
O2 C46 C45 109.0(2) . . ?
C41 C42 C43 112.3(2) . . ?
O5 C51 C50 110.6(2) . . ?
O1 C38 C26 112.2(2) . . ?
C39 C40 C41 113.0(2) . . ?
O4 C50 C51 110.0(2) . . ?
O9 C58 C59 115.0(2) . . ?
O4 C49 C48 112.4(2) . . ?
C46 C45 C44 113.3(2) . . ?
C44 C43 C42 112.9(2) . . ?
C43 C44 C45 115.2(2) . . ?
C34 O6 C53 117.65(19) . . ?
C51 O5 C52 112.03(18) . . ?
C47 O2 C46 113.58(19) . . ?
C50 O4 C49 113.5(2) . . ?
C36 O10 C59 117.44(19) . . ?
C38 O1 C39 112.06(19) . . ?
C28 O3 C48 117.40(19) . . ?
C57 O9 C58 114.7(2) . . ?
C30 O7 C54 127.0(4) . . ?
C30 O7 C54A 107.9(4) . . ?
C56A O8A C55 113.0(9) . . ?
O8A C55A C54 111.0(7) . . ?
O8A C56A C57 113.3(9) . . ?
O7 C54A C55 107.1(5) . . ?
O9 C57 C56 107.9(5) . . ?
O9 C57 C56A 114.2(8) . . ?
C12 C13 C8 121.0(2) . . ?
N2 C13 C12 128.5(2) . . ?
N2 C13 C8 110.48(19) . . ?
N1 C1 C2 123.9(2) . . ?
N2 C1 C2 123.1(2) . . ?
N2 C1 N1 112.99(19) . . ?
C13 C12 C20 123.6(2) . . ?
C11 C12 C13 115.5(2) . . ?
C11 C12 C20 120.7(2) . . ?
C15 C14 C19 118.4(2) . . ?
C15 C14 C9 122.7(2) . . ?
C19 C14 C9 118.9(2) . . ?
C16 C15 C14 120.1(2) . . ?
C24 C25 C20 120.4(2) . . ?
C23 C22 C21 120.8(2) . . ?
C6 C7 C2 120.4(2) . . ?
C18 C19 C14 121.3(2) . . ?
C8 C9 C14 124.3(2) . . ?
C10 C9 C14 120.8(2) . . ?
C10 C9 C8 114.7(2) . . ?
C9 C8 C13 123.0(2) . . ?
N1 C8 C13 104.64(18) . . ?
N1 C8 C9 132.3(2) . . ?
C9 C10 C11 123.1(2) . . ?
C23 C24 C25 120.7(2) . . ?
C12 C11 C10 122.7(2) . . ?
C7 C2 C1 118.7(2) . . ?
C3 C2 C1 122.2(2) . . ?
C3 C2 C7 119.0(2) . . ?
C4 C3 C2 120.1(2) . . ?
C25 C20 C12 120.9(2) . . ?
C25 C20 C21 118.2(2) . . ?
C21 C20 C12 120.7(2) . . ?
C22 C23 C24 119.4(2) . . ?
C17 C16 C15 120.6(2) . . ?
C22 C21 C20 120.4(2) . . ?
C19 C18 C17 119.6(2) . . ?
C5 C4 C3 120.4(2) . . ?
C16 C17 C18 120.0(3) . . ?
C4 C5 C6 120.1(2) . . ?
C5 C6 C7 120.0(3) . . ?
C1 N1 C8 107.30(18) . . ?
C1 N2 C13 104.58(18) . . ?
_iucr_refine_instructions_details
;
TITL KZ86m_0m in P21/n #14
kz86m_0m.res created by SHELXL-2016/4 at 13:51:59 on 16-Feb-2017
REM reset to P21/n #14
CELL 0.71073 12.9848 19.382 22.2953 90 99.8421 90
ZERR 4 0.001 0.0015 0.0017 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 244 304 8 48
L.S. 20
PLAN 20
TEMP 0
BOND
fmap 2
ACTA
OMIT -1 0 1
OMIT 0 1 1
OMIT 0 2 2
OMIT -1 4 1
OMIT 0 0 2
OMIT -1 0 3
OMIT 1 2 2
OMIT 4 0 2
OMIT 1 1 0
OMIT 1 3 3
REM
REM
REM
WGHT 0.059700 2.488700
FVAR 0.08545 0.57534
C35 1 0.647229 0.936304 0.094223 11.00000 0.03584 0.02078 =
0.02974 0.00269 0.00610 -0.00183
AFIX 43
H35 2 0.643152 0.953650 0.132639 11.00000 -1.20000
AFIX 0
C36 1 0.742774 0.919363 0.079102 11.00000 0.03267 0.02150 =
0.03209 0.00324 0.00412 -0.00530
C28 1 0.496598 0.621694 0.191981 11.00000 0.03077 0.03233 =
0.03248 0.00825 0.00874 -0.00025
C34 1 0.556793 0.927090 0.051167 11.00000 0.03147 0.01869 =
0.03752 0.00726 0.00796 -0.00254
C33 1 0.562096 0.902353 -0.006453 11.00000 0.03262 0.02340 =
0.03199 0.00259 0.00115 -0.00406
AFIX 43
H33 2 0.501325 0.895815 -0.034675 11.00000 -1.20000
AFIX 0
C37 1 0.749320 0.895734 0.020673 11.00000 0.03365 0.02481 =
0.03675 0.00394 0.00867 -0.00005
AFIX 43
H37 2 0.814103 0.885668 0.010346 11.00000 -1.20000
AFIX 0
C29 1 0.582029 0.635187 0.236231 11.00000 0.03732 0.02814 =
0.03320 0.00095 0.01215 0.00030
AFIX 43
H29 2 0.576725 0.665741 0.267721 11.00000 -1.20000
AFIX 0
C27 1 0.505069 0.575036 0.145473 11.00000 0.03708 0.03637 =
0.03047 0.00484 0.00620 -0.00371
AFIX 43
H27 2 0.447375 0.566306 0.115515 11.00000 -1.20000
AFIX 0
C39 1 0.693277 0.440930 0.022528 11.00000 0.04949 0.02957 =
0.03072 -0.00547 0.00298 -0.00004
AFIX 23
H39A 2 0.628123 0.441350 -0.006205 11.00000 -1.20000
H39B 2 0.701060 0.395864 0.041688 11.00000 -1.20000
AFIX 0
C32 1 0.659100 0.887345 -0.021810 11.00000 0.03665 0.01897 =
0.03430 0.00220 0.00491 -0.00282
C31 1 0.685177 0.555648 0.187754 11.00000 0.03582 0.02990 =
0.05086 -0.00250 0.01567 -0.00064
AFIX 43
H31 2 0.748549 0.533683 0.186784 11.00000 -1.20000
AFIX 0
C53 1 0.369015 0.925591 0.033141 11.00000 0.03109 0.02580 =
0.03985 0.00527 -0.00058 -0.00249
AFIX 23
H53A 2 0.372889 0.878953 0.017901 11.00000 -1.20000
H53B 2 0.355261 0.956733 -0.001358 11.00000 -1.20000
AFIX 0
C26 1 0.598441 0.541673 0.143525 11.00000 0.04297 0.02976 =
0.03435 0.00338 0.01474 -0.00753
C48 1 0.384737 0.692725 0.241225 11.00000 0.03869 0.04293 =
0.02970 0.00368 0.00973 0.00414
AFIX 23
H48A 2 0.428576 0.733531 0.244302 11.00000 -1.20000
H48B 2 0.402762 0.666308 0.278495 11.00000 -1.20000
AFIX 0
C59 1 0.832335 0.940283 0.180593 11.00000 0.03858 0.04262 =
0.03454 -0.00991 0.00354 -0.00039
AFIX 23
H59A 2 0.784622 0.909731 0.196768 11.00000 -1.20000
H59B 2 0.807513 0.987254 0.182875 11.00000 -1.20000
AFIX 0
C52 1 0.283890 0.930683 0.069996 11.00000 0.03078 0.02718 =
0.04823 0.00513 0.00194 0.00097
AFIX 23
H52A 2 0.283574 0.976382 0.087701 11.00000 -1.20000
H52B 2 0.216729 0.923064 0.044238 11.00000 -1.20000
AFIX 0
C41 1 0.774759 0.522197 -0.044228 11.00000 0.04832 0.03743 =
0.05206 0.00014 0.01570 0.01047
AFIX 23
H41A 2 0.709249 0.522433 -0.072652 11.00000 -1.20000
H41B 2 0.770950 0.558642 -0.014870 11.00000 -1.20000
AFIX 0
C47 1 0.662514 0.864022 -0.086450 11.00000 0.03962 0.03475 =
0.03808 -0.00149 0.00520 -0.00062
AFIX 23
H47A 2 0.607577 0.830327 -0.098326 11.00000 -1.20000
H47B 2 0.647809 0.903371 -0.113439 11.00000 -1.20000
AFIX 0
C30 1 0.675899 0.602621 0.233161 11.00000 0.03203 0.03127 =
0.04313 -0.00294 0.00607 -0.00527
C46 1 0.771907 0.764466 -0.075471 11.00000 0.04045 0.02997 =
0.04324 -0.00144 0.01211 -0.00585
AFIX 23
H46A 2 0.721732 0.735652 -0.101358 11.00000 -1.20000
H46B 2 0.759444 0.760196 -0.033958 11.00000 -1.20000
AFIX 0
C42 1 0.861490 0.539802 -0.079047 11.00000 0.05128 0.04598 =
0.04605 -0.00245 0.01676 0.01189
AFIX 23
H42A 2 0.860146 0.507331 -0.112278 11.00000 -1.20000
H42B 2 0.928281 0.535058 -0.052225 11.00000 -1.20000
AFIX 0
C51 1 0.216572 0.876726 0.149847 11.00000 0.03130 0.03145 =
0.06748 -0.00064 0.02107 0.00342
AFIX 23
H51A 2 0.154532 0.859980 0.123335 11.00000 -1.20000
H51B 2 0.201772 0.922570 0.163618 11.00000 -1.20000
AFIX 0
C38 1 0.602096 0.486346 0.096256 11.00000 0.04759 0.03535 =
0.04594 -0.00678 0.01530 -0.00808
AFIX 23
H38A 2 0.603108 0.441413 0.115506 11.00000 -1.20000
H38B 2 0.539394 0.489123 0.065673 11.00000 -1.20000
AFIX 0
C40 1 0.783501 0.454076 -0.010699 11.00000 0.05366 0.03241 =
0.04172 -0.00677 0.00839 0.01075
AFIX 23
H40A 2 0.786632 0.417065 -0.039618 11.00000 -1.20000
H40B 2 0.848207 0.453431 0.018412 11.00000 -1.20000
AFIX 0
C50 1 0.242499 0.829957 0.203270 11.00000 0.03928 0.04065 =
0.04298 -0.00693 0.02064 -0.00652
AFIX 23
H50A 2 0.309938 0.842495 0.226611 11.00000 -1.20000
H50B 2 0.190402 0.834774 0.229415 11.00000 -1.20000
AFIX 0
C58 1 0.940241 0.933532 0.217173 11.00000 0.04209 0.04814 =
0.04388 -0.01098 0.00089 -0.00223
AFIX 23
H58A 2 0.988054 0.960328 0.197490 11.00000 -1.20000
H58B 2 0.940290 0.953507 0.257070 11.00000 -1.20000
AFIX 0
C49 1 0.271703 0.712973 0.231818 11.00000 0.03842 0.04544 =
0.03656 0.00754 0.01102 0.00631
AFIX 23
H49A 2 0.228898 0.671986 0.223088 11.00000 -1.20000
H49B 2 0.256195 0.733162 0.269077 11.00000 -1.20000
AFIX 0
C45 1 0.880777 0.741470 -0.079173 11.00000 0.03627 0.04620 =
0.04985 -0.00173 0.01141 -0.00331
AFIX 23
H45A 2 0.929995 0.771024 -0.053414 11.00000 -1.20000
H45B 2 0.892560 0.746988 -0.120710 11.00000 -1.20000
AFIX 0
C43 1 0.851515 0.613458 -0.104812 11.00000 0.05326 0.04805 =
0.04051 0.00060 0.01792 0.01280
AFIX 23
H43A 2 0.883606 0.615370 -0.141000 11.00000 -1.20000
H43B 2 0.778043 0.624613 -0.116742 11.00000 -1.20000
AFIX 0
C44 1 0.902161 0.666777 -0.059847 11.00000 0.03736 0.05133 =
0.04766 0.00031 0.01190 0.00302
AFIX 23
H44A 2 0.977131 0.659324 -0.052783 11.00000 -1.20000
H44B 2 0.878106 0.659515 -0.021468 11.00000 -1.20000
AFIX 0
O6 4 0.465595 0.943635 0.071324 11.00000 0.02866 0.02853 =
0.03678 0.00273 0.00490 -0.00116
O5 4 0.300784 0.880000 0.117061 11.00000 0.02589 0.03385 =
0.04118 0.00490 0.00982 0.00328
O2 4 0.759586 0.834518 -0.094710 11.00000 0.04173 0.03389 =
0.04165 -0.00050 0.01466 -0.00431
O4 4 0.245238 0.760903 0.183470 11.00000 0.04427 0.03500 =
0.03481 0.00211 0.00447 0.00838
O10 4 0.835899 0.922619 0.118612 11.00000 0.02901 0.03887 =
0.03320 -0.00314 0.00375 -0.00444
O1 4 0.690634 0.492785 0.067698 11.00000 0.04383 0.02929 =
0.03781 -0.00904 0.01274 -0.00534
O3 4 0.400447 0.651802 0.189869 11.00000 0.03532 0.04243 =
0.03414 -0.00080 0.00602 0.00504
O9 4 0.978642 0.864882 0.224883 11.00000 0.03121 0.05616 =
0.04041 -0.00127 0.00580 0.00172
SAME 0.02 0.02 O7 O8A C55A > C54A C57
O7 4 0.754235 0.619553 0.280731 11.00000 0.03052 0.05668 =
0.07421 -0.02574 -0.00102 0.00396
PART 1
O8 4 0.941148 0.710784 0.307456 21.00000 0.03629 0.05386 =
0.02913 0.00288 0.00442 -0.00035
C55 1 0.919625 0.655624 0.264257 21.00000 0.04455 0.05337 =
0.04182 -0.00440 0.00926 -0.00140
AFIX 23
H55A 2 0.984873 0.637803 0.254910 21.00000 -1.20000
H55B 2 0.878714 0.673081 0.226847 21.00000 -1.20000
AFIX 0
C56 1 0.993463 0.767011 0.285406 21.00000 0.02004 0.05672 =
0.04266 0.01463 -0.00404 -0.00225
AFIX 23
H56A 2 1.031181 0.750425 0.254283 21.00000 -1.20000
H56B 2 1.044308 0.785446 0.318482 21.00000 -1.20000
AFIX 0
C54 1 0.861309 0.598917 0.288556 21.00000 0.03600 0.04086 =
0.04108 0.00918 0.00130 0.00623
AFIX 23
H54A 2 0.868123 0.556433 0.266573 21.00000 -1.20000
H54B 2 0.888594 0.591312 0.331322 21.00000 -1.20000
AFIX 0
PART 0
PART 2
O8A 4 0.924573 0.713500 0.314352 -21.00000 0.04837 0.06581 =
0.03486 -0.01863 0.01759 -0.02034
C55A 1 0.935234 0.640568 0.310202 -21.00000 0.03652 0.06582 =
0.02747 -0.00291 -0.00708 0.00722
AFIX 23
H55C 2 0.924999 0.619459 0.348191 -21.00000 -1.20000
H55D 2 1.005367 0.629538 0.303719 -21.00000 -1.20000
AFIX 0
C56A 1 0.967783 0.751556 0.270584 -21.00000 0.11843 0.09944 =
0.05696 0.00292 0.04391 0.00828
AFIX 23
H56C 2 0.955843 0.726524 0.232350 -21.00000 -1.20000
H56D 2 1.042740 0.755095 0.283817 -21.00000 -1.20000
AFIX 0
C54A 1 0.857310 0.611645 0.258947 -21.00000 0.03063 0.04721 =
0.04025 -0.00282 -0.00495 0.01502
AFIX 23
H54C 2 0.871868 0.563520 0.251865 -21.00000 -1.20000
H54D 2 0.857710 0.637397 0.221682 -21.00000 -1.20000
AFIX 0
PART 0
C57 1 0.923737 0.821916 0.260151 11.00000 0.04283 0.06365 =
0.05308 -0.00651 0.01750 0.00067
PART 1
AFIX 23
H57A 2 0.862160 0.802799 0.234835 21.00000 -1.20000
H57B 2 0.901605 0.848394 0.292614 21.00000 -1.20000
AFIX 23
PART 0
PART 2
H57C 2 0.851686 0.818201 0.239825 -21.00000 -1.20000
H57D 2 0.923601 0.843765 0.299280 -21.00000 -1.20000
AFIX 0
PART 0
C13 1 0.635050 0.739521 0.110580 11.00000 0.02757 0.01717 =
0.02280 0.00137 0.00580 -0.00266
C1 1 0.580244 0.806894 0.174361 11.00000 0.02628 0.02228 =
0.02162 0.00255 0.00527 -0.00325
C12 1 0.695905 0.697734 0.078664 11.00000 0.02648 0.01850 =
0.02868 0.00156 0.00707 -0.00098
C14 1 0.368881 0.741997 0.003899 11.00000 0.02757 0.02101 =
0.02496 -0.00383 0.00324 -0.00525
C15 1 0.285240 0.740387 0.035582 11.00000 0.03201 0.03148 =
0.02847 -0.00391 0.00730 -0.00576
AFIX 43
H15 2 0.296134 0.727226 0.076289 11.00000 -1.20000
AFIX 0
C25 1 0.855992 0.623605 0.096733 11.00000 0.02972 0.02538 =
0.03625 -0.00077 0.00838 -0.00045
AFIX 43
H25 2 0.813909 0.584650 0.089390 11.00000 -1.20000
AFIX 0
C22 1 0.982892 0.737813 0.120064 11.00000 0.02962 0.04012 =
0.03492 -0.00353 0.00557 -0.01089
AFIX 43
H22 2 1.025701 0.776338 0.128182 11.00000 -1.20000
AFIX 0
C7 1 0.644095 0.835344 0.281923 11.00000 0.03228 0.03744 =
0.02861 -0.00445 0.00321 -0.00063
AFIX 43
H7 2 0.687971 0.797186 0.283906 11.00000 -1.20000
AFIX 0
C19 1 0.349711 0.761912 -0.057057 11.00000 0.02935 0.03416 =
0.02521 -0.00082 0.00572 -0.00649
AFIX 43
H19 2 0.404606 0.762553 -0.078931 11.00000 -1.20000
AFIX 0
C9 1 0.477199 0.724057 0.032585 11.00000 0.02826 0.01968 =
0.02444 0.00173 0.00532 -0.00316
C8 1 0.528526 0.751353 0.087946 11.00000 0.02685 0.01759 =
0.02242 0.00140 0.00661 -0.00120
C10 1 0.538345 0.681796 0.003062 11.00000 0.02975 0.02725 =
0.02596 -0.00674 0.00332 -0.00474
AFIX 43
H10 2 0.507952 0.661345 -0.033425 11.00000 -1.20000
AFIX 0
C24 1 0.963461 0.616663 0.107575 11.00000 0.03498 0.03058 =
0.04298 0.00183 0.01131 0.00730
AFIX 43
H24 2 0.993126 0.573012 0.107333 11.00000 -1.20000
AFIX 0
C11 1 0.643003 0.668459 0.025341 11.00000 0.03602 0.02180 =
0.03089 -0.00539 0.01104 0.00136
AFIX 43
H11 2 0.679140 0.638685 0.003640 11.00000 -1.20000
AFIX 0
C2 1 0.576976 0.850489 0.227949 11.00000 0.02574 0.02707 =
0.02553 -0.00460 0.00794 -0.00786
C3 1 0.511537 0.907537 0.225884 11.00000 0.02845 0.02930 =
0.03185 -0.00218 0.00957 -0.00285
AFIX 43
H3 2 0.465867 0.918071 0.190204 11.00000 -1.20000
AFIX 0
C20 1 0.810247 0.688742 0.096740 11.00000 0.02960 0.02438 =
0.02294 0.00072 0.00750 0.00197
C23 1 1.027058 0.673607 0.118724 11.00000 0.02512 0.04947 =
0.03644 0.00206 0.00628 0.00079
AFIX 43
H23 2 1.099354 0.668654 0.125297 11.00000 -1.20000
AFIX 0
C16 1 0.186046 0.758328 0.006593 11.00000 0.02598 0.05398 =
0.04472 -0.00542 0.01059 -0.00607
AFIX 43
H16 2 0.130370 0.756561 0.027825 11.00000 -1.20000
AFIX 0
C21 1 0.875746 0.745870 0.109510 11.00000 0.03322 0.02491 =
0.03256 -0.00124 0.00817 -0.00243
AFIX 43
H21 2 0.846979 0.789661 0.110915 11.00000 -1.20000
AFIX 0
C18 1 0.251217 0.780643 -0.085527 11.00000 0.03735 0.05016 =
0.02997 0.00109 0.00012 -0.00564
AFIX 43
H18 2 0.239999 0.794457 -0.126068 11.00000 -1.20000
AFIX 0
C4 1 0.514314 0.948672 0.276904 11.00000 0.03883 0.03025 =
0.04194 -0.01026 0.01874 -0.00591
AFIX 43
H4 2 0.470344 0.986743 0.275352 11.00000 -1.20000
AFIX 0
C17 1 0.169012 0.778799 -0.053477 11.00000 0.02511 0.06133 =
0.04442 -0.00076 -0.00340 0.00135
AFIX 43
H17 2 0.102235 0.791373 -0.072461 11.00000 -1.20000
AFIX 0
C5 1 0.581518 0.933636 0.329748 11.00000 0.04521 0.04755 =
0.03343 -0.01806 0.01573 -0.01130
AFIX 43
H5 2 0.583635 0.961871 0.363663 11.00000 -1.20000
AFIX 0
C6 1 0.645962 0.876692 0.332646 11.00000 0.04535 0.05268 =
0.02702 -0.00819 0.00244 -0.00584
AFIX 43
H6 2 0.690629 0.866125 0.368693 11.00000 -1.20000
AFIX 0
N1 3 0.496013 0.794840 0.129874 11.00000 0.02019 0.02310 =
0.02342 -0.00177 0.00526 0.00116
AFIX 43
H1 2 0.434129 0.811337 0.128315 11.00000 -1.20000
AFIX 0
N2 3 0.665421 0.774345 0.164881 11.00000 0.02579 0.02308 =
0.02312 -0.00074 0.00412 -0.00188
C1S 1 0.978203 0.950507 -0.079958 11.00000 0.08501 0.08157 =
0.10178 0.01265 -0.00305 -0.03659
AFIX 137
H1SA 2 1.008577 0.991265 -0.094103 11.00000 -1.50000
H1SB 2 1.032092 0.917152 -0.067047 11.00000 -1.50000
H1SC 2 0.944150 0.962133 -0.046333 11.00000 -1.50000
AFIX 0
O1S 4 0.905598 0.922993 -0.126792 11.00000 0.10484 0.10139 =
0.06069 0.00926 0.01833 -0.05241
AFIX 147
H1S 2 0.866869 0.896434 -0.112600 11.00000 -1.50000
AFIX 0
C2S 1 0.775439 0.987835 -0.268998 11.00000 0.11163 0.09006 =
0.06509 -0.00411 -0.00058 0.02827
AFIX 137
H2SA 2 0.752194 0.959027 -0.303699 11.00000 -1.50000
H2SB 2 0.850443 0.989218 -0.261106 11.00000 -1.50000
H2SC 2 0.748569 1.033666 -0.277050 11.00000 -1.50000
AFIX 0
O2S 4 0.739327 0.961131 -0.218419 11.00000 0.12092 0.09058 =
0.10537 -0.00239 0.03247 0.01190
AFIX 147
H2S 2 0.789225 0.951732 -0.191862 11.00000 -1.50000
AFIX 0
HKLF 4
REM KZ86m_0m in P21/n #14
REM R1 = 0.0561 for 6800 Fo > 4sig(Fo) and 0.0890 for all 9760 data
REM 717 parameters refined using 7 restraints
END
WGHT 0.0597 2.5016
REM Highest difference peak 0.714, deepest hole -0.295, 1-sigma level 0.048
Q1 1 0.4103 0.5589 0.1140 11.00000 0.05 0.71
Q2 1 0.8863 0.8954 0.0107 11.00000 0.05 0.60
Q3 1 0.8477 0.4983 -0.0130 11.00000 0.05 0.27
Q4 1 0.5785 0.7410 0.0964 11.00000 0.05 0.24
Q5 1 0.7303 0.7840 0.1850 11.00000 0.05 0.24
Q6 1 0.3129 0.7826 0.1959 11.00000 0.05 0.23
Q7 1 1.0142 0.9228 -0.1148 11.00000 0.05 0.22
Q8 1 0.5166 0.7577 0.0545 11.00000 0.05 0.22
Q9 1 0.6618 0.7044 0.1018 11.00000 0.05 0.22
Q10 1 0.5242 0.6160 0.2286 11.00000 0.05 0.20
Q11 1 0.8397 0.7110 0.1083 11.00000 0.05 0.20
Q12 1 0.7098 0.4847 -0.0328 11.00000 0.05 0.20
Q13 1 0.7045 0.9003 -0.0109 11.00000 0.05 0.20
Q14 1 0.6254 0.5380 0.1751 11.00000 0.05 0.19
Q15 1 0.8380 0.6629 0.0977 11.00000 0.05 0.19
Q16 1 0.8357 0.6895 0.0703 11.00000 0.05 0.18
Q17 1 0.7605 0.7160 0.0839 11.00000 0.05 0.18
Q18 1 0.4165 0.7219 0.0148 11.00000 0.05 0.18
Q19 1 0.8582 0.7755 0.2256 11.00000 0.05 0.18
Q20 1 1.0602 0.9563 -0.0881 11.00000 0.05 0.18
REM The information below was added by Olex2.
REM
REM R1 = 0.0561 for 6800 Fo > 4sig(Fo) and 0.0890 for all 52531 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.71, deepest hole -0.30
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0890
REM R1_gt = 0.0561
REM wR_ref = 0.1490
REM GOOF = 1.024
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 52531
REM Reflections_gt = 6800
REM Parameters = n/a
REM Hole = -0.30
REM Peak = 0.71
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
#######################################################################
#
# 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_kz74a
_database_code_depnum_ccdc_archive 'CCDC 1533272'
_audit_update_record
;
2017-02-17 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;
_audit_creation_date 2017-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number 2016/4
# start Validation Reply Form
_vrf_THETM01_kz74a
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The actual value of 0.555 is very close.
;
_vrf_PLAT701_kz74a
;
PROBLEM: Bond Calc 1.30(4), Rep 1.462(15), Dev.. 4.05 Sigma
RESPONSE: This is the result of the disorder in the polyether chain.
;
_vrf_PLAT702_kz74a
;
PROBLEM: Angle Calc 122(2), Rep 115.8(8), Dev.. 3.10 Sigma
RESPONSE: This is the result of the disorder in the polyether chain.
;
_vrf_PLAT230_kz74a
;
PROBLEM: Hirshfeld Test Diff for C36 -- C37 .. 7.4 s.u.
RESPONSE: This is the result of the disorder/thermal motion in the alkane chain.
;
_vrf_PLAT331_kz74a
;
PROBLEM: Small Average Phenyl C-C Dist. C20 -C25 1.36 Ang.
RESPONSE: This is not an unreasonable value and is chemically valid.
;
# end Validation Reply Form
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C34 H50 O10, C25 H18 N2, C2 H3 N'
_chemical_formula_sum 'C61 H71 N3 O10'
_chemical_formula_weight 1006.20
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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 orthorhombic
_space_group_IT_number 61
_space_group_name_H-M_alt 'P b c a'
_space_group_name_Hall '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
_cell_length_a 17.819(3)
_cell_length_b 17.457(3)
_cell_length_c 34.337(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 10682(3)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9925
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 26.38
_cell_measurement_theta_min 2.37
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.085
_exptl_absorpt_correction_T_max 0.7411
_exptl_absorpt_correction_T_min 0.5036
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1450 before and 0.0994 after correction.
The Ratio of minimum to maximum transmission is 0.6795.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.251
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 4304
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_special_details
;
The data collection nominally covered a full sphere of reciprocal space by
a combination of 4 sets of \w scans each set at different \f and/or
2\q angles and each scan (30 s exposure) covering -0.500\% degrees in \w.
The crystal to detector distance was 6.05 cm.
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1488
_diffrn_reflns_av_unetI/netI 0.0705
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 38
_diffrn_reflns_limit_l_min -38
_diffrn_reflns_number 80139
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 23.256
_diffrn_reflns_theta_max 23.256
_diffrn_reflns_theta_min 2.018
_diffrn_ambient_temperature 173
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator Parallel,graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_source_current 30.0
_diffrn_source_power 1.5
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5437
_reflns_number_total 7663
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection 'SMART V5.631 (?, 2016)'
_computing_data_reduction 'SAINT v7.60A (Bruker, 2009)'
_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 'XS (Sheldrick, 2008)'
_refine_diff_density_max 0.499
_refine_diff_density_min -0.309
_refine_diff_density_rms 0.058
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.166
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 760
_refine_ls_number_reflns 7663
_refine_ls_number_restraints 292
_refine_ls_R_factor_all 0.1513
_refine_ls_R_factor_gt 0.1148
_refine_ls_restrained_S_all 1.167
_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^)+(0.0493P)^2^+32.7204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2232
_refine_ls_wR_factor_ref 0.2406
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C57 \\sim C55 \\sim C56 \\sim O8 \\sim C55A \\sim C56A \\sim O8A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C40 \\sim C45 \\sim C46 \\sim C41 \\sim C43 \\sim C44 \\sim C42 \\sim C40A
\\sim C45A \\sim C46A \\sim C41A \\sim C43A \\sim C44A \\sim C42A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Same fragment restrains
{C54, C57, C55A, C56A, O8A} sigma for 1-2: 0.02, 1-3: 0.02
as
{C54, C57, C55, C56, O8}
{C39, C40A, C45A, C46A, C41A, C43A, C44A, C42A, O2} sigma for 1-2: 0.02, 1-3:
0.02
as
{C39, C40, C45, C46, C41, C43, C44, C42, O2}
4. Others
Sof(H54C)=Sof(H54D)=Sof(H57C)=Sof(H57D)=Sof(C55A)=Sof(H55C)=Sof(H55D)=
Sof(C56A)=Sof(H56C)=Sof(H56D)=Sof(O8A)=1-FVAR(1)
Sof(H54A)=Sof(H54B)=Sof(H57A)=Sof(H57B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=
Sof(H56A)=Sof(H56B)=Sof(O8)=FVAR(1)
Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(C45A)=Sof(H45C)=
Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C41A)=Sof(H41C)=Sof(H41D)=
Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C42A)=
Sof(H42C)=Sof(H42D)=1-FVAR(2)
Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C45)=Sof(H45A)=Sof(H45B)=
Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C43)=Sof(H43A)=
Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C42)=Sof(H42A)=Sof(H42B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
C54(H54A,H54B), C54(H54C,H54D), C57(H57A,H57B), C57(H57C,H57D), C55(H55A,
H55B), C56(H56A,H56B), C48(H48A,H48B), C49(H49A,H49B), C51(H51A,H51B),
C53(H53A,H53B), C50(H50A,H50B), C52(H52A,H52B), C38(H38A,H38B), C47(H47A,H47B),
C59(H59A,H59B), C58(H58A,H58B), C39(H39A,H39B), C39(H39C,H39D), C40(H40A,
H40B), C45(H45A,H45B), C46(H46A,H46B), C41(H41A,H41B), C43(H43A,H43B),
C44(H44A,H44B), C42(H42A,H42B), C40A(H40C,H40D), C45A(H45C,H45D), C46A(H46C,
H46D), C41A(H41C,H41D), C43A(H43C,H43D), C44A(H44C,H44D), C42A(H42C,H42D),
C55A(H55C,H55D), C56A(H56C,H56D)
5.b Aromatic/amide H refined with riding coordinates:
C35(H35), C29(H29), C31(H31), C37(H37), C27(H27), C33(H33), C11(H11),
C15(H15), C19(H19), C17(H17), C18(H18), C10(H10), C16(H16), C3(H3), C25(H25),
C23(H23), C7(H7), C6(H6), C4(H4), C5(H5), C21(H21), C24(H24), C22(H22), N1(H1)
5.c Idealised Me refined as rotating group:
C2S(H2SA,H2SB,H2SC)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_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
C30 C 0.0716(3) 0.8181(3) 0.21152(18) 0.0396(15) Uani 1 1 d . . . . .
C35 C 0.0307(4) 0.4838(3) 0.1110(2) 0.0569(19) Uani 1 1 d . . . . .
H35 H 0.054428 0.453685 0.129602 0.068 Uiso 1 1 calc R . . . .
C29 C 0.1434(3) 0.7963(3) 0.20039(17) 0.0418(15) Uani 1 1 d . . . . .
H29 H 0.168001 0.757262 0.213681 0.050 Uiso 1 1 calc R . . . .
C28 C 0.1781(3) 0.8326(3) 0.16949(18) 0.0433(15) Uani 1 1 d . . . . .
C31 C 0.0349(3) 0.8771(3) 0.19216(18) 0.0456(16) Uani 1 1 d . . . . .
H31 H -0.013527 0.891155 0.199270 0.055 Uiso 1 1 calc R . . . .
C54 C -0.0339(3) 0.7970(4) 0.25365(19) 0.0512(17) Uani 1 1 d D . . . .
H54A H -0.069055 0.786954 0.232677 0.061 Uiso 0.601(13) 1 calc R . P A 1
H54B H -0.037578 0.850595 0.260896 0.061 Uiso 0.601(13) 1 calc R . P A 1
H54C H -0.064948 0.801218 0.230528 0.061 Uiso 0.399(13) 1 calc R . P A 2
H54D H -0.033469 0.846751 0.266246 0.061 Uiso 0.399(13) 1 calc R . P A 2
C57 C -0.1389(4) 0.5604(5) 0.2604(2) 0.081(3) Uani 1 1 d D U . . .
H57A H -0.121779 0.531674 0.282866 0.097 Uiso 0.601(13) 1 calc R . P A 1
H57B H -0.190460 0.546017 0.255109 0.097 Uiso 0.601(13) 1 calc R . P A 1
H57C H -0.151606 0.513896 0.274339 0.097 Uiso 0.399(13) 1 calc R . P A 2
H57D H -0.185070 0.584533 0.251835 0.097 Uiso 0.399(13) 1 calc R . P A 2
C55 C -0.0500(13) 0.7465(8) 0.2879(4) 0.050(5) Uani 0.601(13) 1 d D U P A 1
H55A H -0.008243 0.750233 0.305932 0.060 Uiso 0.601(13) 1 calc R . P A 1
H55B H -0.094081 0.766241 0.301172 0.060 Uiso 0.601(13) 1 calc R . P A 1
C56 C -0.1345(6) 0.6493(7) 0.2693(4) 0.063(4) Uani 0.601(13) 1 d D U P A 1
H56A H -0.149581 0.678030 0.246462 0.076 Uiso 0.601(13) 1 calc R . P A 1
H56B H -0.168613 0.661891 0.290381 0.076 Uiso 0.601(13) 1 calc R . P A 1
O8 O -0.0622(4) 0.6691(4) 0.2796(3) 0.051(3) Uani 0.601(13) 1 d D U P A 1
C48 C 0.2811(3) 0.8324(4) 0.12425(18) 0.0502(17) Uani 1 1 d . . . . .
H48A H 0.296474 0.885282 0.127683 0.060 Uiso 1 1 calc R . . . .
H48B H 0.244192 0.830653 0.103488 0.060 Uiso 1 1 calc R . . . .
C36 C -0.0456(4) 0.5043(3) 0.1163(2) 0.057(2) Uani 1 1 d . . . . .
C37 C -0.0794(5) 0.5458(4) 0.0872(2) 0.069(2) Uani 1 1 d . . . . .
H37 H -0.129865 0.558620 0.089754 0.083 Uiso 1 1 calc R . . . .
C34 C 0.0712(4) 0.5083(3) 0.0780(2) 0.060(2) Uani 1 1 d . . . . .
C27 C 0.1429(3) 0.8926(3) 0.15046(19) 0.0496(17) Uani 1 1 d . . . . .
H27 H 0.166939 0.917798 0.130124 0.059 Uiso 1 1 calc R . . . .
C49 C 0.3471(3) 0.7850(4) 0.11346(19) 0.0554(18) Uani 1 1 d . . . . .
H49A H 0.377724 0.812317 0.094664 0.066 Uiso 1 1 calc R . . . .
H49B H 0.377499 0.775262 0.136377 0.066 Uiso 1 1 calc R . . . .
C26 C 0.0718(4) 0.9149(4) 0.16182(19) 0.0514(17) Uani 1 1 d . . . . .
C51 C 0.3525(4) 0.6014(4) 0.0629(2) 0.074(2) Uani 1 1 d . . . . .
H51A H 0.326412 0.624775 0.041119 0.089 Uiso 1 1 calc R . . . .
H51B H 0.395224 0.573691 0.052495 0.089 Uiso 1 1 calc R . . . .
C33 C 0.0346(5) 0.5505(4) 0.0493(2) 0.073(2) Uani 1 1 d . . . . .
H33 H 0.060209 0.566176 0.027125 0.088 Uiso 1 1 calc R . . . .
C53 C 0.1906(5) 0.5157(4) 0.0456(2) 0.067(2) Uani 1 1 d . . . . .
H53A H 0.183402 0.570483 0.042645 0.081 Uiso 1 1 calc R . . . .
H53B H 0.175883 0.490858 0.021560 0.081 Uiso 1 1 calc R . . . .
C50 C 0.3803(4) 0.6630(5) 0.0891(2) 0.075(2) Uani 1 1 d . . . . .
H50A H 0.398566 0.640574 0.113132 0.090 Uiso 1 1 calc R . . . .
H50B H 0.421726 0.689586 0.076709 0.090 Uiso 1 1 calc R . . . .
C52 C 0.2719(5) 0.4988(4) 0.0543(2) 0.074(2) Uani 1 1 d . . . . .
H52A H 0.275591 0.447498 0.065016 0.089 Uiso 1 1 calc R . . . .
H52B H 0.299903 0.499649 0.030126 0.089 Uiso 1 1 calc R . . . .
C32 C -0.0417(5) 0.5692(4) 0.0544(2) 0.068(2) Uani 1 1 d . . . . .
C38 C 0.0348(5) 0.9817(5) 0.1412(3) 0.087(3) Uani 1 1 d . . . . .
H38A H 0.057086 1.029062 0.150399 0.105 Uiso 1 1 calc R . . . .
H38B H 0.044822 0.977821 0.113473 0.105 Uiso 1 1 calc R . . . .
C47 C -0.0763(5) 0.6186(5) 0.0219(3) 0.095(3) Uani 1 1 d . . . . .
H47A H -0.055440 0.669897 0.023162 0.114 Uiso 1 1 calc R . . . .
H47B H -0.063527 0.596966 -0.003237 0.114 Uiso 1 1 calc R . . . .
C59 C -0.0556(4) 0.4524(4) 0.1802(2) 0.063(2) Uani 1 1 d . . . . .
H59A H -0.005752 0.472636 0.184838 0.075 Uiso 1 1 calc R . . . .
H59B H -0.051489 0.397655 0.175742 0.075 Uiso 1 1 calc R . . . .
C58 C -0.1049(4) 0.4675(4) 0.2147(3) 0.076(2) Uani 1 1 d . . . . .
H58A H -0.157173 0.460710 0.207530 0.091 Uiso 1 1 calc R . . . .
H58B H -0.093184 0.431757 0.235432 0.091 Uiso 1 1 calc R . . . .
O7 O 0.0410(2) 0.7784(2) 0.24200(12) 0.0454(10) Uani 1 1 d . . . . .
O3 O 0.2485(2) 0.8047(2) 0.15935(12) 0.0501(11) Uani 1 1 d . . . . .
O1 O -0.0401(3) 0.9847(3) 0.14679(16) 0.0874(18) Uani 1 1 d . . . . .
O9 O -0.0929(3) 0.5424(3) 0.22735(14) 0.0735(15) Uani 1 1 d . . . . .
O10 O -0.0876(3) 0.4880(3) 0.14758(15) 0.0625(13) Uani 1 1 d . . . . .
O6 O 0.1460(3) 0.4879(3) 0.07709(14) 0.0637(13) Uani 1 1 d . . . . .
O5 O 0.3052(3) 0.5502(3) 0.08046(14) 0.0716(14) Uani 1 1 d . . . . .
O4 O 0.3228(2) 0.7152(3) 0.09739(13) 0.0567(12) Uani 1 1 d . . . . .
C39 C -0.0750(5) 1.0509(5) 0.1299(2) 0.085(3) Uani 1 1 d D . . . .
H39A H -0.049529 1.065077 0.105970 0.102 Uiso 0.818(8) 1 calc R . P B 1
H39B H -0.072314 1.093862 0.147774 0.102 Uiso 0.818(8) 1 calc R . P B 1
H39C H -0.036877 1.076815 0.114589 0.102 Uiso 0.182(8) 1 calc R . P B 2
H39D H -0.087777 1.085021 0.151188 0.102 Uiso 0.182(8) 1 calc R . P B 2
C40 C -0.1555(7) 1.0311(7) 0.1216(4) 0.108(5) Uani 0.818(8) 1 d D U P B 1
H40A H -0.177402 1.005488 0.143936 0.130 Uiso 0.818(8) 1 calc R . P B 1
H40B H -0.183968 1.077467 0.116617 0.130 Uiso 0.818(8) 1 calc R . P B 1
C45 C -0.1940(7) 0.7573(6) 0.0297(4) 0.107(4) Uani 0.818(8) 1 d D U P B 1
H45A H -0.233293 0.753609 0.010267 0.128 Uiso 0.818(8) 1 calc R . P B 1
H45B H -0.147933 0.773005 0.017010 0.128 Uiso 0.818(8) 1 calc R . P B 1
C46 C -0.1834(7) 0.6818(6) 0.0497(3) 0.104(4) Uani 0.818(8) 1 d D U P B 1
H46A H -0.148881 0.688757 0.071262 0.124 Uiso 0.818(8) 1 calc R . P B 1
H46B H -0.231192 0.665710 0.060514 0.124 Uiso 0.818(8) 1 calc R . P B 1
C41 C -0.1586(7) 0.9809(8) 0.0876(3) 0.111(4) Uani 0.818(8) 1 d D U P B 1
H41A H -0.128234 0.936003 0.093002 0.133 Uiso 0.818(8) 1 calc R . P B 1
H41B H -0.135416 1.007485 0.065886 0.133 Uiso 0.818(8) 1 calc R . P B 1
C43 C -0.2284(7) 0.8925(8) 0.0448(3) 0.111(4) Uani 0.818(8) 1 d D U P B 1
H43A H -0.273833 0.891609 0.029239 0.134 Uiso 0.818(8) 1 calc R . P B 1
H43B H -0.186975 0.904956 0.027660 0.134 Uiso 0.818(8) 1 calc R . P B 1
C44 C -0.2159(7) 0.8152(8) 0.0613(4) 0.124(5) Uani 0.818(8) 1 d D U P B 1
H44A H -0.261383 0.798042 0.074207 0.149 Uiso 0.818(8) 1 calc R . P B 1
H44B H -0.176398 0.817767 0.080725 0.149 Uiso 0.818(8) 1 calc R . P B 1
C42 C -0.2355(6) 0.9539(8) 0.0747(3) 0.103(4) Uani 0.818(8) 1 d D U P B 1
H42A H -0.262992 0.934523 0.096984 0.123 Uiso 0.818(8) 1 calc R . P B 1
H42B H -0.263344 0.996696 0.063922 0.123 Uiso 0.818(8) 1 calc R . P B 1
O2 O -0.1558(4) 0.6227(3) 0.02559(18) 0.103(2) Uani 1 1 d D . . . .
C40A C -0.143(2) 1.045(2) 0.1048(16) 0.119(13) Uani 0.182(8) 1 d D U P B 2
H40C H -0.174391 1.089164 0.109040 0.143 Uiso 0.182(8) 1 calc R . P B 2
H40D H -0.127476 1.044868 0.077716 0.143 Uiso 0.182(8) 1 calc R . P B 2
C45A C -0.223(3) 0.736(2) 0.0500(11) 0.115(10) Uani 0.182(8) 1 d D U P B 2
H45C H -0.182674 0.737337 0.069199 0.138 Uiso 0.182(8) 1 calc R . P B 2
H45D H -0.265690 0.711364 0.061564 0.138 Uiso 0.182(8) 1 calc R . P B 2
C46A C -0.197(3) 0.691(2) 0.0151(10) 0.133(12) Uani 0.182(8) 1 d D U P B 2
H46C H -0.240522 0.676666 -0.000255 0.159 Uiso 0.182(8) 1 calc R . P B 2
H46D H -0.165358 0.723295 -0.001083 0.159 Uiso 0.182(8) 1 calc R . P B 2
C41A C -0.1873(19) 0.976(3) 0.1121(12) 0.109(10) Uani 0.182(8) 1 d D U P B 2
H41C H -0.239658 0.990412 0.113571 0.131 Uiso 0.182(8) 1 calc R . P B 2
H41D H -0.173231 0.955754 0.137476 0.131 Uiso 0.182(8) 1 calc R . P B 2
C43A C -0.249(2) 0.871(2) 0.0732(14) 0.135(10) Uani 0.182(8) 1 d D U P B 2
H43C H -0.287940 0.907677 0.067852 0.163 Uiso 0.182(8) 1 calc R . P B 2
H43D H -0.264284 0.841033 0.095714 0.163 Uiso 0.182(8) 1 calc R . P B 2
C44A C -0.243(3) 0.8173(17) 0.0390(11) 0.114(10) Uani 0.182(8) 1 d D U P B 2
H44C H -0.205592 0.836977 0.021078 0.136 Uiso 0.182(8) 1 calc R . P B 2
H44D H -0.290821 0.816696 0.025395 0.136 Uiso 0.182(8) 1 calc R . P B 2
C42A C -0.180(2) 0.912(2) 0.0830(14) 0.110(9) Uani 0.182(8) 1 d D U P B 2
H42C H -0.159671 0.932810 0.059127 0.132 Uiso 0.182(8) 1 calc R . P B 2
H42D H -0.144240 0.874963 0.092910 0.132 Uiso 0.182(8) 1 calc R . P B 2
C55A C -0.069(2) 0.7411(12) 0.2803(6) 0.070(9) Uani 0.399(13) 1 d D U P A 2
H55C H -0.034702 0.729537 0.301600 0.084 Uiso 0.399(13) 1 calc R . P A 2
H55D H -0.114750 0.761590 0.290982 0.084 Uiso 0.399(13) 1 calc R . P A 2
C56A C -0.0968(10) 0.6132(9) 0.2864(4) 0.063(6) Uani 0.399(13) 1 d D U P A 2
H56C H -0.126841 0.630673 0.308177 0.076 Uiso 0.399(13) 1 calc R . P A 2
H56D H -0.050413 0.590748 0.295796 0.076 Uiso 0.399(13) 1 calc R . P A 2
O8A O -0.0835(8) 0.6736(6) 0.2580(3) 0.047(4) Uani 0.399(13) 1 d D U P A 2
C8 C 0.0366(3) 0.6666(3) 0.15126(15) 0.0283(12) Uani 1 1 d . . . . .
C1 C -0.0803(3) 0.7111(3) 0.15190(16) 0.0321(13) Uani 1 1 d . . . . .
C13 C 0.0237(3) 0.7181(3) 0.12046(15) 0.0290(12) Uani 1 1 d . . . . .
C11 C 0.1475(3) 0.6954(3) 0.09911(16) 0.0340(13) Uani 1 1 d . . . . .
H11 H 0.186006 0.702726 0.081202 0.041 Uiso 1 1 calc R . . . .
C12 C 0.0804(3) 0.7338(3) 0.09324(15) 0.0325(13) Uani 1 1 d . . . . .
C20 C 0.0699(3) 0.7866(3) 0.05968(16) 0.0331(13) Uani 1 1 d . . . . .
C14 C 0.1201(3) 0.5771(3) 0.19073(16) 0.0305(13) Uani 1 1 d . . . . .
C2 C -0.1582(3) 0.7232(3) 0.16534(15) 0.0330(13) Uani 1 1 d . . . . .
C15 C 0.0875(3) 0.5874(3) 0.22737(17) 0.0355(14) Uani 1 1 d . . . . .
H15 H 0.056841 0.629629 0.231893 0.043 Uiso 1 1 calc R . . . .
C9 C 0.1056(3) 0.6294(3) 0.15774(15) 0.0268(12) Uani 1 1 d . . . . .
C19 C 0.1685(3) 0.5142(3) 0.18603(18) 0.0399(14) Uani 1 1 d . . . . .
H19 H 0.192033 0.506560 0.162181 0.048 Uiso 1 1 calc R . . . .
C17 C 0.1476(3) 0.4736(3) 0.2518(2) 0.0475(16) Uani 1 1 d . . . . .
H17 H 0.156381 0.439303 0.272028 0.057 Uiso 1 1 calc R . . . .
C18 C 0.1817(3) 0.4635(3) 0.2161(2) 0.0462(16) Uani 1 1 d . . . . .
H18 H 0.213739 0.422137 0.212244 0.055 Uiso 1 1 calc R . . . .
C10 C 0.1604(3) 0.6464(3) 0.13039(16) 0.0352(14) Uani 1 1 d . . . . .
H10 H 0.207568 0.624284 0.133059 0.042 Uiso 1 1 calc R . . . .
C16 C 0.1006(3) 0.5351(3) 0.25706(18) 0.0440(15) Uani 1 1 d . . . . .
H16 H 0.077002 0.541837 0.280985 0.053 Uiso 1 1 calc R . . . .
C3 C -0.2033(3) 0.6642(4) 0.1773(2) 0.063(2) Uani 1 1 d . . . . .
H3 H -0.185615 0.614147 0.176385 0.075 Uiso 1 1 calc R . . . .
C25 C 0.1135(5) 0.7846(5) 0.0278(2) 0.093(3) Uani 1 1 d . . . . .
H25 H 0.150552 0.747116 0.026485 0.112 Uiso 1 1 calc R . . . .
C23 C 0.0525(4) 0.8863(5) -0.0039(2) 0.068(2) Uani 1 1 d . . . . .
H23 H 0.045456 0.917349 -0.025627 0.082 Uiso 1 1 calc R . . . .
C7 C -0.1858(3) 0.7965(4) 0.16593(19) 0.0541(17) Uani 1 1 d . . . . .
H7 H -0.155843 0.836985 0.157671 0.065 Uiso 1 1 calc R . . . .
C6 C -0.2583(4) 0.8103(5) 0.1789(2) 0.081(3) Uani 1 1 d . . . . .
H6 H -0.277074 0.859997 0.178705 0.097 Uiso 1 1 calc R . . . .
C4 C -0.2751(4) 0.6788(6) 0.1909(2) 0.079(2) Uani 1 1 d . . . . .
H4 H -0.304921 0.638551 0.199489 0.094 Uiso 1 1 calc R . . . .
C5 C -0.3023(4) 0.7519(6) 0.1917(2) 0.074(2) Uani 1 1 d . . . . .
H5 H -0.350425 0.761601 0.200975 0.089 Uiso 1 1 calc R . . . .
C21 C 0.0173(4) 0.8430(5) 0.0592(3) 0.095(3) Uani 1 1 d . . . . .
H21 H -0.013654 0.848853 0.080772 0.115 Uiso 1 1 calc R . . . .
C24 C 0.1070(5) 0.8344(5) -0.0029(2) 0.101(3) Uani 1 1 d . . . . .
H24 H 0.141213 0.831752 -0.023333 0.121 Uiso 1 1 calc R . . . .
C22 C 0.0076(4) 0.8926(6) 0.0276(3) 0.114(4) Uani 1 1 d . . . . .
H22 H -0.029689 0.929860 0.028332 0.137 Uiso 1 1 calc R . . . .
N2 N -0.0497(2) 0.7459(2) 0.12212(12) 0.0310(10) Uani 1 1 d . . . . .
N1 N -0.0319(2) 0.6623(2) 0.17053(12) 0.0293(10) Uani 1 1 d . . . . .
H1 H -0.042033 0.634207 0.190432 0.035 Uiso 1 1 calc R . . . .
C1S C 0.0594(6) 0.7961(7) 0.4069(4) 0.118(4) Uani 1 1 d . . . . .
C2S C 0.0641(8) 0.8380(7) 0.4435(4) 0.173(6) Uani 1 1 d . . . . .
H2SA H 0.033574 0.883231 0.441899 0.259 Uiso 1 1 calc GR . . . .
H2SB H 0.115303 0.852408 0.448220 0.259 Uiso 1 1 calc GR . . . .
H2SC H 0.046582 0.806168 0.464343 0.259 Uiso 1 1 calc GR . . . .
N1S N 0.0537(6) 0.7623(7) 0.3784(4) 0.149(4) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C30 0.035(3) 0.034(3) 0.050(4) -0.013(3) -0.004(3) 0.000(3)
C35 0.072(5) 0.033(4) 0.066(5) 0.005(3) -0.028(4) -0.007(4)
C29 0.039(3) 0.043(4) 0.044(4) -0.004(3) -0.011(3) -0.011(3)
C28 0.043(4) 0.035(3) 0.052(4) -0.011(3) -0.003(3) -0.003(3)
C31 0.039(3) 0.040(4) 0.058(4) -0.014(3) 0.003(3) 0.002(3)
C54 0.045(4) 0.056(4) 0.053(4) -0.014(3) 0.005(3) 0.007(3)
C57 0.051(4) 0.114(7) 0.078(6) 0.036(5) 0.016(4) -0.029(5)
C55 0.030(9) 0.070(9) 0.051(8) -0.001(7) 0.009(6) 0.002(6)
C56 0.049(7) 0.104(10) 0.036(7) -0.005(7) 0.001(6) -0.023(7)
O8 0.038(5) 0.059(6) 0.054(6) 0.023(5) 0.014(4) -0.007(4)
C48 0.047(4) 0.052(4) 0.051(4) -0.007(3) 0.008(3) -0.019(3)
C36 0.079(5) 0.027(3) 0.065(5) 0.001(3) -0.050(4) -0.007(3)
C37 0.080(5) 0.041(4) 0.086(6) -0.013(4) -0.021(5) -0.024(4)
C34 0.085(6) 0.023(3) 0.071(5) -0.004(3) -0.033(4) -0.007(4)
C27 0.048(4) 0.042(4) 0.059(4) -0.005(3) 0.015(3) -0.009(3)
C49 0.039(4) 0.076(5) 0.051(4) -0.009(4) 0.000(3) -0.013(4)
C26 0.057(4) 0.038(4) 0.059(4) 0.002(3) 0.000(4) -0.002(3)
C51 0.062(5) 0.074(5) 0.086(6) -0.010(5) 0.027(4) 0.004(4)
C33 0.095(6) 0.041(4) 0.082(6) -0.009(4) -0.023(5) -0.023(4)
C53 0.105(6) 0.042(4) 0.054(4) -0.009(4) -0.005(5) -0.006(4)
C50 0.039(4) 0.098(6) 0.087(6) -0.009(5) 0.012(4) 0.011(4)
C52 0.094(6) 0.061(5) 0.068(5) -0.008(4) 0.018(5) -0.002(5)
C32 0.097(6) 0.027(4) 0.081(6) -0.006(4) -0.054(5) -0.015(4)
C38 0.076(6) 0.077(6) 0.110(7) 0.025(5) 0.018(5) 0.010(5)
C47 0.100(7) 0.072(6) 0.114(8) -0.007(5) -0.046(6) -0.020(5)
C59 0.053(4) 0.043(4) 0.092(6) 0.013(4) -0.033(4) -0.006(3)
C58 0.044(4) 0.067(5) 0.116(7) 0.039(5) -0.001(5) -0.011(4)
O7 0.038(2) 0.047(2) 0.051(3) -0.004(2) 0.008(2) 0.004(2)
O3 0.032(2) 0.063(3) 0.055(3) -0.005(2) 0.000(2) -0.006(2)
O1 0.086(4) 0.090(4) 0.086(4) 0.035(3) 0.027(3) 0.044(3)
O9 0.056(3) 0.096(4) 0.069(3) 0.007(3) 0.011(3) -0.046(3)
O10 0.056(3) 0.059(3) 0.072(3) 0.003(3) -0.013(3) -0.009(2)
O6 0.073(3) 0.052(3) 0.067(3) -0.001(2) -0.001(3) -0.001(3)
O5 0.076(3) 0.071(3) 0.068(3) -0.007(3) 0.021(3) 0.000(3)
O4 0.026(2) 0.062(3) 0.083(3) -0.004(3) 0.008(2) 0.002(2)
C39 0.085(6) 0.084(6) 0.085(6) 0.027(5) 0.012(5) 0.043(5)
C40 0.134(11) 0.109(10) 0.082(9) 0.035(8) 0.024(8) 0.066(9)
C45 0.095(8) 0.074(8) 0.152(11) 0.060(8) -0.019(8) -0.005(7)
C46 0.126(10) 0.079(8) 0.105(9) 0.020(7) -0.043(8) -0.005(7)
C41 0.115(9) 0.129(10) 0.089(8) 0.021(8) 0.050(7) 0.035(9)
C43 0.097(8) 0.151(11) 0.086(8) 0.049(8) 0.004(7) 0.022(8)
C44 0.092(8) 0.164(12) 0.117(10) 0.024(9) -0.034(7) 0.059(8)
C42 0.063(7) 0.154(11) 0.092(8) 0.035(8) 0.006(6) 0.052(7)
O2 0.131(6) 0.068(4) 0.109(5) -0.019(4) -0.067(4) 0.010(4)
C40A 0.14(2) 0.13(2) 0.10(2) 0.03(2) 0.01(2) 0.02(2)
C45A 0.111(19) 0.109(19) 0.125(19) 0.058(18) -0.046(18) 0.006(18)
C46A 0.14(2) 0.10(2) 0.15(2) 0.09(2) -0.03(2) 0.00(2)
C41A 0.116(19) 0.124(19) 0.088(18) 0.031(19) 0.011(18) 0.032(19)
C43A 0.105(18) 0.17(2) 0.127(19) 0.046(19) -0.010(18) 0.030(19)
C44A 0.098(18) 0.134(19) 0.108(19) 0.049(19) -0.020(17) 0.001(18)
C42A 0.085(16) 0.147(18) 0.097(16) 0.038(17) 0.002(16) 0.041(17)
C55A 0.053(18) 0.098(17) 0.059(14) -0.004(13) 0.018(14) 0.002(12)
C56A 0.047(10) 0.113(14) 0.029(9) 0.038(9) -0.002(8) 0.003(11)
O8A 0.057(9) 0.067(8) 0.017(6) 0.019(6) 0.005(6) -0.001(6)
C8 0.026(3) 0.022(3) 0.036(3) -0.004(2) -0.001(2) -0.004(2)
C1 0.026(3) 0.033(3) 0.038(3) 0.001(3) 0.000(3) 0.000(3)
C13 0.022(3) 0.034(3) 0.031(3) -0.008(3) 0.001(2) 0.002(2)
C11 0.021(3) 0.040(3) 0.042(3) -0.007(3) 0.009(3) -0.002(2)
C12 0.031(3) 0.028(3) 0.039(3) -0.013(3) 0.004(3) -0.005(2)
C20 0.027(3) 0.033(3) 0.040(3) -0.007(3) 0.005(3) -0.011(3)
C14 0.019(3) 0.029(3) 0.043(3) -0.004(3) 0.000(2) -0.005(2)
C2 0.022(3) 0.051(4) 0.026(3) 0.003(3) 0.001(2) 0.001(3)
C15 0.023(3) 0.028(3) 0.056(4) 0.003(3) -0.002(3) -0.004(2)
C9 0.024(3) 0.021(3) 0.036(3) -0.009(2) 0.004(2) -0.004(2)
C19 0.029(3) 0.032(3) 0.059(4) -0.006(3) -0.002(3) 0.000(3)
C17 0.036(3) 0.037(4) 0.069(5) 0.010(3) -0.013(3) -0.009(3)
C18 0.033(3) 0.030(3) 0.075(5) -0.004(3) -0.012(3) -0.002(3)
C10 0.025(3) 0.035(3) 0.045(4) -0.008(3) -0.005(3) 0.002(2)
C16 0.038(3) 0.041(4) 0.053(4) -0.003(3) 0.000(3) -0.012(3)
C3 0.033(4) 0.072(5) 0.083(5) 0.017(4) 0.014(3) 0.001(4)
C25 0.120(7) 0.083(6) 0.077(6) 0.036(5) 0.051(5) 0.055(5)
C23 0.068(5) 0.083(6) 0.054(5) 0.026(4) 0.000(4) -0.010(4)
C7 0.037(4) 0.058(4) 0.068(5) -0.003(4) 0.010(3) 0.010(3)
C6 0.050(5) 0.096(6) 0.096(6) -0.003(5) 0.020(5) 0.032(5)
C4 0.034(4) 0.117(7) 0.085(6) 0.022(5) 0.013(4) -0.007(5)
C5 0.026(4) 0.132(8) 0.064(5) 0.005(5) 0.015(3) 0.016(5)
C21 0.067(5) 0.120(7) 0.100(7) 0.069(6) 0.046(5) 0.039(5)
C24 0.126(8) 0.101(7) 0.075(6) 0.038(5) 0.066(6) 0.044(6)
C22 0.060(5) 0.155(9) 0.127(8) 0.092(7) 0.041(5) 0.046(6)
N2 0.027(2) 0.033(3) 0.033(3) 0.000(2) 0.002(2) -0.001(2)
N1 0.024(2) 0.032(2) 0.031(2) 0.002(2) 0.007(2) -0.001(2)
C1S 0.070(6) 0.113(9) 0.170(13) -0.023(9) 0.001(8) 0.008(6)
C2S 0.208(15) 0.135(11) 0.177(13) -0.036(10) -0.088(12) 0.042(10)
N1S 0.116(8) 0.154(10) 0.176(11) -0.041(8) 0.042(8) -0.021(7)
_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
C30 C29 1.388(8) . ?
C30 C31 1.389(8) . ?
C30 O7 1.369(7) . ?
C45Ab C46A 1.51(2) . ?
C40Ab C41A 1.46(2) . ?
C45Ab C44A 1.51(2) . ?
C43Ab C44A 1.50(2) . ?
C43Ab C42A 1.46(2) . ?
C41Ab C42A 1.51(2) . ?
C56Ab O8A 1.453(14) . ?
C55Ab O8A 1.430(17) . ?
C35 C36 1.416(10) . ?
C35 C34 1.410(10) . ?
C29 C28 1.383(8) . ?
C28 C27 1.386(8) . ?
C28 O3 1.389(7) . ?
C31 C26 1.398(8) . ?
C54 C55 1.499(13) . ?
C54 O7 1.432(7) . ?
C54 C55A 1.472(15) . ?
C57 C56 1.583(13) . ?
C57 O9 1.434(8) . ?
C57 C56A 1.487(16) . ?
C48 C49 1.486(8) . ?
C48 O3 1.422(7) . ?
C36 C37 1.375(9) . ?
C36 O10 1.341(8) . ?
C37 C32 1.372(10) . ?
C34 C33 1.391(10) . ?
C34 O6 1.380(8) . ?
C27 C26 1.380(8) . ?
C49 O4 1.407(7) . ?
C26 C38 1.516(9) . ?
C51 C50 1.488(10) . ?
C51 O5 1.368(8) . ?
C33 C32 1.409(11) . ?
C53 C52 1.508(10) . ?
C53 O6 1.426(8) . ?
C50 O4 1.400(8) . ?
C52 O5 1.401(8) . ?
C32 C47 1.539(10) . ?
C38 O1 1.350(9) . ?
C47 O2 1.424(10) . ?
C59 C58 1.498(10) . ?
C59 O10 1.401(7) . ?
C58 O9 1.394(9) . ?
O1 C39 1.436(8) . ?
C39 C40 1.503(14) . ?
C39 C40A 1.49(2) . ?
O2 C46A 1.45(2) . ?
C40A C41 1.462(15) . ?
C45A C46 1.498(13) . ?
C45A C44 1.534(16) . ?
C46A O2 1.411(12) . ?
C41A C42 1.515(16) . ?
C43A C44 1.481(15) . ?
C43A C42 1.488(15) . ?
C55A O8 1.398(13) . ?
C56A O8 1.380(12) . ?
C8 C13 1.407(7) . ?
C8 C9 1.408(7) . ?
C8 N1 1.391(6) . ?
C1 C2 1.478(7) . ?
C1 N2 1.309(6) . ?
C1 N1 1.370(6) . ?
C13 C12 1.404(7) . ?
C13 N2 1.396(6) . ?
C11 C12 1.386(7) . ?
C11 C10 1.391(7) . ?
C12 C20 1.487(8) . ?
C20 C25 1.344(8) . ?
C20 C21 1.360(9) . ?
C14 C15 1.397(7) . ?
C14 C9 1.478(7) . ?
C14 C19 1.405(7) . ?
C2 C3 1.369(8) . ?
C2 C7 1.371(8) . ?
C15 C16 1.388(8) . ?
C9 C10 1.388(7) . ?
C19 C18 1.380(8) . ?
C17 C18 1.379(9) . ?
C17 C16 1.374(8) . ?
C3 C4 1.385(9) . ?
C25 C24 1.372(10) . ?
C23 C24 1.330(10) . ?
C23 C22 1.350(10) . ?
C7 C6 1.388(9) . ?
C6 C5 1.360(11) . ?
C4 C5 1.365(11) . ?
C21 C22 1.397(10) . ?
C1S C2S 1.455(16) . ?
C1S N1S 1.148(14) . ?
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
C29 C30 C31 120.4(6) . . ?
O7 C30 C29 116.0(5) . . ?
O8Ab C55Ab C54 107.1(13) . . ?
O7 C30 C31 123.7(5) . . ?
O8Ab C56Ab C57 97.4(10) . . ?
C41Ab C40Ab C39 114(2) . . ?
C43Ab C44Ab C45A 114(2) . . ?
C34 C35 C36 121.2(7) . . ?
C28 C29 C30 119.9(6) . . ?
C29 C28 C27 120.4(6) . . ?
C43Ab C42Ab C41A 117(2) . . ?
C42Ab C43Ab C44A 115(2) . . ?
C46Ab C45Ab C44A 111(2) . . ?
C29 C28 O3 115.9(5) . . ?
C40Ab C41Ab C42A 117(2) . . ?
C27 C28 O3 123.8(6) . . ?
C55Ab O8Ab C56A 105.7(11) . . ?
C30 C31 C26 119.0(6) . . ?
O7 C54 C55 105.3(10) . . ?
O7 C54 C55A 114.4(17) . . ?
O9 C57 C56 109.9(7) . . ?
O9 C57 C56A 108.8(8) . . ?
O3 C48 C49 110.2(5) . . ?
C37 C36 C35 117.4(8) . . ?
O10 C36 C35 125.8(6) . . ?
O10 C36 C37 116.7(7) . . ?
C32 C37 C36 122.5(8) . . ?
C33 C34 C35 119.3(8) . . ?
O6 C34 C35 115.7(6) . . ?
O6 C34 C33 125.0(8) . . ?
C26 C27 C28 119.7(6) . . ?
O4 C49 C48 109.6(5) . . ?
C31 C26 C38 120.5(6) . . ?
C27 C26 C31 120.6(6) . . ?
C27 C26 C38 118.9(6) . . ?
O5 C51 C50 114.2(7) . . ?
C34 C33 C32 119.2(8) . . ?
O6 C53 C52 108.6(6) . . ?
O4 C50 C51 110.5(6) . . ?
O5 C52 C53 114.1(6) . . ?
C37 C32 C33 120.3(7) . . ?
C37 C32 C47 124.3(8) . . ?
C33 C32 C47 115.3(8) . . ?
O1 C38 C26 113.2(6) . . ?
O2 C47 C32 111.2(8) . . ?
O10 C59 C58 108.4(6) . . ?
O9 C58 C59 108.8(6) . . ?
C30 O7 C54 118.0(5) . . ?
C28 O3 C48 117.5(5) . . ?
C38 O1 C39 113.7(6) . . ?
C58 O9 C57 111.4(6) . . ?
C36 O10 C59 120.5(5) . . ?
C34 O6 C53 117.9(6) . . ?
C51 O5 C52 113.4(6) . . ?
C50 O4 C49 114.7(5) . . ?
O1 C39 C40 107.7(8) . . ?
O1 C39 C40A 121.7(16) . . ?
C47 O2 C46A 122(3) . . ?
O2 C46Ab C45A 113(2) . . ?
C46A O2 C47 115.8(8) . . ?
C41A C40A C39 109.0(10) . . ?
C46A C45A C44 106.8(10) . . ?
O2 C46A C45 114.7(10) . . ?
C40A C41A C42 117.0(10) . . ?
C44A C43A C42 113.9(10) . . ?
C43A C44A C45 111.6(11) . . ?
C43A C42A C41 110.4(9) . . ?
O8A C55A C54 116.0(10) . . ?
O8A C56A C57 110.0(9) . . ?
C56A O8A C55 116.1(12) . . ?
C13 C8 C9 123.9(5) . . ?
N1 C8 C13 104.4(4) . . ?
N1 C8 C9 131.7(5) . . ?
N2 C1 C2 124.6(5) . . ?
N2 C1 N1 113.1(4) . . ?
N1 C1 C2 122.2(5) . . ?
C12 C13 C8 120.5(5) . . ?
N2 C13 C8 110.2(4) . . ?
N2 C13 C12 129.3(5) . . ?
C12 C11 C10 123.5(5) . . ?
C13 C12 C20 123.1(5) . . ?
C11 C12 C13 115.5(5) . . ?
C11 C12 C20 121.4(5) . . ?
C25 C20 C12 122.8(5) . . ?
C25 C20 C21 114.0(6) . . ?
C21 C20 C12 123.1(5) . . ?
C15 C14 C9 122.5(5) . . ?
C15 C14 C19 117.4(5) . . ?
C19 C14 C9 120.1(5) . . ?
C3 C2 C1 122.5(5) . . ?
C3 C2 C7 119.1(5) . . ?
C7 C2 C1 118.4(5) . . ?
C16 C15 C14 120.4(5) . . ?
C8 C9 C14 124.0(4) . . ?
C10 C9 C8 114.1(5) . . ?
C10 C9 C14 121.9(5) . . ?
C18 C19 C14 121.3(6) . . ?
C16 C17 C18 119.0(6) . . ?
C17 C18 C19 120.5(6) . . ?
C9 C10 C11 122.6(5) . . ?
C17 C16 C15 121.3(6) . . ?
C2 C3 C4 120.4(7) . . ?
C20 C25 C24 124.1(7) . . ?
C24 C23 C22 117.9(7) . . ?
C2 C7 C6 120.1(7) . . ?
C5 C6 C7 120.7(7) . . ?
C5 C4 C3 120.5(7) . . ?
C6 C5 C4 119.3(6) . . ?
C20 C21 C22 123.0(7) . . ?
C23 C24 C25 120.9(7) . . ?
C23 C22 C21 119.9(8) . . ?
C1 N2 C13 105.1(4) . . ?
C1 N1 C8 107.2(4) . . ?
N1S C1S C2S 178.1(14) . . ?
_iucr_refine_instructions_details
;
TITL KZ74a in Pbca #61
kz74a.res created by SHELXL-2016/4 at 13:50:59 on 16-Feb-2017
REM reset to Pbca #61
CELL 0.71073 17.8191 17.4575 34.3374 90 90 90
ZERR 8 0.003 0.003 0.005 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 488 568 24 80
SIMU C57 C55 C56 O8 C55A C56A O8A
SIMU C40 C45 C46 C41 C43 C44 C42 C40A C45A C46A C41A C43A C44A C42A
L.S. 20
PLAN 20
TEMP 0
BIND C45A C46A
BIND C46A O2
FREE C46A C47
BOND
fmap 2
acta
OMIT 1 1 1
REM
REM
REM
WGHT 0.049300 32.720402
FVAR 0.06164 0.60054 0.81795
C30 1 0.071612 0.818134 0.211523 11.00000 0.03499 0.03366 =
0.05009 -0.01307 -0.00385 -0.00032
C35 1 0.030663 0.483807 0.110975 11.00000 0.07215 0.03261 =
0.06600 0.00490 -0.02768 -0.00667
AFIX 43
H35 2 0.054428 0.453685 0.129602 11.00000 -1.20000
AFIX 0
C29 1 0.143364 0.796273 0.200388 11.00000 0.03865 0.04322 =
0.04358 -0.00412 -0.01061 -0.01051
AFIX 43
H29 2 0.168001 0.757262 0.213681 11.00000 -1.20000
AFIX 0
C28 1 0.178143 0.832614 0.169490 11.00000 0.04286 0.03523 =
0.05184 -0.01131 -0.00259 -0.00324
C31 1 0.034906 0.877065 0.192163 11.00000 0.03887 0.03967 =
0.05812 -0.01350 0.00269 0.00212
AFIX 43
H31 2 -0.013527 0.891155 0.199270 11.00000 -1.20000
AFIX 0
SAME 0.02 0.02 C54 C57 C55A C56A O8A
C54 1 -0.033945 0.797019 0.253650 11.00000 0.04529 0.05561 =
0.05269 -0.01424 0.00547 0.00689
PART 1
AFIX 23
H54A 2 -0.069055 0.786954 0.232677 21.00000 -1.20000
H54B 2 -0.037578 0.850595 0.260896 21.00000 -1.20000
AFIX 23
PART 0
PART 2
H54C 2 -0.064948 0.801218 0.230528 -21.00000 -1.20000
H54D 2 -0.033469 0.846751 0.266246 -21.00000 -1.20000
AFIX 0
PART 0
C57 1 -0.138873 0.560418 0.260377 11.00000 0.05051 0.11436 =
0.07841 0.03601 0.01604 -0.02913
PART 1
AFIX 23
H57A 2 -0.121779 0.531674 0.282866 21.00000 -1.20000
H57B 2 -0.190460 0.546017 0.255109 21.00000 -1.20000
AFIX 23
PART 0
PART 2
H57C 2 -0.151606 0.513896 0.274339 -21.00000 -1.20000
H57D 2 -0.185070 0.584533 0.251835 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C55 1 -0.050049 0.746495 0.287939 21.00000 0.03004 0.06975 =
0.05084 -0.00120 0.00930 0.00247
AFIX 23
H55A 2 -0.008243 0.750233 0.305932 21.00000 -1.20000
H55B 2 -0.094081 0.766241 0.301172 21.00000 -1.20000
AFIX 0
C56 1 -0.134496 0.649258 0.269326 21.00000 0.04915 0.10403 =
0.03601 -0.00504 0.00100 -0.02343
AFIX 23
H56A 2 -0.149581 0.678030 0.246462 21.00000 -1.20000
H56B 2 -0.168613 0.661891 0.290381 21.00000 -1.20000
AFIX 0
O8 4 -0.062196 0.669094 0.279647 21.00000 0.03836 0.05933 =
0.05389 0.02331 0.01384 -0.00691
PART 0
C48 1 0.281062 0.832421 0.124251 11.00000 0.04742 0.05239 =
0.05072 -0.00678 0.00783 -0.01866
AFIX 23
H48A 2 0.296474 0.885282 0.127683 11.00000 -1.20000
H48B 2 0.244192 0.830653 0.103488 11.00000 -1.20000
AFIX 0
C36 1 -0.045558 0.504284 0.116280 11.00000 0.07857 0.02688 =
0.06479 0.00088 -0.04969 -0.00746
C37 1 -0.079448 0.545838 0.087151 11.00000 0.07954 0.04132 =
0.08603 -0.01315 -0.02076 -0.02424
AFIX 43
H37 2 -0.129865 0.558620 0.089754 11.00000 -1.20000
AFIX 0
C34 1 0.071178 0.508265 0.077959 11.00000 0.08486 0.02327 =
0.07108 -0.00395 -0.03261 -0.00725
C27 1 0.142864 0.892630 0.150464 11.00000 0.04810 0.04200 =
0.05856 -0.00532 0.01481 -0.00889
AFIX 43
H27 2 0.166939 0.917798 0.130124 11.00000 -1.20000
AFIX 0
C49 1 0.347129 0.785029 0.113465 11.00000 0.03886 0.07631 =
0.05105 -0.00920 0.00020 -0.01294
AFIX 23
H49A 2 0.377724 0.812317 0.094664 11.00000 -1.20000
H49B 2 0.377499 0.775262 0.136377 11.00000 -1.20000
AFIX 0
C26 1 0.071847 0.914907 0.161823 11.00000 0.05738 0.03810 =
0.05860 0.00192 0.00018 -0.00163
C51 1 0.352465 0.601357 0.062878 11.00000 0.06172 0.07440 =
0.08588 -0.01014 0.02702 0.00385
AFIX 23
H51A 2 0.326412 0.624775 0.041119 11.00000 -1.20000
H51B 2 0.395224 0.573691 0.052495 11.00000 -1.20000
AFIX 0
C33 1 0.034609 0.550471 0.049336 11.00000 0.09549 0.04147 =
0.08215 -0.00861 -0.02326 -0.02347
AFIX 43
H33 2 0.060209 0.566176 0.027125 11.00000 -1.20000
AFIX 0
C53 1 0.190637 0.515727 0.045633 11.00000 0.10509 0.04237 =
0.05407 -0.00869 -0.00528 -0.00597
AFIX 23
H53A 2 0.183402 0.570483 0.042645 11.00000 -1.20000
H53B 2 0.175883 0.490858 0.021560 11.00000 -1.20000
AFIX 0
C50 1 0.380301 0.663002 0.089087 11.00000 0.03947 0.09795 =
0.08683 -0.00926 0.01199 0.01073
AFIX 23
H50A 2 0.398566 0.640574 0.113132 11.00000 -1.20000
H50B 2 0.421726 0.689586 0.076709 11.00000 -1.20000
AFIX 0
C52 1 0.271897 0.498807 0.054345 11.00000 0.09435 0.06062 =
0.06777 -0.00836 0.01813 -0.00208
AFIX 23
H52A 2 0.275591 0.447498 0.065016 11.00000 -1.20000
H52B 2 0.299903 0.499649 0.030126 11.00000 -1.20000
AFIX 0
C32 1 -0.041718 0.569168 0.054386 11.00000 0.09747 0.02656 =
0.08082 -0.00564 -0.05438 -0.01458
C38 1 0.034822 0.981719 0.141170 11.00000 0.07611 0.07678 =
0.10952 0.02524 0.01833 0.01034
AFIX 23
H38A 2 0.057086 1.029062 0.150399 11.00000 -1.20000
H38B 2 0.044822 0.977821 0.113473 11.00000 -1.20000
AFIX 0
C47 1 -0.076316 0.618640 0.021913 11.00000 0.10022 0.07167 =
0.11401 -0.00710 -0.04614 -0.02026
AFIX 23
H47A 2 -0.055440 0.669897 0.023162 11.00000 -1.20000
H47B 2 -0.063527 0.596966 -0.003237 11.00000 -1.20000
AFIX 0
C59 1 -0.055634 0.452367 0.180175 11.00000 0.05279 0.04316 =
0.09241 0.01310 -0.03251 -0.00559
AFIX 23
H59A 2 -0.005752 0.472636 0.184838 11.00000 -1.20000
H59B 2 -0.051489 0.397655 0.175742 11.00000 -1.20000
AFIX 0
C58 1 -0.104932 0.467502 0.214681 11.00000 0.04408 0.06711 =
0.11623 0.03862 -0.00051 -0.01096
AFIX 23
H58A 2 -0.157173 0.460710 0.207530 11.00000 -1.20000
H58B 2 -0.093184 0.431757 0.235432 11.00000 -1.20000
AFIX 0
O7 4 0.041023 0.778369 0.242002 11.00000 0.03789 0.04726 =
0.05115 -0.00384 0.00840 0.00433
O3 4 0.248499 0.804744 0.159351 11.00000 0.03211 0.06284 =
0.05542 -0.00542 -0.00022 -0.00561
O1 4 -0.040084 0.984718 0.146795 11.00000 0.08614 0.08969 =
0.08650 0.03458 0.02699 0.04406
O9 4 -0.092923 0.542392 0.227352 11.00000 0.05599 0.09578 =
0.06860 0.00673 0.01144 -0.04621
O10 4 -0.087588 0.487972 0.147578 11.00000 0.05644 0.05884 =
0.07235 0.00332 -0.01262 -0.00862
O6 4 0.146012 0.487896 0.077087 11.00000 0.07250 0.05164 =
0.06709 -0.00053 -0.00077 -0.00103
O5 4 0.305225 0.550204 0.080457 11.00000 0.07638 0.07057 =
0.06772 -0.00733 0.02131 0.00043
O4 4 0.322802 0.715193 0.097394 11.00000 0.02568 0.06179 =
0.08253 -0.00397 0.00766 0.00191
SAME 0.02 0.02 C39 C40A C45A > C42A O2
C39 1 -0.074986 1.050947 0.129884 11.00000 0.08497 0.08418 =
0.08511 0.02661 0.01189 0.04259
PART 1
AFIX 23
H39A 2 -0.049529 1.065077 0.105970 31.00000 -1.20000
H39B 2 -0.072314 1.093862 0.147774 31.00000 -1.20000
AFIX 23
PART 0
PART 2
H39C 2 -0.036877 1.076815 0.114589 -31.00000 -1.20000
H39D 2 -0.087777 1.085021 0.151188 -31.00000 -1.20000
AFIX 0
PART 0
PART 1
C40 1 -0.155517 1.031118 0.121593 31.00000 0.13423 0.10950 =
0.08177 0.03523 0.02403 0.06619
AFIX 23
H40A 2 -0.177402 1.005488 0.143936 31.00000 -1.20000
H40B 2 -0.183968 1.077467 0.116617 31.00000 -1.20000
AFIX 0
C45 1 -0.194028 0.757305 0.029742 31.00000 0.09472 0.07404 =
0.15246 0.05951 -0.01895 -0.00487
AFIX 23
H45A 2 -0.233293 0.753609 0.010267 31.00000 -1.20000
H45B 2 -0.147933 0.773005 0.017010 31.00000 -1.20000
AFIX 0
C46 1 -0.183415 0.681773 0.049716 31.00000 0.12603 0.07911 =
0.10546 0.02031 -0.04264 -0.00542
AFIX 23
H46A 2 -0.148881 0.688757 0.071262 31.00000 -1.20000
H46B 2 -0.231192 0.665710 0.060514 31.00000 -1.20000
AFIX 0
C41 1 -0.158597 0.980865 0.087569 31.00000 0.11458 0.12881 =
0.08882 0.02083 0.05030 0.03532
AFIX 23
H41A 2 -0.128234 0.936003 0.093002 31.00000 -1.20000
H41B 2 -0.135416 1.007485 0.065886 31.00000 -1.20000
AFIX 0
C43 1 -0.228449 0.892530 0.044831 31.00000 0.09684 0.15137 =
0.08587 0.04890 0.00365 0.02223
AFIX 23
H43A 2 -0.273833 0.891609 0.029239 31.00000 -1.20000
H43B 2 -0.186975 0.904956 0.027660 31.00000 -1.20000
AFIX 0
C44 1 -0.215933 0.815232 0.061349 31.00000 0.09181 0.16446 =
0.11701 0.02423 -0.03404 0.05888
AFIX 23
H44A 2 -0.261383 0.798042 0.074207 31.00000 -1.20000
H44B 2 -0.176398 0.817767 0.080725 31.00000 -1.20000
AFIX 0
C42 1 -0.235487 0.953912 0.074688 31.00000 0.06251 0.15405 =
0.09166 0.03469 0.00553 0.05230
AFIX 23
H42A 2 -0.262992 0.934523 0.096984 31.00000 -1.20000
H42B 2 -0.263344 0.996696 0.063922 31.00000 -1.20000
AFIX 0
PART 0
O2 4 -0.155834 0.622674 0.025592 11.00000 0.13123 0.06760 =
0.10916 -0.01943 -0.06690 0.00977
PART 2
C40A 1 -0.142945 1.044582 0.104800 -31.00000 0.13506 0.12501 =
0.09782 0.02511 0.00732 0.01805
AFIX 23
H40C 2 -0.174391 1.089164 0.109040 -31.00000 -1.20000
H40D 2 -0.127476 1.044868 0.077716 -31.00000 -1.20000
AFIX 0
C45A 1 -0.222507 0.736321 0.049952 -31.00000 0.11102 0.10923 =
0.12495 0.05832 -0.04601 0.00586
AFIX 23
H45C 2 -0.182674 0.737337 0.069199 -31.00000 -1.20000
H45D 2 -0.265690 0.711364 0.061564 -31.00000 -1.20000
AFIX 0
C46A 1 -0.197007 0.691097 0.015050 -31.00000 0.13917 0.10420 =
0.15467 0.09432 -0.02697 -0.00368
AFIX 23
H46C 2 -0.240522 0.676666 -0.000255 -31.00000 -1.20000
H46D 2 -0.165358 0.723295 -0.001083 -31.00000 -1.20000
AFIX 0
C41A 1 -0.187251 0.975653 0.112124 -31.00000 0.11597 0.12433 =
0.08804 0.03090 0.01081 0.03238
AFIX 23
H41C 2 -0.239658 0.990412 0.113571 -31.00000 -1.20000
H41D 2 -0.173231 0.955754 0.137476 -31.00000 -1.20000
AFIX 0
C43A 1 -0.248791 0.870506 0.073156 -31.00000 0.10480 0.17478 =
0.12673 0.04585 -0.00966 0.03018
AFIX 23
H43C 2 -0.287940 0.907677 0.067852 -31.00000 -1.20000
H43D 2 -0.264284 0.841033 0.095714 -31.00000 -1.20000
AFIX 0
C44A 1 -0.243073 0.817306 0.038957 -31.00000 0.09837 0.13427 =
0.10826 0.04949 -0.01959 0.00106
AFIX 23
H44C 2 -0.205592 0.836977 0.021078 -31.00000 -1.20000
H44D 2 -0.290821 0.816696 0.025395 -31.00000 -1.20000
AFIX 0
C42A 1 -0.180309 0.911688 0.082959 -31.00000 0.08503 0.14678 =
0.09704 0.03797 0.00170 0.04068
AFIX 23
H42C 2 -0.159671 0.932810 0.059127 -31.00000 -1.20000
H42D 2 -0.144240 0.874963 0.092910 -31.00000 -1.20000
AFIX 0
C55A 1 -0.068533 0.741143 0.280271 -21.00000 0.05277 0.09801 =
0.05914 -0.00365 0.01846 0.00198
AFIX 23
H55C 2 -0.034702 0.729537 0.301600 -21.00000 -1.20000
H55D 2 -0.114750 0.761590 0.290982 -21.00000 -1.20000
AFIX 0
C56A 1 -0.096754 0.613240 0.286367 -21.00000 0.04723 0.11326 =
0.02862 0.03804 -0.00185 0.00271
AFIX 23
H56C 2 -0.126841 0.630673 0.308177 -21.00000 -1.20000
H56D 2 -0.050413 0.590748 0.295796 -21.00000 -1.20000
AFIX 0
O8A 4 -0.083548 0.673573 0.258031 -21.00000 0.05687 0.06721 =
0.01701 0.01868 0.00511 -0.00079
PART 0
C8 1 0.036621 0.666622 0.151256 11.00000 0.02614 0.02235 =
0.03634 -0.00437 -0.00136 -0.00447
C1 1 -0.080252 0.711054 0.151896 11.00000 0.02590 0.03276 =
0.03779 0.00057 -0.00006 -0.00024
C13 1 0.023675 0.718104 0.120464 11.00000 0.02234 0.03352 =
0.03108 -0.00831 0.00128 0.00178
C11 1 0.147522 0.695392 0.099112 11.00000 0.02064 0.03979 =
0.04158 -0.00749 0.00888 -0.00159
AFIX 43
H11 2 0.186006 0.702726 0.081202 11.00000 -1.20000
AFIX 0
C12 1 0.080411 0.733802 0.093240 11.00000 0.03113 0.02761 =
0.03885 -0.01348 0.00420 -0.00511
C20 1 0.069873 0.786555 0.059684 11.00000 0.02666 0.03255 =
0.03996 -0.00702 0.00517 -0.01073
C14 1 0.120101 0.577083 0.190735 11.00000 0.01920 0.02913 =
0.04332 -0.00380 0.00021 -0.00451
C2 1 -0.158159 0.723164 0.165343 11.00000 0.02180 0.05101 =
0.02606 0.00257 0.00128 0.00088
C15 1 0.087488 0.587436 0.227370 11.00000 0.02272 0.02752 =
0.05635 0.00315 -0.00245 -0.00393
AFIX 43
H15 2 0.056841 0.629629 0.231893 11.00000 -1.20000
AFIX 0
C9 1 0.105552 0.629365 0.157740 11.00000 0.02364 0.02104 =
0.03572 -0.00893 0.00426 -0.00450
C19 1 0.168452 0.514175 0.186031 11.00000 0.02890 0.03194 =
0.05888 -0.00552 -0.00232 0.00019
AFIX 43
H19 2 0.192033 0.506560 0.162181 11.00000 -1.20000
AFIX 0
C17 1 0.147617 0.473593 0.251806 11.00000 0.03639 0.03737 =
0.06860 0.00978 -0.01295 -0.00861
AFIX 43
H17 2 0.156381 0.439303 0.272028 11.00000 -1.20000
AFIX 0
C18 1 0.181650 0.463462 0.216093 11.00000 0.03320 0.03050 =
0.07495 -0.00366 -0.01198 -0.00198
AFIX 43
H18 2 0.213739 0.422137 0.212244 11.00000 -1.20000
AFIX 0
C10 1 0.160382 0.646433 0.130385 11.00000 0.02485 0.03550 =
0.04532 -0.00829 -0.00463 0.00203
AFIX 43
H10 2 0.207568 0.624284 0.133059 11.00000 -1.20000
AFIX 0
C16 1 0.100561 0.535117 0.257060 11.00000 0.03845 0.04062 =
0.05295 -0.00259 -0.00046 -0.01198
AFIX 43
H16 2 0.077002 0.541837 0.280985 11.00000 -1.20000
AFIX 0
C3 1 -0.203273 0.664243 0.177340 11.00000 0.03327 0.07205 =
0.08259 0.01662 0.01411 0.00113
AFIX 43
H3 2 -0.185615 0.614147 0.176385 11.00000 -1.20000
AFIX 0
C25 1 0.113549 0.784595 0.027806 11.00000 0.11980 0.08346 =
0.07687 0.03552 0.05075 0.05494
AFIX 43
H25 2 0.150552 0.747116 0.026485 11.00000 -1.20000
AFIX 0
C23 1 0.052468 0.886329 -0.003911 11.00000 0.06754 0.08292 =
0.05365 0.02622 -0.00016 -0.00984
AFIX 43
H23 2 0.045456 0.917349 -0.025627 11.00000 -1.20000
AFIX 0
C7 1 -0.185765 0.796475 0.165933 11.00000 0.03656 0.05773 =
0.06799 -0.00321 0.01046 0.01039
AFIX 43
H7 2 -0.155843 0.836985 0.157671 11.00000 -1.20000
AFIX 0
C6 1 -0.258338 0.810277 0.178852 11.00000 0.05048 0.09600 =
0.09563 -0.00296 0.02020 0.03183
AFIX 43
H6 2 -0.277074 0.859997 0.178705 11.00000 -1.20000
AFIX 0
C4 1 -0.275055 0.678831 0.190888 11.00000 0.03419 0.11660 =
0.08535 0.02240 0.01300 -0.00666
AFIX 43
H4 2 -0.304921 0.638551 0.199489 11.00000 -1.20000
AFIX 0
C5 1 -0.302312 0.751882 0.191716 11.00000 0.02619 0.13170 =
0.06371 0.00507 0.01483 0.01616
AFIX 43
H5 2 -0.350425 0.761601 0.200975 11.00000 -1.20000
AFIX 0
C21 1 0.017272 0.843001 0.059159 11.00000 0.06673 0.11963 =
0.09999 0.06879 0.04561 0.03896
AFIX 43
H21 2 -0.013654 0.848853 0.080772 11.00000 -1.20000
AFIX 0
C24 1 0.107018 0.834371 -0.002915 11.00000 0.12590 0.10063 =
0.07499 0.03759 0.06593 0.04433
AFIX 43
H24 2 0.141213 0.831752 -0.023333 11.00000 -1.20000
AFIX 0
C22 1 0.007590 0.892603 0.027614 11.00000 0.06003 0.15471 =
0.12714 0.09157 0.04057 0.04643
AFIX 43
H22 2 -0.029689 0.929860 0.028332 11.00000 -1.20000
AFIX 0
N2 3 -0.049691 0.745927 0.122123 11.00000 0.02678 0.03299 =
0.03332 0.00000 0.00203 -0.00088
N1 3 -0.031906 0.662275 0.170532 11.00000 0.02440 0.03204 =
0.03134 0.00248 0.00675 -0.00111
AFIX 43
H1 2 -0.042033 0.634207 0.190432 11.00000 -1.20000
AFIX 0
C1S 1 0.059410 0.796050 0.406926 11.00000 0.07011 0.11263 =
0.17029 -0.02347 0.00095 0.00836
C2S 1 0.064118 0.838036 0.443454 11.00000 0.20757 0.13459 =
0.17650 -0.03559 -0.08775 0.04194
AFIX 137
H2SA 2 0.033574 0.883231 0.441899 11.00000 -1.50000
H2SB 2 0.115303 0.852408 0.448220 11.00000 -1.50000
H2SC 2 0.046582 0.806168 0.464343 11.00000 -1.50000
AFIX 0
N1S 3 0.053704 0.762322 0.378381 11.00000 0.11615 0.15412 =
0.17583 -0.04051 0.04206 -0.02121
HKLF 4
REM KZ74a in Pbca #61
REM R1 = 0.1148 for 5437 Fo > 4sig(Fo) and 0.1513 for all 7663 data
REM 760 parameters refined using 292 restraints
END
WGHT 0.0492 32.7180
REM Highest difference peak 0.499, deepest hole -0.309, 1-sigma level 0.058
Q1 1 -0.1278 0.7080 0.0306 11.00000 0.05 0.50
Q2 1 -0.1983 0.6583 0.0009 11.00000 0.05 0.37
Q3 1 -0.1224 0.6551 0.0002 11.00000 0.05 0.37
Q4 1 -0.1869 0.8756 0.0514 11.00000 0.05 0.33
Q5 1 -0.0351 0.6371 0.0001 11.00000 0.05 0.31
Q6 1 -0.0218 0.5015 0.0885 11.00000 0.05 0.27
Q7 1 0.2784 0.6031 0.0657 11.00000 0.05 0.26
Q8 1 0.0339 0.5015 0.0688 11.00000 0.05 0.26
Q9 1 0.0069 0.8006 0.0410 11.00000 0.05 0.26
Q10 1 0.0005 0.9501 0.1195 11.00000 0.05 0.26
Q11 1 -0.1094 1.0234 0.0971 11.00000 0.05 0.25
Q12 1 0.3575 0.7181 0.1175 11.00000 0.05 0.25
Q13 1 0.0315 0.8198 0.1958 11.00000 0.05 0.24
Q14 1 -0.2127 0.7364 0.0007 11.00000 0.05 0.23
Q15 1 0.0815 0.8348 0.0592 11.00000 0.05 0.22
Q16 1 0.1097 0.5201 0.0552 11.00000 0.05 0.22
Q17 1 0.0954 0.4796 0.2529 11.00000 0.05 0.22
Q18 1 0.0363 0.6650 0.1225 11.00000 0.05 0.22
Q19 1 -0.0900 0.9950 0.1613 11.00000 0.05 0.21
Q20 1 0.0330 0.9196 0.1417 11.00000 0.05 0.21
REM The information below was added by Olex2.
REM
REM R1 = 0.1148 for 5437 Fo > 4sig(Fo) and 0.1513 for all 84536 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.50, deepest hole -0.31
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.1513
REM R1_gt = 0.1148
REM wR_ref = 0.2406
REM GOOF = 1.166
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 84536
REM Reflections_gt = 5437
REM Parameters = n/a
REM Hole = -0.31
REM Peak = 0.50
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'