# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# 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.
#
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data_mo_kt_l1np_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1933983'
loop_
_audit_author_name
_audit_author_address
'Juliane Maerz'
;Helmholtz Zentrum Dresden Rossendorf
Germany
;
_audit_update_record
;
2019-06-18 deposited with the CCDC. 2020-02-03 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_mo_kt_l1np_0m_a
;
PROBLEM: Atom C8 has ADP max/min Ratio ..... 6.7 prolat
RESPONSE: Such a relatively large anisotropic displacement has also been found in the U(IV)-analogue (CCDC 1848978), and therefore it is usual trend in this class of hexanitratoactinate(IV) compounds.
;
_vrf_PLAT213_mo_kt_l1np_0m_a_2
;
PROBLEM: Atom C2 has ADP max/min Ratio ..... 4.1 prolat
RESPONSE: Such a relatively large anisotropic displacement has also been found in the U(IV)-analogue (CCDC 1848978), and therefore it is usual trend in this class of hexanitratoactinate(IV) compounds.
;
_vrf_PLAT250_mo_kt_l1np_0m_a
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 5.5 Note
RESPONSE: Such a relatively large anisotropic displacement has also been found in the U(IV)-analogue (CCDC 1848978), and therefore it is usual trend in this class of hexanitratoactinate(IV) compounds.
;
_vrf_PLAT780_mo_kt_l1np_0m_a
;
PROBLEM: Coordinates do not Form a Properly Connected Set Please Do !
RESPONSE: This alert would arise from formation of hydrogen bond polymer like O11...H10...O10, where there are no actual covalent bonds.
;
# Added during the CSD deposition process: Tuesday 18 June 2019 05:06 AM
# end Validation Reply Form
_audit_creation_date 2018-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H46 N10 Np1 O22'
_chemical_formula_sum 'C28 H46 N10 Np1 O22'
_chemical_formula_weight 1113.76
_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'
Np Np -11.4937 4.1493 '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 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 18.1413(10)
_cell_length_b 10.9944(6)
_cell_length_c 21.6888(12)
_cell_angle_alpha 90
_cell_angle_beta 109.931(2)
_cell_angle_gamma 90
_cell_volume 4066.8(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2189
_cell_measurement_theta_min 2.1826
_cell_measurement_theta_max 22.4981
_cell_measurement_temperature 100(2)
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.652
_exptl_absorpt_correction_T_max 0.820
_exptl_absorpt_correction_T_min 0.739
_exptl_absorpt_correction_type 'Numerical Mu Calculated'
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_density_diffrn 1.814
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_size_max 0.157
_exptl_crystal_size_mid 0.098
_exptl_crystal_size_min 0.075
_diffrn_reflns_av_R_equivalents 0.0323
_diffrn_reflns_av_unetI/netI 0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 57492
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.728
_diffrn_reflns_theta_min 2.245
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method 'generic \f and \o scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3582
_reflns_number_total 4312
_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 ?
_computing_data_collection ?
_computing_data_reduction ?
_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 0.474
_refine_diff_density_min -0.523
_refine_diff_density_rms 0.074
_refine_ls_extinction_coef 0.00041(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 310
_refine_ls_number_reflns 4312
_refine_ls_number_restraints 5
_refine_ls_R_factor_all 0.0270
_refine_ls_R_factor_gt 0.0192
_refine_ls_restrained_S_all 1.071
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+13.0348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0394
_refine_ls_wR_factor_ref 0.0420
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
N5-C14 \\sim N5A-C14
with sigma of 0.02
N5-C11 \\sim N5A-C11
with sigma of 0.02
C7-C6 \\sim C7A-C6A
with sigma of 0.02
N4-C6 \\sim N4-C6A
with sigma of 0.04
N5-C7 \\sim N5A-C7A
with sigma of 0.04
3. Others
Sof(H5B)=Sof(H14C)=Sof(H14D)=Sof(H8B)=Sof(N5A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
Sof(N5)=Sof(H5A)=Sof(H14A)=Sof(H14B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C6)=
Sof(H6A)=Sof(H6B)=Sof(H8A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
C5(H5A), C5(H5B), C8(H8A), C8(H8B)
4.b Secondary CH2 refined with riding coordinates:
C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B), C10(H10A,H10B), C9(H9A,H9B), C14(H14A,
H14B), C14(H14C,H14D), C13(H13A,H13B), C12(H12A,H12B), C7(H7A,H7B), C6(H6A,
H6B), C7A(H7AA,H7AB), C6A(H6AA,H6AB)
;
_atom_sites_solution_hydrogens mixed
_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
Np1 Np 0.500000 1.000000 0.500000 0.01446(5) Uani 1 2 d S T P . .
O1 O 0.53627(10) 0.94613(18) 0.40177(8) 0.0282(4) Uani 1 1 d . . . . .
O2 O 0.61699(9) 0.88667(16) 0.49484(8) 0.0232(4) Uani 1 1 d . . . . .
O3 O 0.64998(13) 0.8706(3) 0.40773(10) 0.0573(7) Uani 1 1 d . . . . .
O4 O 0.38083(10) 0.97552(15) 0.39984(8) 0.0237(4) Uani 1 1 d . . . . .
O5 O 0.44205(9) 1.14538(16) 0.40713(8) 0.0237(4) Uani 1 1 d . . . . .
O6 O 0.32811(11) 1.12065(18) 0.33027(9) 0.0366(5) Uani 1 1 d . . . . .
O7 O 0.46705(9) 0.78413(16) 0.46540(9) 0.0246(4) Uani 1 1 d . . . . .
O9 O 0.37283(12) 0.68010(17) 0.48193(12) 0.0424(5) Uani 1 1 d . . . . .
O8 O 0.39850(10) 0.86588(16) 0.51808(9) 0.0254(4) Uani 1 1 d . . . . .
N3 N 0.41101(12) 0.77300(19) 0.48817(11) 0.0265(5) Uani 1 1 d . . . . .
N1 N 0.60293(13) 0.8999(2) 0.43366(11) 0.0318(5) Uani 1 1 d . . . . .
N2 N 0.38166(12) 1.0821(2) 0.37735(10) 0.0237(5) Uani 1 1 d . . . . .
O10 O 0.20299(12) 0.6878(2) 0.33287(12) 0.0457(6) Uani 1 1 d . . . . .
O11 O 0.59521(12) 0.3133(2) 0.33661(12) 0.0477(6) Uani 1 1 d . . . . .
N4 N 0.23190(11) 0.4994(2) 0.30571(11) 0.0278(5) Uani 1 1 d D . . . .
N5 N 0.5658(5) 0.4976(10) 0.3714(4) 0.036(2) Uani 0.516(15) 1 d D . . A 1
C4 C 0.19543(15) 0.3886(3) 0.27193(17) 0.0437(9) Uani 1 1 d . . . . .
H4A H 0.212959 0.316627 0.300644 0.052 Uiso 1 1 calc R . . . .
H4B H 0.208097 0.376151 0.231450 0.052 Uiso 1 1 calc R . . . .
C3 C 0.10669(16) 0.4112(4) 0.25566(15) 0.0546(11) Uani 1 1 d . . . . .
H3A H 0.078425 0.402023 0.208007 0.066 Uiso 1 1 calc R . . . .
H3B H 0.084667 0.352677 0.279441 0.066 Uiso 1 1 calc R . . . .
C2 C 0.09899(16) 0.5407(4) 0.27747(19) 0.0584(12) Uani 1 1 d . . . . .
H2A H 0.070153 0.592232 0.239465 0.070 Uiso 1 1 calc R . . . .
H2B H 0.070996 0.542035 0.309468 0.070 Uiso 1 1 calc R . . . .
C1 C 0.18178(15) 0.5842(3) 0.30850(16) 0.0391(8) Uani 1 1 d . . . . .
C5 C 0.31714(13) 0.5202(2) 0.33187(13) 0.0212(5) Uani 1 1 d . . . . .
H5A H 0.322438 0.593655 0.360273 0.025 Uiso 0.516(15) 1 calc R . . A 1
H5B H 0.330086 0.603174 0.351509 0.025 Uiso 0.484(15) 1 calc R . . A 2
C10 C 0.35777(16) 0.4229(3) 0.3795(2) 0.0567(11) Uani 1 1 d . . . . .
H10A H 0.348990 0.342945 0.357148 0.068 Uiso 1 1 calc R . . . .
H10B H 0.335965 0.419420 0.415569 0.068 Uiso 1 1 calc R . . . .
C9 C 0.44623(15) 0.4498(3) 0.40768(18) 0.0435(9) Uani 1 1 d . . . . .
H9A H 0.455132 0.526350 0.433246 0.052 Uiso 1 1 calc R . . . .
H9B H 0.473311 0.383311 0.437592 0.052 Uiso 1 1 calc R . . . .
C14 C 0.60138(18) 0.5812(5) 0.4256(2) 0.0814(17) Uani 1 1 d D . . . .
H14A H 0.595172 0.552378 0.466751 0.098 Uiso 0.516(15) 1 calc R . . A 1
H14B H 0.579485 0.664277 0.415512 0.098 Uiso 0.516(15) 1 calc R . . A 1
H14C H 0.597992 0.582706 0.470152 0.098 Uiso 0.484(15) 1 calc R . . A 2
H14D H 0.575165 0.654615 0.401516 0.098 Uiso 0.484(15) 1 calc R . . A 2
C13 C 0.68748(19) 0.5759(5) 0.4289(2) 0.0788(15) Uani 1 1 d . . . . .
H13A H 0.697137 0.633184 0.397331 0.095 Uiso 1 1 calc R . . . .
H13B H 0.723488 0.595458 0.473613 0.095 Uiso 1 1 calc R . . . .
C12 C 0.69788(17) 0.4454(4) 0.41106(18) 0.0618(12) Uani 1 1 d . . . . .
H12A H 0.732458 0.440601 0.384339 0.074 Uiso 1 1 calc R . . . .
H12B H 0.720240 0.394733 0.450818 0.074 Uiso 1 1 calc R . . . .
C11 C 0.61572(17) 0.4060(4) 0.37212(15) 0.0480(9) Uani 1 1 d D . . . .
C7 C 0.4384(3) 0.5943(9) 0.3111(3) 0.0253(18) Uani 0.516(15) 1 d D . . A 1
H7A H 0.445960 0.664088 0.341422 0.030 Uiso 0.516(15) 1 calc R . . A 1
H7B H 0.462197 0.613939 0.277392 0.030 Uiso 0.516(15) 1 calc R . . A 1
C6 C 0.3508(3) 0.5631(9) 0.2791(3) 0.0231(17) Uani 0.516(15) 1 d D . . A 1
H6A H 0.344231 0.498152 0.246041 0.028 Uiso 0.516(15) 1 calc R . . A 1
H6B H 0.321747 0.635817 0.256469 0.028 Uiso 0.516(15) 1 calc R . . A 1
C8 C 0.47932(16) 0.4614(4) 0.35363(18) 0.0631(13) Uani 1 1 d . . . . .
H8A H 0.466401 0.388730 0.324150 0.076 Uiso 0.516(15) 1 calc R . . A 1
H8B H 0.472901 0.376812 0.335630 0.076 Uiso 0.484(15) 1 calc R . . A 2
N5A N 0.5638(5) 0.4664(9) 0.3892(4) 0.030(2) Uani 0.484(15) 1 d D . . A 2
C7A C 0.4379(3) 0.5234(11) 0.3030(4) 0.028(2) Uani 0.484(15) 1 d D . . A 2
H7AA H 0.458514 0.507340 0.267060 0.034 Uiso 0.484(15) 1 calc R . . A 2
H7AB H 0.446428 0.610844 0.314169 0.034 Uiso 0.484(15) 1 calc R . . A 2
C6A C 0.3490(3) 0.5006(12) 0.2766(3) 0.028(2) Uani 0.484(15) 1 d D . . A 2
H6AA H 0.323449 0.557270 0.240094 0.034 Uiso 0.484(15) 1 calc R . . A 2
H6AB H 0.338200 0.416342 0.259861 0.034 Uiso 0.484(15) 1 calc R . . A 2
H10 H 0.143(3) 0.758(5) 0.334(2) 0.127(19) Uiso 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
Np1 0.00815(6) 0.01622(7) 0.01508(7) -0.00600(6) -0.00113(4) 0.00271(5)
O1 0.0171(9) 0.0421(11) 0.0213(9) -0.0060(8) 0.0011(7) 0.0127(8)
O2 0.0165(8) 0.0290(10) 0.0205(9) -0.0058(7) 0.0014(7) 0.0075(7)
O3 0.0382(12) 0.103(2) 0.0335(12) -0.0015(13) 0.0164(10) 0.0434(13)
O4 0.0173(8) 0.0218(10) 0.0243(9) -0.0081(7) -0.0032(7) 0.0045(7)
O5 0.0138(8) 0.0262(9) 0.0249(9) -0.0012(7) -0.0014(7) 0.0033(7)
O6 0.0279(10) 0.0370(11) 0.0274(10) -0.0081(8) -0.0132(8) 0.0179(9)
O7 0.0142(8) 0.0214(9) 0.0322(10) -0.0073(7) 0.0004(7) 0.0030(7)
O9 0.0304(11) 0.0187(10) 0.0701(15) 0.0024(10) 0.0068(10) -0.0046(8)
O8 0.0165(8) 0.0233(9) 0.0334(10) -0.0016(8) 0.0046(8) 0.0036(7)
N3 0.0153(10) 0.0176(11) 0.0370(13) 0.0016(9) -0.0033(9) 0.0030(8)
N1 0.0222(11) 0.0448(15) 0.0253(12) -0.0074(10) 0.0042(9) 0.0143(10)
N2 0.0173(10) 0.0274(11) 0.0196(11) -0.0075(9) -0.0024(8) 0.0093(9)
O10 0.0256(11) 0.0483(14) 0.0698(16) 0.0179(12) 0.0248(11) 0.0232(10)
O11 0.0249(11) 0.0721(17) 0.0496(14) 0.0117(13) 0.0171(10) 0.0331(11)
N4 0.0087(9) 0.0338(12) 0.0366(12) 0.0178(11) 0.0024(8) 0.0010(10)
N5 0.007(2) 0.084(6) 0.015(4) -0.015(4) 0.001(2) 0.007(4)
C4 0.0189(14) 0.0377(17) 0.058(2) 0.0241(15) -0.0078(13) -0.0096(12)
C3 0.0151(14) 0.102(3) 0.0327(17) 0.0338(19) -0.0105(12) -0.0186(17)
C2 0.0098(13) 0.084(3) 0.076(3) 0.059(2) 0.0074(14) 0.0091(14)
C1 0.0117(12) 0.057(2) 0.0503(19) 0.0374(17) 0.0125(12) 0.0154(13)
C5 0.0070(10) 0.0186(14) 0.0371(14) 0.0088(10) 0.0065(9) 0.0036(9)
C10 0.0145(13) 0.0392(18) 0.089(3) 0.0391(18) -0.0181(15) -0.0082(13)
C9 0.0122(13) 0.0265(14) 0.072(2) 0.0191(15) -0.0114(13) -0.0012(11)
C14 0.0114(14) 0.140(4) 0.086(3) -0.069(3) 0.0082(17) -0.009(2)
C13 0.0147(16) 0.134(4) 0.083(3) -0.034(3) 0.0115(17) 0.002(2)
C12 0.0106(14) 0.122(4) 0.053(2) 0.017(2) 0.0103(14) 0.0160(18)
C11 0.0184(14) 0.095(3) 0.0308(16) 0.0044(18) 0.0080(12) 0.0259(17)
C7 0.012(2) 0.028(5) 0.037(3) 0.001(3) 0.009(2) -0.001(2)
C6 0.010(2) 0.023(4) 0.034(3) 0.006(3) 0.004(2) -0.001(2)
C8 0.0067(12) 0.098(3) 0.069(2) -0.060(2) -0.0066(14) 0.0163(15)
N5A 0.011(3) 0.066(5) 0.015(4) 0.004(3) 0.008(3) 0.012(3)
C7A 0.012(3) 0.032(6) 0.043(4) 0.010(3) 0.014(2) -0.001(3)
C6A 0.011(3) 0.038(6) 0.035(3) 0.021(4) 0.007(2) 0.003(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Np1 O1 2.5055(17) 5_676 ?
Np1 O1 2.5056(17) . ?
Np1 O2 2.4962(16) 5_676 ?
Np1 O2 2.4963(16) . ?
Np1 O4 2.5027(16) . ?
Np1 O4 2.5027(16) 5_676 ?
Np1 O5 2.5048(17) 5_676 ?
Np1 O5 2.5047(17) . ?
Np1 O7 2.4995(17) . ?
Np1 O7 2.4994(17) 5_676 ?
Np1 O8 2.4922(18) . ?
Np1 O8 2.4922(18) 5_676 ?
O1 N1 1.277(3) . ?
O2 N1 1.271(3) . ?
O3 N1 1.215(3) . ?
O4 N2 1.271(3) . ?
O5 N2 1.273(3) . ?
O6 N2 1.221(3) . ?
O7 N3 1.278(3) . ?
O9 N3 1.215(3) . ?
O8 N3 1.271(3) . ?
O10 C1 1.260(4) . ?
O11 C11 1.255(4) . ?
N4 C4 1.459(4) . ?
N4 C1 1.318(4) . ?
N4 C5 1.472(3) . ?
N5 C14 1.457(8) . ?
N5 C11 1.351(9) . ?
N5 C8 1.536(10) . ?
C4 C3 1.546(4) . ?
C3 C2 1.521(6) . ?
C2 C1 1.500(4) . ?
C5 C10 1.496(3) . ?
C5 C6 1.543(7) . ?
C5 C6A 1.514(8) . ?
C10 C9 1.539(4) . ?
C9 C8 1.493(5) . ?
C14 C13 1.540(4) . ?
C14 N5A 1.520(10) . ?
C13 C12 1.514(7) . ?
C12 C11 1.505(5) . ?
C11 N5A 1.306(9) . ?
C7 C6 1.542(7) . ?
C7 C8 1.752(10) . ?
C8 N5A 1.464(10) . ?
C8 C7A 1.293(8) . ?
C7A C6A 1.536(7) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Np1 O1 180.0 5_676 . ?
O2 Np1 O1 129.04(5) 5_676 . ?
O2 Np1 O1 50.96(5) . . ?
O2 Np1 O1 129.04(5) . 5_676 ?
O2 Np1 O1 50.96(5) 5_676 5_676 ?
O2 Np1 O2 180.0 5_676 . ?
O2 Np1 O4 66.20(5) 5_676 . ?
O2 Np1 O4 113.80(5) 5_676 5_676 ?
O2 Np1 O4 66.20(5) . 5_676 ?
O2 Np1 O4 113.80(5) . . ?
O2 Np1 O5 114.37(6) . . ?
O2 Np1 O5 65.63(6) 5_676 . ?
O2 Np1 O5 65.63(6) . 5_676 ?
O2 Np1 O5 114.37(6) 5_676 5_676 ?
O2 Np1 O7 68.44(6) . . ?
O2 Np1 O7 111.55(6) 5_676 . ?
O2 Np1 O7 111.56(6) . 5_676 ?
O2 Np1 O7 68.45(6) 5_676 5_676 ?
O4 Np1 O1 111.34(6) 5_676 . ?
O4 Np1 O1 68.66(6) . . ?
O4 Np1 O1 68.66(6) 5_676 5_676 ?
O4 Np1 O1 111.34(6) . 5_676 ?
O4 Np1 O4 180.0 5_676 . ?
O4 Np1 O5 129.12(6) . 5_676 ?
O4 Np1 O5 50.88(6) . . ?
O4 Np1 O5 129.12(6) 5_676 . ?
O4 Np1 O5 50.88(6) 5_676 5_676 ?
O5 Np1 O1 111.90(6) . 5_676 ?
O5 Np1 O1 68.10(6) . . ?
O5 Np1 O1 68.10(6) 5_676 5_676 ?
O5 Np1 O1 111.90(6) 5_676 . ?
O5 Np1 O5 180.0 . 5_676 ?
O7 Np1 O1 68.01(6) 5_676 5_676 ?
O7 Np1 O1 111.99(6) . 5_676 ?
O7 Np1 O1 68.01(6) . . ?
O7 Np1 O1 111.99(6) 5_676 . ?
O7 Np1 O4 114.21(5) . 5_676 ?
O7 Np1 O4 65.79(5) . . ?
O7 Np1 O4 114.21(5) 5_676 . ?
O7 Np1 O4 65.79(5) 5_676 5_676 ?
O7 Np1 O5 111.88(6) 5_676 5_676 ?
O7 Np1 O5 111.88(6) . . ?
O7 Np1 O5 68.12(6) . 5_676 ?
O7 Np1 O5 68.12(6) 5_676 . ?
O7 Np1 O7 180.0 5_676 . ?
O8 Np1 O1 65.40(6) 5_676 . ?
O8 Np1 O1 65.40(6) . 5_676 ?
O8 Np1 O1 114.60(6) . . ?
O8 Np1 O1 114.60(6) 5_676 5_676 ?
O8 Np1 O2 66.62(6) . 5_676 ?
O8 Np1 O2 113.38(6) . . ?
O8 Np1 O2 113.38(6) 5_676 5_676 ?
O8 Np1 O2 66.62(6) 5_676 . ?
O8 Np1 O4 113.14(6) 5_676 . ?
O8 Np1 O4 66.86(6) 5_676 5_676 ?
O8 Np1 O4 113.14(6) . 5_676 ?
O8 Np1 O4 66.86(6) . . ?
O8 Np1 O5 68.03(6) 5_676 . ?
O8 Np1 O5 111.96(6) 5_676 5_676 ?
O8 Np1 O5 111.97(6) . . ?
O8 Np1 O5 68.04(6) . 5_676 ?
O8 Np1 O7 128.94(6) . 5_676 ?
O8 Np1 O7 128.94(6) 5_676 . ?
O8 Np1 O7 51.06(6) 5_676 5_676 ?
O8 Np1 O7 51.06(6) . . ?
O8 Np1 O8 180.0 . 5_676 ?
N1 O1 Np1 96.23(14) . . ?
N1 O2 Np1 96.82(13) . . ?
N2 O4 Np1 96.56(12) . . ?
N2 O5 Np1 96.42(14) . . ?
N3 O7 Np1 96.62(13) . . ?
N3 O8 Np1 97.17(14) . . ?
O7 N3 Np1 57.75(11) . . ?
O9 N3 Np1 178.44(18) . . ?
O9 N3 O7 122.4(2) . . ?
O9 N3 O8 122.5(2) . . ?
O8 N3 Np1 57.38(12) . . ?
O8 N3 O7 115.1(2) . . ?
O1 N1 Np1 58.13(12) . . ?
O2 N1 Np1 57.68(11) . . ?
O2 N1 O1 115.3(2) . . ?
O3 N1 Np1 172.7(2) . . ?
O3 N1 O1 122.7(2) . . ?
O3 N1 O2 122.0(2) . . ?
O4 N2 Np1 57.94(10) . . ?
O4 N2 O5 115.47(18) . . ?
O5 N2 Np1 58.04(11) . . ?
O6 N2 Np1 173.30(17) . . ?
O6 N2 O4 122.1(2) . . ?
O6 N2 O5 122.5(2) . . ?
C4 N4 C5 124.1(2) . . ?
C1 N4 C4 114.3(2) . . ?
C1 N4 C5 121.5(3) . . ?
C14 N5 C8 120.0(6) . . ?
C11 N5 C14 110.5(6) . . ?
C11 N5 C8 115.6(7) . . ?
N4 C4 C3 103.8(3) . . ?
C2 C3 C4 106.2(3) . . ?
C1 C2 C3 104.7(3) . . ?
O10 C1 N4 122.8(3) . . ?
O10 C1 C2 126.4(3) . . ?
N4 C1 C2 110.8(3) . . ?
N4 C5 C10 111.1(2) . . ?
N4 C5 C6 113.0(3) . . ?
N4 C5 C6A 107.9(3) . . ?
C10 C5 C6 120.3(4) . . ?
C10 C5 C6A 102.3(4) . . ?
C5 C10 C9 109.7(2) . . ?
C8 C9 C10 110.4(3) . . ?
N5 C14 C13 100.2(4) . . ?
N5A C14 C13 105.1(4) . . ?
C12 C13 C14 103.7(4) . . ?
C11 C12 C13 103.3(3) . . ?
O11 C11 N5 122.8(4) . . ?
O11 C11 C12 127.5(3) . . ?
O11 C11 N5A 119.8(5) . . ?
N5 C11 C12 108.8(5) . . ?
N5A C11 C12 111.5(5) . . ?
C6 C7 C8 103.8(4) . . ?
C7 C6 C5 110.0(4) . . ?
N5 C8 C7 97.4(6) . . ?
C9 C8 N5 118.3(4) . . ?
C9 C8 C7 105.9(3) . . ?
N5A C8 C9 102.6(4) . . ?
C7A C8 C9 116.0(4) . . ?
C7A C8 N5A 129.0(7) . . ?
C11 N5A C14 109.3(7) . . ?
C11 N5A C8 123.9(7) . . ?
C8 N5A C14 120.6(6) . . ?
C8 C7A C6A 117.6(5) . . ?
C5 C6A C7A 108.5(5) . . ?
_shelx_res_file
;
TITL mo_KT_L1Np_0m_a in C2/c #15
mo_kt_l1np_0m_a.res
created by SHELXL-2017/1 at 14:01:04 on 03-Dec-2018
REM reset to C2/c #15
CELL 0.71073 18.1413 10.9944 21.6888 90 109.931 90
ZERR 44 0.001 0.0006 0.0012 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N Np O
UNIT 112 180.35 40 4 88
SADI N5 C14 N5A C14
SADI N5 C11 N5A C11
SADI C7 C6 C7A C6A
SADI 0.04 N4 C6 N4 C6A
SADI 0.04 N5 C7 N5A C7A
L.S. 10
PLAN 20
TEMP -273.15
fmap 2
acta
REM
REM
REM
WGHT 0.013200 13.034800
EXTI 0.000407
FVAR 0.15568 0.51618
NP1 4 0.500000 1.000000 0.500000 10.50000 0.00815 0.01622 =
0.01508 -0.00600 -0.00113 0.00271
O1 5 0.536266 0.946135 0.401774 11.00000 0.01711 0.04214 =
0.02126 -0.00603 0.00107 0.01267
O2 5 0.616990 0.886675 0.494836 11.00000 0.01645 0.02902 =
0.02051 -0.00584 0.00143 0.00753
O3 5 0.649985 0.870614 0.407730 11.00000 0.03822 0.10338 =
0.03355 -0.00151 0.01640 0.04336
O4 5 0.380825 0.975520 0.399844 11.00000 0.01726 0.02177 =
0.02427 -0.00808 -0.00315 0.00453
O5 5 0.442050 1.145385 0.407129 11.00000 0.01377 0.02623 =
0.02494 -0.00125 -0.00144 0.00331
O6 5 0.328108 1.120647 0.330270 11.00000 0.02789 0.03703 =
0.02738 -0.00809 -0.01321 0.01794
O7 5 0.467045 0.784131 0.465402 11.00000 0.01421 0.02144 =
0.03223 -0.00726 0.00043 0.00298
O9 5 0.372832 0.680103 0.481933 11.00000 0.03039 0.01871 =
0.07009 0.00244 0.00685 -0.00463
O8 5 0.398498 0.865885 0.518084 11.00000 0.01645 0.02335 =
0.03340 -0.00162 0.00458 0.00365
N3 3 0.411013 0.773002 0.488172 11.00000 0.01529 0.01760 =
0.03702 0.00157 -0.00333 0.00304
N1 3 0.602930 0.899851 0.433657 11.00000 0.02224 0.04481 =
0.02535 -0.00742 0.00424 0.01432
N2 3 0.381657 1.082091 0.377353 11.00000 0.01735 0.02744 =
0.01964 -0.00748 -0.00238 0.00928
O10 5 0.202987 0.687839 0.332875 11.00000 0.02555 0.04834 =
0.06980 0.01790 0.02480 0.02323
O11 5 0.595206 0.313263 0.336613 11.00000 0.02487 0.07211 =
0.04961 0.01171 0.01710 0.03306
N4 3 0.231897 0.499393 0.305706 11.00000 0.00875 0.03378 =
0.03665 0.01777 0.00245 0.00100
PART 1
N5 3 0.565826 0.497647 0.371409 21.00000 0.00733 0.08398 =
0.01485 -0.01500 0.00132 0.00713
PART 0
C4 1 0.195430 0.388605 0.271935 11.00000 0.01889 0.03769 =
0.05836 0.02415 -0.00782 -0.00957
AFIX 23
H4A 2 0.212959 0.316627 0.300644 11.00000 -1.20000
H4B 2 0.208097 0.376151 0.231450 11.00000 -1.20000
AFIX 0
C3 1 0.106686 0.411210 0.255663 11.00000 0.01514 0.10171 =
0.03270 0.03377 -0.01046 -0.01860
AFIX 23
H3A 2 0.078425 0.402023 0.208007 11.00000 -1.20000
H3B 2 0.084667 0.352677 0.279441 11.00000 -1.20000
AFIX 0
C2 1 0.098989 0.540696 0.277468 11.00000 0.00979 0.08431 =
0.07566 0.05919 0.00745 0.00914
AFIX 23
H2A 2 0.070153 0.592232 0.239465 11.00000 -1.20000
H2B 2 0.070996 0.542035 0.309468 11.00000 -1.20000
AFIX 0
C1 1 0.181779 0.584230 0.308504 11.00000 0.01172 0.05688 =
0.05027 0.03740 0.01254 0.01543
C5 1 0.317136 0.520228 0.331873 11.00000 0.00703 0.01862 =
0.03709 0.00878 0.00650 0.00356
PART 1
AFIX 13
H5A 2 0.322438 0.593655 0.360273 21.00000 -1.20000
AFIX 13
PART 0
PART 2
H5B 2 0.330086 0.603174 0.351509 -21.00000 -1.20000
AFIX 0
PART 0
C10 1 0.357772 0.422860 0.379521 11.00000 0.01450 0.03922 =
0.08882 0.03906 -0.01814 -0.00823
AFIX 23
H10A 2 0.348990 0.342945 0.357148 11.00000 -1.20000
H10B 2 0.335965 0.419420 0.415569 11.00000 -1.20000
AFIX 0
C9 1 0.446232 0.449845 0.407675 11.00000 0.01216 0.02648 =
0.07209 0.01913 -0.01140 -0.00120
AFIX 23
H9A 2 0.455132 0.526350 0.433246 11.00000 -1.20000
H9B 2 0.473311 0.383311 0.437592 11.00000 -1.20000
AFIX 0
C14 1 0.601376 0.581218 0.425555 11.00000 0.01143 0.13992 =
0.08617 -0.06883 0.00818 -0.00939
PART 1
AFIX 23
H14A 2 0.595172 0.552378 0.466751 21.00000 -1.20000
H14B 2 0.579485 0.664277 0.415512 21.00000 -1.20000
AFIX 23
PART 0
PART 2
H14C 2 0.597992 0.582706 0.470152 -21.00000 -1.20000
H14D 2 0.575165 0.654615 0.401516 -21.00000 -1.20000
AFIX 0
PART 0
C13 1 0.687484 0.575853 0.428949 11.00000 0.01466 0.13425 =
0.08345 -0.03391 0.01155 0.00234
AFIX 23
H13A 2 0.697137 0.633184 0.397331 11.00000 -1.20000
H13B 2 0.723488 0.595458 0.473613 11.00000 -1.20000
AFIX 0
C12 1 0.697883 0.445426 0.411064 11.00000 0.01059 0.12153 =
0.05291 0.01677 0.01031 0.01596
AFIX 23
H12A 2 0.732458 0.440601 0.384339 11.00000 -1.20000
H12B 2 0.720240 0.394733 0.450818 11.00000 -1.20000
AFIX 0
C11 1 0.615719 0.405974 0.372118 11.00000 0.01843 0.09458 =
0.03077 0.00442 0.00797 0.02585
PART 1
C7 1 0.438449 0.594276 0.311061 21.00000 0.01210 0.02772 =
0.03650 0.00073 0.00896 -0.00106
AFIX 23
H7A 2 0.445960 0.664088 0.341422 21.00000 -1.20000
H7B 2 0.462197 0.613939 0.277392 21.00000 -1.20000
AFIX 0
C6 1 0.350759 0.563135 0.279080 21.00000 0.01044 0.02281 =
0.03354 0.00551 0.00430 -0.00085
AFIX 23
H6A 2 0.344231 0.498152 0.246041 21.00000 -1.20000
H6B 2 0.321747 0.635817 0.256469 21.00000 -1.20000
AFIX 0
PART 0
C8 1 0.479315 0.461409 0.353627 11.00000 0.00667 0.09847 =
0.06919 -0.05983 -0.00659 0.01628
PART 1
AFIX 13
H8A 2 0.466401 0.388730 0.324150 21.00000 -1.20000
AFIX 13
PART 0
PART 2
H8B 2 0.472901 0.376812 0.335630 -21.00000 -1.20000
AFIX 0
N5A 3 0.563806 0.466445 0.389242 -21.00000 0.01084 0.06594 =
0.01518 0.00381 0.00817 0.01246
C7A 1 0.437854 0.523450 0.303037 -21.00000 0.01237 0.03202 =
0.04337 0.00985 0.01402 -0.00059
AFIX 23
H7AA 2 0.458514 0.507340 0.267060 -21.00000 -1.20000
H7AB 2 0.446428 0.610844 0.314169 -21.00000 -1.20000
AFIX 0
C6A 1 0.349043 0.500605 0.276604 -21.00000 0.01124 0.03847 =
0.03500 0.02139 0.00700 0.00312
AFIX 23
H6AA 2 0.323449 0.557270 0.240094 -21.00000 -1.20000
H6AB 2 0.338200 0.416342 0.259861 -21.00000 -1.20000
AFIX 0
PART 0
H10 2 0.143329 0.758168 0.334175 11.00000 0.12686
HKLF 4
REM mo_KT_L1Np_0m_a in C2/c #15
REM R1 = 0.0192 for 3582 Fo > 4sig(Fo) and 0.0270 for all 4312 data
REM 310 parameters refined using 5 restraints
END
WGHT 0.0132 13.0348
REM Highest difference peak 0.474, deepest hole -0.523, 1-sigma level 0.074
Q1 1 0.4682 0.4163 0.3506 11.00000 0.05 0.47
Q2 1 0.4840 0.4983 0.3387 11.00000 0.05 0.47
Q3 1 0.5914 0.5393 0.4247 11.00000 0.05 0.47
Q4 1 0.6087 0.6298 0.4081 11.00000 0.05 0.40
Q5 1 0.3461 0.4263 0.3908 11.00000 0.05 0.40
Q6 1 0.3638 0.3994 0.3544 11.00000 0.05 0.39
Q7 1 0.4654 0.4602 0.3809 11.00000 0.05 0.35
Q8 1 0.3358 0.3539 0.3819 11.00000 0.05 0.35
Q9 1 0.0902 0.5842 0.2831 11.00000 0.05 0.34
Q10 1 0.2141 0.4425 0.2908 11.00000 0.05 0.32
Q11 1 0.4532 0.4448 0.4300 11.00000 0.05 0.31
Q12 1 0.3574 0.3411 0.3196 11.00000 0.05 0.31
Q13 1 0.4052 0.4430 0.3924 11.00000 0.05 0.31
Q14 1 0.6995 0.5408 0.4667 11.00000 0.05 0.30
Q15 1 0.6658 0.9043 0.4085 11.00000 0.05 0.30
Q16 1 0.4636 0.3827 0.4021 11.00000 0.05 0.30
Q17 1 0.7035 0.3843 0.4184 11.00000 0.05 0.30
Q18 1 0.6711 0.4032 0.4021 11.00000 0.05 0.29
Q19 1 0.4661 0.3306 0.3481 11.00000 0.05 0.29
Q20 1 0.1170 0.5570 0.2986 11.00000 0.05 0.29
;
_shelx_res_checksum 34873
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_mo_kt_l2np_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1933984'
loop_
_audit_author_name
_audit_author_address
'Juliane Maerz'
;Helmholtz Zentrum Dresden Rossendorf
Germany
;
_audit_update_record
;
2019-08-27 deposited with the CCDC. 2020-02-03 downloaded from the CCDC.
;
_audit_creation_date 2018-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H46 N10 Np O22'
_chemical_formula_sum 'C28 H46 N10 Np O22'
_chemical_formula_weight 1113.76
_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'
Np Np -11.4937 4.1493 '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 9.8264(10)
_cell_length_b 10.7164(11)
_cell_length_c 19.517(2)
_cell_angle_alpha 90
_cell_angle_beta 103.175(4)
_cell_angle_gamma 90
_cell_volume 2001.1(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 2678
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 26.3237
_cell_measurement_theta_min 2.1573
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.695
_exptl_absorpt_correction_T_max 0.6836
_exptl_absorpt_correction_T_min 0.6331
_exptl_absorpt_correction_type 'Numerical Mu Calculated'
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.848
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description platelet
_exptl_crystal_F_000 1110
_exptl_crystal_size_max 0.110
_exptl_crystal_size_mid 0.098
_exptl_crystal_size_min 0.080
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0346
_diffrn_reflns_av_unetI/netI 0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 53411
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.730
_diffrn_reflns_theta_min 2.182
_diffrn_ambient_temperature 100.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method 'generic \f and \o scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3596
_reflns_number_total 4249
_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 'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_collection ?
_computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 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 0.975
_refine_diff_density_min -1.196
_refine_diff_density_rms 0.289
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.340
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 281
_refine_ls_number_reflns 4249
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0268
_refine_ls_R_factor_gt 0.0188
_refine_ls_restrained_S_all 1.340
_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^)+(0.0387P)^2^+0.1923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0588
_refine_ls_wR_factor_ref 0.0691
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
C10(H10), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B), C4(H4A,H4B), C14(H14A,H14B), C6(H6A,
H6B), C12(H12A,H12B), C13(H13A,H13B), C2(H2A,H2B), C3(H3A,H3B)
;
_atom_sites_solution_hydrogens mixed
_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
Np1 Np 1.500000 1.000000 0.500000 0.00972(7) Uani 1 2 d S T P . .
O7 O 1.3046(2) 1.11046(17) 0.41681(10) 0.0175(4) Uani 1 1 d . . . . .
O9 O 1.1479(2) 1.22774(19) 0.44900(11) 0.0246(5) Uani 1 1 d . . . . .
O4 O 1.42122(19) 0.87544(18) 0.38875(10) 0.0170(4) Uani 1 1 d . . . . .
O6 O 1.5119(2) 0.8983(2) 0.29716(10) 0.0251(5) Uani 1 1 d . . . . .
O1 O 1.5588(2) 1.22231(17) 0.47883(10) 0.0178(4) Uani 1 1 d . . . . .
N3 N 1.2529(2) 1.1648(2) 0.46359(12) 0.0152(5) Uani 1 1 d . . . . .
N1 N 1.6919(3) 1.2084(2) 0.49348(12) 0.0168(5) Uani 1 1 d . . . . .
O5 O 1.5516(2) 1.0349(2) 0.38268(11) 0.0164(4) Uani 1 1 d . . . . .
O3 O 1.7715(2) 1.2938(2) 0.49168(11) 0.0277(5) Uani 1 1 d . . . . .
N2 N 1.4956(2) 0.9352(2) 0.35362(12) 0.0161(5) Uani 1 1 d . . . . .
O10 O 1.68170(19) 1.29844(17) 0.31019(10) 0.0169(4) Uani 1 1 d . . . . .
O11 O 1.6426(2) 1.68384(18) 0.23225(10) 0.0190(4) Uani 1 1 d . . . . .
H11 H 1.731(5) 1.745(4) 0.210(3) 0.096(17) Uiso 1 1 d . . . . .
N4 N 1.6446(3) 1.4797(2) 0.36190(14) 0.0146(5) Uani 1 1 d . . . . .
N5 N 1.4943(3) 1.5208(2) 0.21984(14) 0.0117(5) Uani 1 1 d . . . . .
C11 C 1.5892(3) 1.5873(2) 0.19887(14) 0.0122(5) Uani 1 1 d . . . . .
C9 C 1.2746(3) 1.5487(3) 0.25846(15) 0.0162(6) Uani 1 1 d . . . . .
H9A H 1.245206 1.463370 0.241984 0.019 Uiso 1 1 calc R . . . .
H9B H 1.239342 1.607274 0.219222 0.019 Uiso 1 1 calc R . . . .
C1 C 1.7279(3) 1.3965(2) 0.34430(14) 0.0133(6) Uani 1 1 d . . . . .
C10 C 1.4336(3) 1.5550(3) 0.27904(13) 0.0105(5) Uani 1 1 d . . . . .
H10 H 1.461188 1.642987 0.292656 0.013 Uiso 1 1 calc R . . . .
C8 C 1.2114(3) 1.5820(3) 0.32080(15) 0.0184(6) Uani 1 1 d . . . . .
H8A H 1.235020 1.669427 0.335206 0.022 Uiso 1 1 calc R . . . .
H8B H 1.108308 1.574929 0.306654 0.022 Uiso 1 1 calc R . . . .
C5 C 1.4916(3) 1.4704(3) 0.34282(15) 0.0123(6) Uani 1 1 d . . . . .
H5 H 1.466102 1.382224 0.328827 0.015 Uiso 1 1 calc R . . . .
C7 C 1.2671(4) 1.4954(2) 0.3822(2) 0.0230(8) Uani 1 1 d . . . . .
H7A H 1.239254 1.408502 0.368571 0.028 Uiso 1 1 calc R . . . .
H7B H 1.226246 1.518434 0.422411 0.028 Uiso 1 1 calc R . . . .
C4 C 1.7220(3) 1.5839(3) 0.40277(16) 0.0221(6) Uani 1 1 d . . . . .
H4A H 1.718461 1.578466 0.452974 0.027 Uiso 1 1 calc R . . . .
H4B H 1.683759 1.665461 0.383756 0.027 Uiso 1 1 calc R . . . .
C14 C 1.4496(3) 1.4110(3) 0.17395(14) 0.0156(6) Uani 1 1 d . . . . .
H14A H 1.355856 1.424278 0.142996 0.019 Uiso 1 1 calc R . . . .
H14B H 1.447978 1.334495 0.202156 0.019 Uiso 1 1 calc R . . . .
C6 C 1.4260(4) 1.5040(2) 0.40433(18) 0.0204(7) Uani 1 1 d . . . . .
H6A H 1.460953 1.446214 0.444035 0.024 Uiso 1 1 calc R . . . .
H6B H 1.453557 1.589792 0.420484 0.024 Uiso 1 1 calc R . . . .
C12 C 1.6208(3) 1.5366(3) 0.13310(16) 0.0183(6) Uani 1 1 d . . . . .
H12A H 1.722564 1.536088 0.135706 0.022 Uiso 1 1 calc R . . . .
H12B H 1.573023 1.585241 0.091402 0.022 Uiso 1 1 calc R . . . .
C13 C 1.5621(3) 1.4028(3) 0.13103(16) 0.0204(6) Uani 1 1 d . . . . .
H13A H 1.520947 1.376567 0.082054 0.025 Uiso 1 1 calc R . . . .
H13B H 1.636200 1.342895 0.152578 0.025 Uiso 1 1 calc R . . . .
C2 C 1.8787(3) 1.4326(3) 0.36921(16) 0.0184(6) Uani 1 1 d . . . . .
H2A H 1.928329 1.427565 0.330488 0.022 Uiso 1 1 calc R . . . .
H2B H 1.926711 1.378403 0.408396 0.022 Uiso 1 1 calc R . . . .
C3 C 1.8709(4) 1.5658(4) 0.3936(2) 0.0451(11) Uani 1 1 d . . . . .
H3A H 1.890997 1.624788 0.358104 0.054 Uiso 1 1 calc R . . . .
H3B H 1.939302 1.579897 0.438662 0.054 Uiso 1 1 calc R . . . .
O2 O 1.7344(2) 1.09750(18) 0.50967(10) 0.0157(4) Uani 1 1 d . . . . .
O8 O 1.3206(2) 1.14732(19) 0.52660(10) 0.0167(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
Np1 0.01039(9) 0.00904(10) 0.00995(10) -0.00110(5) 0.00275(6) 0.00109(5)
O7 0.0188(10) 0.0184(11) 0.0154(10) -0.0023(8) 0.0039(8) 0.0010(8)
O9 0.0171(11) 0.0198(11) 0.0350(13) 0.0023(9) 0.0020(9) 0.0084(9)
O4 0.0161(10) 0.0188(10) 0.0165(10) -0.0021(8) 0.0044(8) -0.0019(8)
O6 0.0276(12) 0.0336(13) 0.0155(10) -0.0076(9) 0.0080(9) 0.0066(10)
O1 0.0177(10) 0.0147(10) 0.0204(10) -0.0005(8) 0.0030(8) 0.0014(8)
N3 0.0144(12) 0.0125(12) 0.0185(13) 0.0005(10) 0.0032(10) 0.0006(10)
N1 0.0227(13) 0.0153(13) 0.0131(12) -0.0008(10) 0.0059(10) -0.0044(11)
O5 0.0177(11) 0.0166(9) 0.0152(11) -0.0016(9) 0.0043(9) -0.0008(9)
O3 0.0312(12) 0.0233(11) 0.0288(12) 0.0027(10) 0.0073(10) -0.0141(10)
N2 0.0125(12) 0.0204(14) 0.0152(12) -0.0016(10) 0.0026(10) 0.0044(10)
O10 0.0155(10) 0.0117(10) 0.0246(11) -0.0045(8) 0.0070(8) 0.0024(8)
O11 0.0204(10) 0.0148(10) 0.0253(11) -0.0019(9) 0.0127(9) -0.0065(8)
N4 0.0162(13) 0.0109(12) 0.0149(13) -0.0014(9) -0.0006(11) 0.0035(9)
N5 0.0128(12) 0.0109(11) 0.0117(12) 0.0004(9) 0.0037(10) -0.0011(9)
C11 0.0089(12) 0.0132(13) 0.0144(13) 0.0036(11) 0.0028(10) 0.0029(10)
C9 0.0122(14) 0.0213(15) 0.0159(14) 0.0006(13) 0.0047(11) 0.0013(12)
C1 0.0149(13) 0.0135(14) 0.0116(13) 0.0036(11) 0.0032(11) 0.0018(11)
C10 0.0107(13) 0.0099(13) 0.0121(13) 0.0011(11) 0.0051(10) 0.0015(11)
C8 0.0154(14) 0.0206(15) 0.0226(15) 0.0013(12) 0.0114(12) 0.0040(12)
C5 0.0153(14) 0.0100(12) 0.0119(14) 0.0003(11) 0.0039(11) 0.0030(11)
C7 0.031(2) 0.0213(18) 0.0233(18) 0.0033(11) 0.0195(16) 0.0055(12)
C4 0.0251(16) 0.0164(14) 0.0202(15) -0.0073(13) -0.0046(13) -0.0008(12)
C14 0.0139(14) 0.0185(14) 0.0143(13) -0.0060(11) 0.0028(11) -0.0030(11)
C6 0.0296(19) 0.0215(17) 0.0128(15) 0.0046(11) 0.0103(14) 0.0102(12)
C12 0.0181(15) 0.0228(14) 0.0162(15) 0.0028(13) 0.0085(12) 0.0031(13)
C13 0.0191(15) 0.0241(16) 0.0196(15) -0.0071(13) 0.0075(12) -0.0010(12)
C2 0.0153(14) 0.0179(16) 0.0213(15) 0.0022(12) 0.0024(12) 0.0000(12)
C3 0.0220(18) 0.032(2) 0.074(3) -0.024(2) -0.0051(18) 0.0017(16)
O2 0.0168(10) 0.0147(10) 0.0157(10) 0.0008(8) 0.0038(8) -0.0005(8)
O8 0.0176(10) 0.0162(10) 0.0152(10) -0.0031(8) 0.0013(8) 0.0048(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Np1 O7 2.5107(19) . ?
Np1 O7 2.5107(19) 3_876 ?
Np1 O4 2.5158(19) 3_876 ?
Np1 O4 2.5158(19) . ?
Np1 O1 2.5077(19) . ?
Np1 O1 2.5078(19) 3_876 ?
Np1 O5 2.484(2) 3_876 ?
Np1 O5 2.484(2) . ?
Np1 O2 2.4966(19) 3_876 ?
Np1 O2 2.4966(19) . ?
Np1 O8 2.5075(19) . ?
Np1 O8 2.5075(19) 3_876 ?
O7 N3 1.282(3) . ?
O9 N3 1.211(3) . ?
O4 N2 1.281(3) . ?
O6 N2 1.215(3) . ?
O1 N1 1.283(3) . ?
N3 O8 1.272(3) . ?
N1 O3 1.209(3) . ?
N1 O2 1.275(3) . ?
O5 N2 1.274(3) . ?
O10 C1 1.271(3) . ?
O11 C11 1.271(3) . ?
N4 C1 1.308(4) . ?
N4 C5 1.467(4) . ?
N4 C4 1.478(4) . ?
N5 C11 1.311(3) . ?
N5 C10 1.463(3) . ?
N5 C14 1.483(3) . ?
C11 C12 1.490(4) . ?
C9 C10 1.523(4) . ?
C9 C8 1.530(4) . ?
C1 C2 1.501(4) . ?
C10 C5 1.540(4) . ?
C8 C7 1.517(4) . ?
C5 C6 1.530(4) . ?
C7 C6 1.525(5) . ?
C4 C3 1.526(5) . ?
C14 C13 1.534(4) . ?
C12 C13 1.542(4) . ?
C2 C3 1.512(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
O7 Np1 O7 180.00(7) . 3_876 ?
O7 Np1 O4 110.33(6) 3_876 . ?
O7 Np1 O4 110.34(6) . 3_876 ?
O7 Np1 O4 69.66(6) . . ?
O7 Np1 O4 69.66(6) 3_876 3_876 ?
O4 Np1 O4 180.0 . 3_876 ?
O1 Np1 O7 67.45(6) . . ?
O1 Np1 O7 112.55(6) 3_876 . ?
O1 Np1 O7 112.55(6) . 3_876 ?
O1 Np1 O7 67.44(6) 3_876 3_876 ?
O1 Np1 O4 113.52(6) . . ?
O1 Np1 O4 66.49(6) . 3_876 ?
O1 Np1 O4 113.51(6) 3_876 3_876 ?
O1 Np1 O4 66.48(6) 3_876 . ?
O1 Np1 O1 180.0 . 3_876 ?
O5 Np1 O7 112.35(7) . 3_876 ?
O5 Np1 O7 112.35(7) 3_876 . ?
O5 Np1 O7 67.65(7) . . ?
O5 Np1 O7 67.65(7) 3_876 3_876 ?
O5 Np1 O4 51.07(7) . . ?
O5 Np1 O4 51.07(7) 3_876 3_876 ?
O5 Np1 O4 128.94(7) . 3_876 ?
O5 Np1 O4 128.93(7) 3_876 . ?
O5 Np1 O1 66.55(7) 3_876 3_876 ?
O5 Np1 O1 66.55(7) . . ?
O5 Np1 O1 113.45(7) 3_876 . ?
O5 Np1 O1 113.45(7) . 3_876 ?
O5 Np1 O5 180.00(14) . 3_876 ?
O5 Np1 O2 68.16(7) . . ?
O5 Np1 O2 111.84(7) 3_876 . ?
O5 Np1 O2 68.16(7) 3_876 3_876 ?
O5 Np1 O2 111.84(7) . 3_876 ?
O5 Np1 O8 113.40(7) . . ?
O5 Np1 O8 66.60(7) . 3_876 ?
O5 Np1 O8 66.60(7) 3_876 . ?
O5 Np1 O8 113.40(7) 3_876 3_876 ?
O2 Np1 O7 114.07(6) 3_876 3_876 ?
O2 Np1 O7 114.07(6) . . ?
O2 Np1 O7 65.93(6) 3_876 . ?
O2 Np1 O7 65.93(6) . 3_876 ?
O2 Np1 O4 112.61(6) . . ?
O2 Np1 O4 67.39(6) . 3_876 ?
O2 Np1 O4 67.39(6) 3_876 . ?
O2 Np1 O4 112.60(6) 3_876 3_876 ?
O2 Np1 O1 51.08(6) . . ?
O2 Np1 O1 128.92(6) . 3_876 ?
O2 Np1 O1 128.92(6) 3_876 . ?
O2 Np1 O1 51.08(6) 3_876 3_876 ?
O2 Np1 O2 180.0 . 3_876 ?
O2 Np1 O8 113.63(6) . . ?
O2 Np1 O8 113.63(6) 3_876 3_876 ?
O2 Np1 O8 66.37(6) 3_876 . ?
O2 Np1 O8 66.37(6) . 3_876 ?
O8 Np1 O7 129.29(6) . 3_876 ?
O8 Np1 O7 129.29(6) 3_876 . ?
O8 Np1 O7 50.71(6) 3_876 3_876 ?
O8 Np1 O7 50.72(6) . . ?
O8 Np1 O4 114.84(6) 3_876 3_876 ?
O8 Np1 O4 65.16(6) 3_876 . ?
O8 Np1 O4 114.84(6) . . ?
O8 Np1 O4 65.16(6) . 3_876 ?
O8 Np1 O1 68.60(6) . . ?
O8 Np1 O1 111.40(6) 3_876 . ?
O8 Np1 O1 111.40(6) . 3_876 ?
O8 Np1 O1 68.60(6) 3_876 3_876 ?
O8 Np1 O8 180.00(6) 3_876 . ?
N3 O7 Np1 97.03(15) . . ?
N2 O4 Np1 95.50(15) . . ?
N1 O1 Np1 96.57(15) . . ?
O7 N3 Np1 57.48(12) . . ?
O9 N3 Np1 177.07(19) . . ?
O9 N3 O7 122.7(2) . . ?
O9 N3 O8 122.6(2) . . ?
O8 N3 Np1 57.28(12) . . ?
O8 N3 O7 114.7(2) . . ?
O1 N1 Np1 57.79(12) . . ?
O3 N1 Np1 179.2(2) . . ?
O3 N1 O1 122.6(2) . . ?
O3 N1 O2 122.4(2) . . ?
O2 N1 Np1 57.25(13) . . ?
O2 N1 O1 115.0(2) . . ?
N2 O5 Np1 97.21(15) . . ?
O4 N2 Np1 58.70(12) . . ?
O6 N2 Np1 170.17(18) . . ?
O6 N2 O4 122.1(2) . . ?
O6 N2 O5 122.9(2) . . ?
O5 N2 Np1 57.23(13) . . ?
O5 N2 O4 115.0(2) . . ?
C1 N4 C5 123.6(2) . . ?
C1 N4 C4 112.4(3) . . ?
C5 N4 C4 124.0(2) . . ?
C11 N5 C10 123.9(2) . . ?
C11 N5 C14 112.1(2) . . ?
C10 N5 C14 123.9(2) . . ?
O11 C11 N5 121.5(2) . . ?
O11 C11 C12 126.6(2) . . ?
N5 C11 C12 111.9(2) . . ?
C10 C9 C8 111.0(2) . . ?
O10 C1 N4 122.1(3) . . ?
O10 C1 C2 126.2(2) . . ?
N4 C1 C2 111.7(2) . . ?
N5 C10 C9 111.0(2) . . ?
N5 C10 C5 110.4(2) . . ?
C9 C10 C5 110.8(2) . . ?
C7 C8 C9 110.3(2) . . ?
N4 C5 C10 109.5(2) . . ?
N4 C5 C6 112.1(3) . . ?
C6 C5 C10 110.6(2) . . ?
C8 C7 C6 110.4(3) . . ?
N4 C4 C3 103.3(2) . . ?
N5 C14 C13 103.0(2) . . ?
C7 C6 C5 110.6(3) . . ?
C11 C12 C13 102.2(2) . . ?
C14 C13 C12 104.1(2) . . ?
C1 C2 C3 103.2(2) . . ?
C2 C3 C4 106.0(3) . . ?
N1 O2 Np1 97.31(15) . . ?
N3 O8 Np1 97.47(14) . . ?
_shelx_res_file
;
TITL mo_KT_L2Np_0m_a in P21/n #14
mo_kt_l2np_0m_a.res
created by SHELXL-2017/1 at 14:14:07 on 03-Dec-2018
REM reset to P21/n #14
CELL 0.71073 9.8264 10.7164 19.5172 90 103.175 90
ZERR 2 0.001 0.0011 0.002 0 0.004 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N Np O
UNIT 56 96 20 2 44
L.S. 20
PLAN 20
TEMP -173.15
BOND
fmap 2
acta
REM
REM
REM
WGHT 0.038700 0.192300
FVAR 0.33121
NP1 4 1.500000 1.000000 0.500000 10.50000 0.01039 0.00904 =
0.00995 -0.00110 0.00275 0.00109
O7 5 1.304590 1.110465 0.416806 11.00000 0.01881 0.01837 =
0.01537 -0.00225 0.00388 0.00100
O9 5 1.147887 1.227743 0.448996 11.00000 0.01707 0.01982 =
0.03505 0.00227 0.00202 0.00839
O4 5 1.421223 0.875441 0.388751 11.00000 0.01615 0.01880 =
0.01649 -0.00210 0.00444 -0.00185
O6 5 1.511870 0.898276 0.297159 11.00000 0.02762 0.03365 =
0.01546 -0.00763 0.00802 0.00665
O1 5 1.558776 1.222311 0.478834 11.00000 0.01773 0.01473 =
0.02040 -0.00046 0.00301 0.00140
N3 3 1.252857 1.164760 0.463589 11.00000 0.01436 0.01251 =
0.01851 0.00045 0.00316 0.00062
N1 3 1.691909 1.208402 0.493477 11.00000 0.02273 0.01533 =
0.01309 -0.00079 0.00585 -0.00438
O5 5 1.551642 1.034879 0.382675 11.00000 0.01775 0.01658 =
0.01522 -0.00157 0.00430 -0.00078
O3 5 1.771468 1.293818 0.491680 11.00000 0.03125 0.02334 =
0.02876 0.00266 0.00729 -0.01409
N2 3 1.495579 0.935175 0.353623 11.00000 0.01254 0.02039 =
0.01523 -0.00157 0.00259 0.00443
O10 5 1.681702 1.298445 0.310194 11.00000 0.01555 0.01173 =
0.02456 -0.00454 0.00703 0.00239
O11 5 1.642616 1.683839 0.232253 11.00000 0.02037 0.01484 =
0.02530 -0.00191 0.01275 -0.00646
H11 2 1.731432 1.744851 0.209653 11.00000 0.09583
N4 3 1.644584 1.479669 0.361896 11.00000 0.01617 0.01088 =
0.01489 -0.00136 -0.00056 0.00352
N5 3 1.494305 1.520753 0.219836 11.00000 0.01281 0.01095 =
0.01172 0.00041 0.00370 -0.00109
C11 1 1.589247 1.587263 0.198870 11.00000 0.00895 0.01325 =
0.01436 0.00365 0.00283 0.00293
C9 1 1.274620 1.548666 0.258461 11.00000 0.01218 0.02125 =
0.01586 0.00057 0.00471 0.00130
AFIX 23
H9A 2 1.245206 1.463370 0.241984 11.00000 -1.20000
H9B 2 1.239342 1.607274 0.219222 11.00000 -1.20000
AFIX 0
C1 1 1.727875 1.396459 0.344299 11.00000 0.01486 0.01345 =
0.01159 0.00359 0.00320 0.00185
C10 1 1.433593 1.555019 0.279038 11.00000 0.01072 0.00991 =
0.01213 0.00107 0.00506 0.00153
AFIX 13
H10 2 1.461188 1.642987 0.292656 11.00000 -1.20000
AFIX 0
C8 1 1.211364 1.582048 0.320803 11.00000 0.01538 0.02063 =
0.02255 0.00130 0.01137 0.00402
AFIX 23
H8A 2 1.235020 1.669427 0.335206 11.00000 -1.20000
H8B 2 1.108308 1.574929 0.306654 11.00000 -1.20000
AFIX 0
C5 1 1.491640 1.470438 0.342822 11.00000 0.01530 0.00999 =
0.01187 0.00025 0.00386 0.00304
AFIX 13
H5 2 1.466102 1.382224 0.328827 11.00000 -1.20000
AFIX 0
C7 1 1.267097 1.495407 0.382243 11.00000 0.03086 0.02127 =
0.02326 0.00331 0.01948 0.00548
AFIX 23
H7A 2 1.239254 1.408502 0.368571 11.00000 -1.20000
H7B 2 1.226246 1.518434 0.422411 11.00000 -1.20000
AFIX 0
C4 1 1.722010 1.583862 0.402773 11.00000 0.02506 0.01638 =
0.02021 -0.00730 -0.00458 -0.00077
AFIX 23
H4A 2 1.718461 1.578466 0.452974 11.00000 -1.20000
H4B 2 1.683759 1.665461 0.383756 11.00000 -1.20000
AFIX 0
C14 1 1.449611 1.411030 0.173946 11.00000 0.01391 0.01852 =
0.01426 -0.00595 0.00283 -0.00300
AFIX 23
H14A 2 1.355856 1.424278 0.142996 11.00000 -1.20000
H14B 2 1.447978 1.334495 0.202156 11.00000 -1.20000
AFIX 0
C6 1 1.425971 1.503953 0.404331 11.00000 0.02960 0.02147 =
0.01282 0.00458 0.01033 0.01023
AFIX 23
H6A 2 1.460953 1.446214 0.444035 11.00000 -1.20000
H6B 2 1.453557 1.589792 0.420484 11.00000 -1.20000
AFIX 0
C12 1 1.620762 1.536591 0.133098 11.00000 0.01807 0.02280 =
0.01620 0.00276 0.00853 0.00307
AFIX 23
H12A 2 1.722564 1.536088 0.135706 11.00000 -1.20000
H12B 2 1.573023 1.585241 0.091402 11.00000 -1.20000
AFIX 0
C13 1 1.562072 1.402814 0.131032 11.00000 0.01906 0.02415 =
0.01962 -0.00709 0.00750 -0.00097
AFIX 23
H13A 2 1.520947 1.376567 0.082054 11.00000 -1.20000
H13B 2 1.636200 1.342895 0.152578 11.00000 -1.20000
AFIX 0
C2 1 1.878693 1.432586 0.369214 11.00000 0.01525 0.01787 =
0.02128 0.00215 0.00239 -0.00002
AFIX 23
H2A 2 1.928329 1.427565 0.330488 11.00000 -1.20000
H2B 2 1.926711 1.378403 0.408396 11.00000 -1.20000
AFIX 0
C3 1 1.870873 1.565786 0.393558 11.00000 0.02204 0.03203 =
0.07358 -0.02356 -0.00507 0.00173
AFIX 23
H3A 2 1.890997 1.624788 0.358104 11.00000 -1.20000
H3B 2 1.939302 1.579897 0.438662 11.00000 -1.20000
AFIX 0
O2 5 1.734369 1.097503 0.509673 11.00000 0.01676 0.01471 =
0.01567 0.00084 0.00380 -0.00048
O8 5 1.320572 1.147317 0.526596 11.00000 0.01762 0.01617 =
0.01519 -0.00314 0.00125 0.00477
HKLF 4
REM mo_KT_L2Np_0m_a in P21/n #14
REM R1 = 0.0188 for 3596 Fo > 4sig(Fo) and 0.0268 for all 4249 data
REM 281 parameters refined using 0 restraints
END
WGHT 0.0387 0.1923
REM Highest difference peak 0.975, deepest hole -1.196, 1-sigma level 0.289
Q1 1 1.8601 1.5342 0.4340 11.00000 0.05 0.97
Q2 1 1.2427 1.5355 0.3498 11.00000 0.05 0.75
Q3 1 1.9632 1.6183 0.4257 11.00000 0.05 0.75
Q4 1 1.9097 1.4954 0.4804 11.00000 0.05 0.75
Q5 1 2.0835 1.5543 0.4331 11.00000 0.05 0.73
Q6 1 1.0933 1.4583 0.4419 11.00000 0.05 0.72
Q7 1 2.0108 1.4820 0.4453 11.00000 0.05 0.71
Q8 1 1.1774 1.4801 0.4347 11.00000 0.05 0.70
Q9 1 2.0577 1.5941 0.4730 11.00000 0.05 0.70
Q10 1 1.2330 1.4943 0.3979 11.00000 0.05 0.69
Q11 1 1.2493 1.5697 0.2923 11.00000 0.05 0.68
Q12 1 1.1228 1.5108 0.4723 11.00000 0.05 0.68
Q13 1 1.9012 1.5403 0.5136 11.00000 0.05 0.67
Q14 1 2.0137 1.5532 0.5140 11.00000 0.05 0.67
Q15 1 2.0111 1.5180 0.4803 11.00000 0.05 0.67
Q16 1 1.1463 1.4275 0.4044 11.00000 0.05 0.65
Q17 1 2.0567 1.4276 0.4047 11.00000 0.05 0.62
Q18 1 2.0293 1.4015 0.4484 11.00000 0.05 0.61
Q19 1 2.0285 1.6963 0.4389 11.00000 0.05 0.61
Q20 1 1.1630 1.6053 0.3218 11.00000 0.05 0.59
;
_shelx_res_checksum 52463
_olex2_submission_special_instructions 'No special instructions were received'