#------------------------------------------------------------------------------
#$Date: 2019-07-08 10:51:59 +0300 (Mon, 08 Jul 2019) $
#$Revision: 216822 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552013.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1552013
loop_
_publ_author_name
'Michal S. Dutkiewicz'
'Joy H. Farnaby'
'Christos Apostolidis'
'Eric Colineau'
'Olaf Walter'
'Nicola Magnani'
'Michael G. Gardiner'
'Jason B. Love'
'Nikolas Kaltsoyannis'
'Roberto Caciuffo'
'Polly L. Arnold'
_publ_section_title
;
 Organometallic neptunium(III) complexes
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              797
_journal_page_last               802
_journal_paper_doi               10.1038/nchem.2520
_journal_volume                  8
_journal_year                    2016
_chemical_formula_moiety         'C37 H48 K N2 Np O3'
_chemical_formula_sum            'C37 H48 K N2 Np O3'
_chemical_formula_weight         844.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 105.645(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.205(3)
_cell_length_b                   20.025(5)
_cell_length_c                   17.800(4)
_cell_measurement_reflns_used    2723
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.309
_cell_volume                     3502.8(16)
_computing_cell_refinement       'APEX II (Bruker, 2007)'
_computing_data_collection       'APEX II (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'XPMA (Zsolnai, 1996), ORTEP (Farrugia, 1997)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker Apex II Quazar'
_diffrn_measurement_method       'combined omega- and phi-scan'
_diffrn_radiation_source         'Microfocus Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1154
_diffrn_reflns_av_unetI/netI     0.1552
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29115
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.421
_diffrn_reflns_theta_min         1.564
_exptl_absorpt_coefficient_mu    3.122
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs)
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.009
_refine_diff_density_max         2.817
_refine_diff_density_min         -2.311
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1405
_refine_ls_R_factor_gt           0.0664
_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/[σ²(Fo²)+(0.0471P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4613
_reflns_number_total             8007
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            nchem.2520-s4.cif
_cod_data_source_block           mdit78a
_cod_original_cell_volume        3502.7(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1552013
_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.
;
_shelx_estimated_absorpt_t_min   0.506
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2013-2
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'
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 0.03561(4) 0.96498(2) 0.10772(2) 0.02125(11) Uani 1 1 d . . . . .
K1 K 0.1155(2) 0.89082(9) 0.31206(11) 0.0268(5) Uani 1 1 d . . . . .
O1 O 0.1220(5) 0.9786(2) 0.0022(3) 0.0230(14) Uani 1 1 d . . . . .
N1 N 0.1330(7) 1.0267(3) 0.2562(4) 0.0218(16) Uani 1 1 d . . . . .
N2 N -0.0331(7) 0.8383(3) 0.1618(4) 0.0220(17) Uani 1 1 d . . . . .
C1 C 0.2225(8) 1.0423(4) 0.2132(5) 0.0206(19) Uani 1 1 d . . . . .
C2 C 0.1657(9) 1.0904(4) 0.1570(5) 0.027(2) Uani 1 1 d . . . . .
H2 H 0.2059 1.1087 0.1193 0.007(13) Uiso 1 1 calc R U . . .
C3 C 0.0369(9) 1.1065(4) 0.1673(5) 0.028(2) Uani 1 1 d . . . . .
H3 H -0.0267 1.1376 0.1377 0.007(13) Uiso 1 1 calc R U . . .
C4 C 0.0215(8) 1.0679(4) 0.2294(5) 0.023(2) Uani 1 1 d . . . . .
C5 C -0.0817(8) 1.0769(4) 0.2760(5) 0.025(2) Uani 1 1 d . . . . .
C6 C -0.2027(9) 1.1173(4) 0.2324(5) 0.031(2) Uani 1 1 d . . . . .
H6A H -0.1721 1.1613 0.2198 0.020(9) Uiso 1 1 calc R U . . .
H6B H -0.2656 1.1229 0.2650 0.020(9) Uiso 1 1 calc R U . . .
H6C H -0.2493 1.0941 0.1841 0.020(9) Uiso 1 1 calc R U . . .
C7 C -0.0084(9) 1.1166(4) 0.3502(5) 0.032(2) Uani 1 1 d . . . . .
H7A H 0.0689 1.0905 0.3809 0.020(9) Uiso 1 1 calc R U . . .
H7B H -0.0721 1.1251 0.3816 0.020(9) Uiso 1 1 calc R U . . .
H7C H 0.0244 1.1591 0.3350 0.020(9) Uiso 1 1 calc R U . . .
C8 C -0.1291(8) 1.0086(4) 0.2954(5) 0.023(2) Uani 1 1 d . . . . .
C9 C -0.1145(9) 0.9840(4) 0.3699(6) 0.031(2) Uani 1 1 d . . . . .
H9 H -0.0748 1.0114 0.4137 0.030(12) Uiso 1 1 calc R U . . .
C10 C -0.1574(9) 0.9192(4) 0.3816(5) 0.031(2) Uani 1 1 d . . . . .
H10 H -0.1523 0.9037 0.4328 0.030(12) Uiso 1 1 calc R U . . .
C11 C -0.2073(9) 0.8779(4) 0.3178(5) 0.027(2) Uani 1 1 d . . . . .
H11 H -0.2326 0.8334 0.3259 0.030(12) Uiso 1 1 calc R U . . .
C12 C -0.2211(8) 0.9004(4) 0.2421(5) 0.022(2) Uani 1 1 d . . . . .
C13 C -0.1828(8) 0.9672(4) 0.2331(5) 0.0233(19) Uani 1 1 d . . . . .
H13 H -0.1947 0.9841 0.1819 0.030(12) Uiso 1 1 calc R U . . .
C14 C -0.2731(9) 0.8588(4) 0.1668(5) 0.023(2) Uani 1 1 d . . . . .
C15 C -0.2954(9) 0.7859(4) 0.1868(5) 0.031(2) Uani 1 1 d . . . . .
H15A H -0.3589 0.7842 0.2193 0.033(10) Uiso 1 1 calc R U . . .
H15B H -0.2082 0.7661 0.2152 0.033(10) Uiso 1 1 calc R U . . .
H15C H -0.3332 0.7608 0.1385 0.033(10) Uiso 1 1 calc R U . . .
C16 C -0.4074(8) 0.8862(4) 0.1167(5) 0.031(2) Uani 1 1 d . . . . .
H16A H -0.4338 0.8618 0.0672 0.033(10) Uiso 1 1 calc R U . . .
H16B H -0.3970 0.9337 0.1063 0.033(10) Uiso 1 1 calc R U . . .
H16C H -0.4779 0.8807 0.1442 0.033(10) Uiso 1 1 calc R U . . .
C17 C -0.1610(8) 0.8592(4) 0.1247(5) 0.022(2) Uani 1 1 d . . . . .
C18 C -0.1758(8) 0.8657(4) 0.0440(5) 0.023(2) Uani 1 1 d . . . . .
H18 H -0.2531 0.8816 0.0055 0.080 Uiso 1 1 calc R U . . .
C19 C -0.0521(9) 0.8436(3) 0.0327(5) 0.023(2) Uani 1 1 d . . . . .
H19 H -0.0304 0.8411 -0.0159 0.080 Uiso 1 1 calc R U . . .
C20 C 0.0327(9) 0.8262(3) 0.1046(5) 0.0174(17) Uani 1 1 d . . . . .
C21 C 0.1689(9) 0.7918(4) 0.1270(5) 0.027(2) Uani 1 1 d . . . . .
C22 C 0.1453(9) 0.7200(4) 0.1542(5) 0.032(2) Uani 1 1 d . . . . .
H22A H 0.1121 0.7226 0.2009 0.041(11) Uiso 1 1 calc R U . . .
H22B H 0.2311 0.6951 0.1662 0.041(11) Uiso 1 1 calc R U . . .
H22C H 0.0777 0.6971 0.1125 0.041(11) Uiso 1 1 calc R U . . .
C23 C 0.2264(9) 0.7866(4) 0.0557(6) 0.035(2) Uani 1 1 d . . . . .
H23A H 0.1617 0.7625 0.0138 0.041(11) Uiso 1 1 calc R U . . .
H23B H 0.3131 0.7624 0.0703 0.041(11) Uiso 1 1 calc R U . . .
H23C H 0.2411 0.8315 0.0377 0.041(11) Uiso 1 1 calc R U . . .
C24 C 0.2685(8) 0.8324(4) 0.1915(5) 0.024(2) Uani 1 1 d . . . . .
C25 C 0.3584(9) 0.7996(4) 0.2547(5) 0.027(2) Uani 1 1 d . . . . .
H25 H 0.3574 0.7523 0.2585 0.019(12) Uiso 1 1 calc R U . . .
C26 C 0.4468(10) 0.8364(5) 0.3104(6) 0.042(3) Uani 1 1 d . . . . .
H26 H 0.5068 0.8144 0.3535 0.019(12) Uiso 1 1 calc R U . . .
C27 C 0.4502(9) 0.9063(4) 0.3050(6) 0.034(2) Uani 1 1 d . . . . .
H27 H 0.5142 0.9313 0.3433 0.019(12) Uiso 1 1 calc R U . . .
C28 C 0.3605(8) 0.9387(4) 0.2439(5) 0.022(2) Uani 1 1 d . . . . .
C29 C 0.2638(8) 0.9037(4) 0.1855(5) 0.023(2) Uani 1 1 d . . . . .
C30 C 0.3646(9) 1.0149(4) 0.2370(5) 0.024(2) Uani 1 1 d . . . . .
C31 C 0.4446(9) 1.0494(4) 0.3125(6) 0.036(3) Uani 1 1 d . . . . .
H31A H 0.4404 1.0979 0.3050 0.036(10) Uiso 1 1 calc R U . . .
H31B H 0.5397 1.0347 0.3256 0.036(10) Uiso 1 1 calc R U . . .
H31C H 0.4048 1.0375 0.3550 0.036(10) Uiso 1 1 calc R U . . .
C32 C 0.4399(8) 1.0334(4) 0.1745(5) 0.030(2) Uani 1 1 d . . . . .
H32A H 0.3912 1.0141 0.1241 0.036(10) Uiso 1 1 calc R U . . .
H32B H 0.5328 1.0156 0.1904 0.036(10) Uiso 1 1 calc R U . . .
H32C H 0.4431 1.0821 0.1697 0.036(10) Uiso 1 1 calc R U . . .
C33 C 0.2501(9) 0.9581(4) -0.0113(5) 0.032(2) Uani 1 1 d . . . . .
H33A H 0.3061 0.9359 0.0355 0.07(2) Uiso 1 1 calc R U . . .
H33B H 0.2984 0.9974 -0.0229 0.07(2) Uiso 1 1 calc R U . . .
H33C H 0.2325 0.9271 -0.0555 0.07(2) Uiso 1 1 calc R U . . .
O2 O 0.2139(7) 0.9081(4) 0.4689(4) 0.054(2) Uani 1 1 d . . . . .
O3 O 0.1263(9) 0.7838(4) 0.4045(4) 0.060(2) Uani 1 1 d . . . . .
C34 C 0.3070(12) 0.9640(7) 0.4842(7) 0.072(4) Uani 1 1 d . . . . .
H34A H 0.3210 0.9788 0.5383 0.11(2) Uiso 1 1 calc R U . . .
H34B H 0.2687 1.0008 0.4488 0.11(2) Uiso 1 1 calc R U . . .
H34C H 0.3943 0.9504 0.4759 0.11(2) Uiso 1 1 calc R U . . .
C35 C 0.2710(13) 0.8480(7) 0.5043(7) 0.072(4) Uani 1 1 d . . . . .
H35A H 0.3022 0.8537 0.5616 0.058(16) Uiso 1 1 calc R U . . .
H35B H 0.3505 0.8354 0.4854 0.058(16) Uiso 1 1 calc R U . . .
C36 C 0.1660(15) 0.7949(6) 0.4843(7) 0.069(4) Uani 1 1 d . . . . .
H36A H 0.2028 0.7531 0.5115 0.058(16) Uiso 1 1 calc R U . . .
H36B H 0.0859 0.8083 0.5021 0.058(16) Uiso 1 1 calc R U . . .
C37 C 0.0351(16) 0.7309(6) 0.3833(8) 0.086(5) Uani 1 1 d . . . . .
H37A H 0.0754 0.6904 0.4111 0.11(2) Uiso 1 1 calc R U . . .
H37B H 0.0151 0.7233 0.3270 0.11(2) Uiso 1 1 calc R U . . .
H37C H -0.0494 0.7416 0.3970 0.11(2) Uiso 1 1 calc R U . . .
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'
K K 0.2009 0.2494 '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'
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
O1 Np1 O1 66.8(2) . 3_575
O1 Np1 C29 90.3(2) . .
O1 Np1 C29 157.1(2) 3_575 .
O1 Np1 C1 98.2(2) . .
O1 Np1 C1 118.0(2) 3_575 .
C29 Np1 C1 63.8(2) . .
O1 Np1 C20 96.1(2) . .
O1 Np1 C20 116.3(2) 3_575 .
C29 Np1 C20 63.5(2) . .
C1 Np1 C20 125.2(2) . .
O1 Np1 C19 81.8(2) . .
O1 Np1 C19 87.8(2) 3_575 .
C29 Np1 C19 88.3(2) . .
C1 Np1 C19 152.1(2) . .
C20 Np1 C19 28.7(2) . .
O1 Np1 N1 126.40(19) . .
O1 Np1 N1 122.14(17) 3_575 .
C29 Np1 N1 71.3(2) . .
C1 Np1 N1 28.4(2) . .
C20 Np1 N1 116.9(2) . .
C19 Np1 N1 143.8(2) . .
O1 Np1 C2 84.1(2) . .
O1 Np1 C2 89.5(2) 3_575 .
C29 Np1 C2 88.6(2) . .
C1 Np1 C2 28.7(2) . .
C20 Np1 C2 152.1(2) . .
C19 Np1 C2 165.6(3) . .
N1 Np1 C2 46.9(2) . .
O1 Np1 N2 124.23(19) . .
O1 Np1 N2 120.59(18) 3_575 .
C29 Np1 N2 71.1(2) . .
C1 Np1 N2 117.0(2) . .
C20 Np1 N2 28.3(2) . .
C19 Np1 N2 46.9(2) . .
N1 Np1 N2 97.40(19) . .
C2 Np1 N2 143.9(2) . .
O1 Np1 C18 99.7(2) . .
O1 Np1 C18 75.3(2) 3_575 .
C29 Np1 C18 109.7(2) . .
C1 Np1 C18 161.0(2) . .
C20 Np1 C18 46.4(2) . .
C19 Np1 C18 28.2(2) . .
N1 Np1 C18 133.8(2) . .
C2 Np1 C18 161.1(2) . .
N2 Np1 C18 46.2(2) . .
O1 Np1 C17 125.7(2) . .
O1 Np1 C17 95.3(2) 3_575 .
C29 Np1 C17 97.9(2) . .
C1 Np1 C17 133.5(2) . .
C20 Np1 C17 44.7(2) . .
C19 Np1 C17 45.3(2) . .
N1 Np1 C17 106.9(2) . .
C2 Np1 C17 149.2(3) . .
N2 Np1 C17 26.77(19) . .
C18 Np1 C17 27.5(2) . .
O1 Np1 C4 127.4(2) . .
O1 Np1 C4 96.3(2) 3_575 .
C29 Np1 C4 98.4(2) . .
C1 Np1 C4 44.6(2) . .
C20 Np1 C4 134.0(2) . .
C19 Np1 C4 149.7(2) . .
N1 Np1 C4 27.05(19) . .
C2 Np1 C4 44.8(3) . .
N2 Np1 C4 107.5(2) . .
C18 Np1 C4 124.7(2) . .
C17 Np1 C4 104.4(2) . .
O3 K1 O2 62.0(2) . .
O3 K1 N2 101.6(2) . .
O2 K1 N2 161.9(2) . .
O3 K1 N1 163.0(2) . .
O2 K1 N1 101.0(2) . .
N2 K1 N1 95.11(18) . .
O3 K1 C29 125.1(2) . .
O2 K1 C29 128.9(2) . .
N2 K1 C29 65.7(2) . .
N1 K1 C29 65.2(2) . .
O3 K1 C24 99.9(2) . .
O2 K1 C24 128.5(2) . .
N2 K1 C24 58.4(2) . .
N1 K1 C24 91.5(2) . .
C29 K1 C24 26.4(2) . .
O3 K1 C28 124.3(2) . .
O2 K1 C28 103.9(2) . .
N2 K1 C28 91.5(2) . .
N1 K1 C28 57.8(2) . .
C29 K1 C28 25.9(2) . .
C24 K1 C28 44.2(2) . .
O3 K1 C12 98.2(2) . .
O2 K1 C12 115.8(2) . .
N2 K1 C12 56.3(2) . .
N1 K1 C12 88.32(19) . .
C29 K1 C12 112.8(2) . .
C24 K1 C12 114.3(2) . .
C28 K1 C12 132.3(2) . .
O3 K1 C11 78.3(2) . .
O2 K1 C11 94.2(2) . .
N2 K1 C11 74.0(2) . .
N1 K1 C11 103.6(2) . .
C29 K1 C11 136.2(2) . .
C24 K1 C11 131.2(2) . .
C28 K1 C11 155.9(2) . .
C12 K1 C11 24.1(2) . .
O3 K1 C13 120.2(2) . .
O2 K1 C13 114.4(2) . .
N2 K1 C13 65.7(2) . .
N1 K1 C13 64.20(19) . .
C29 K1 C13 103.1(2) . .
C24 K1 C13 116.0(2) . .
C28 K1 C13 114.6(2) . .
C12 K1 C13 24.42(18) . .
C11 K1 C13 41.9(2) . .
O3 K1 C9 99.9(2) . .
O2 K1 C9 73.2(2) . .
N2 K1 C9 104.4(2) . .
N1 K1 C9 72.5(2) . .
C29 K1 C9 134.8(2) . .
C24 K1 C9 156.1(2) . .
C28 K1 C9 128.9(2) . .
C12 K1 C9 49.4(2) . .
C11 K1 C9 42.1(2) . .
C13 K1 C9 41.2(2) . .
O3 K1 C10 79.1(2) . .
O2 K1 C10 73.5(2) . .
N2 K1 C10 97.0(2) . .
N1 K1 C10 95.8(2) . .
C29 K1 C10 151.4(2) . .
C24 K1 C10 154.9(2) . .
C28 K1 C10 152.9(2) . .
C12 K1 C10 42.2(2) . .
C11 K1 C10 23.8(2) . .
C13 K1 C10 48.3(2) . .
C9 K1 C10 24.0(2) . .
C33 O1 Np1 131.5(5) . .
C33 O1 Np1 115.2(5) . 3_575
Np1 O1 Np1 113.2(2) . 3_575
C1 N1 C4 106.3(7) . .
C1 N1 Np1 72.5(4) . .
C4 N1 Np1 83.7(5) . .
C1 N1 K1 120.7(5) . .
C4 N1 K1 123.6(5) . .
Np1 N1 K1 82.71(16) . .
C17 N2 C20 106.8(7) . .
C17 N2 Np1 81.6(4) . .
C20 N2 Np1 72.3(4) . .
C17 N2 K1 122.1(5) . .
C20 N2 K1 120.4(5) . .
Np1 N2 K1 82.75(16) . .
N1 C1 C2 110.2(7) . .
N1 C1 C30 119.7(7) . .
C2 C1 C30 129.6(8) . .
N1 C1 Np1 79.1(4) . .
C2 C1 Np1 79.8(4) . .
C30 C1 Np1 115.1(5) . .
C1 C2 C3 106.6(8) . .
C1 C2 Np1 71.5(4) . .
C3 C2 Np1 82.5(5) . .
C1 C2 H2 126.7 . .
C3 C2 H2 126.7 . .
Np1 C2 H2 112.0 . .
C4 C3 C2 106.5(8) . .
C4 C3 Np1 76.5(5) . .
C2 C3 Np1 69.9(4) . .
C4 C3 H3 126.8 . .
C2 C3 H3 126.8 . .
Np1 C3 H3 118.8 . .
N1 C4 C3 110.3(7) . .
N1 C4 C5 120.7(7) . .
C3 C4 C5 127.7(7) . .
N1 C4 Np1 69.3(4) . .
C3 C4 Np1 76.9(5) . .
C5 C4 Np1 130.3(5) . .
C6 C5 C4 112.1(8) . .
C6 C5 C8 109.5(7) . .
C4 C5 C8 109.2(7) . .
C6 C5 C7 107.7(7) . .
C4 C5 C7 106.3(7) . .
C8 C5 C7 112.2(8) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C13 C8 C9 118.3(8) . .
C13 C8 C5 116.2(8) . .
C9 C8 C5 125.4(8) . .
C13 C8 K1 76.9(5) . .
C9 C8 K1 77.4(5) . .
C5 C8 K1 111.9(5) . .
C8 C9 C10 120.9(8) . .
C8 C9 K1 79.0(5) . .
C10 C9 K1 78.7(5) . .
C8 C9 H9 119.6 . .
C10 C9 H9 119.6 . .
K1 C9 H9 113.1 . .
C11 C10 C9 119.4(9) . .
C11 C10 K1 75.9(5) . .
C9 C10 K1 77.3(5) . .
C11 C10 H10 120.3 . .
C9 C10 H10 120.3 . .
K1 C10 H10 117.3 . .
C10 C11 C12 121.3(8) . .
C10 C11 K1 80.3(5) . .
C12 C11 K1 77.7(5) . .
C10 C11 H11 119.4 . .
C12 C11 H11 119.4 . .
K1 C11 H11 112.9 . .
C11 C12 C13 117.2(8) . .
C11 C12 C14 125.9(7) . .
C13 C12 C14 116.9(7) . .
C11 C12 K1 78.1(5) . .
C13 C12 K1 78.9(5) . .
C14 C12 K1 111.8(5) . .
C8 C13 C12 122.8(8) . .
C8 C13 K1 79.5(5) . .
C12 C13 K1 76.6(5) . .
C8 C13 H13 118.6 . .
C12 C13 H13 118.6 . .
K1 C13 H13 115.5 . .
C16 C14 C17 112.6(7) . .
C16 C14 C15 108.2(7) . .
C17 C14 C15 107.2(7) . .
C16 C14 C12 111.0(7) . .
C17 C14 C12 107.2(7) . .
C15 C14 C12 110.5(7) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N2 C17 C18 110.4(7) . .
N2 C17 C14 120.5(7) . .
C18 C17 C14 127.8(7) . .
N2 C17 Np1 71.6(4) . .
C18 C17 Np1 73.8(4) . .
C14 C17 Np1 131.7(5) . .
C19 C18 C17 105.4(7) . .
C19 C18 Np1 70.9(4) . .
C17 C18 Np1 78.6(5) . .
C19 C18 H18 127.3 . .
C17 C18 H18 127.3 . .
Np1 C18 H18 115.7 . .
C20 C19 C18 108.0(8) . .
C20 C19 Np1 74.8(4) . .
C18 C19 Np1 80.9(4) . .
C20 C19 H19 126.0 . .
C18 C19 H19 126.0 . .
Np1 C19 H19 111.0 . .
C19 C20 N2 109.3(8) . .
C19 C20 C21 131.6(8) . .
N2 C20 C21 118.7(7) . .
C19 C20 Np1 76.5(4) . .
N2 C20 Np1 79.4(4) . .
C21 C20 Np1 116.7(5) . .
C20 C21 C23 110.0(7) . .
C20 C21 C24 109.3(7) . .
C23 C21 C24 109.2(7) . .
C20 C21 C22 107.2(7) . .
C23 C21 C22 108.6(7) . .
C24 C21 C22 112.5(7) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C25 C24 C29 121.8(8) . .
C25 C24 C21 120.3(7) . .
C29 C24 C21 117.9(7) . .
C25 C24 K1 88.0(6) . .
C29 C24 K1 70.9(5) . .
C21 C24 K1 110.5(5) . .
C26 C25 C24 119.4(8) . .
C26 C25 K1 83.5(6) . .
C24 C25 K1 67.9(5) . .
C26 C25 H25 120.3 . .
C24 C25 H25 120.3 . .
K1 C25 H25 119.1 . .
C25 C26 C27 120.8(9) . .
C25 C26 H26 119.6 . .
C27 C26 H26 119.6 . .
C28 C27 C26 120.0(8) . .
C28 C27 K1 67.7(5) . .
C26 C27 K1 82.2(5) . .
C28 C27 H27 120.0 . .
C26 C27 H27 120.0 . .
K1 C27 H27 121.0 . .
C27 C28 C29 122.0(8) . .
C27 C28 C30 120.3(8) . .
C29 C28 C30 117.6(7) . .
C27 C28 K1 88.9(6) . .
C29 C28 K1 70.6(5) . .
C30 C28 K1 111.7(5) . .
C28 C29 C24 115.9(7) . .
C28 C29 Np1 119.6(5) . .
C24 C29 Np1 120.3(5) . .
C28 C29 K1 83.5(5) . .
C24 C29 K1 82.7(5) . .
Np1 C29 K1 83.4(2) . .
C1 C30 C28 110.0(7) . .
C1 C30 C31 109.2(7) . .
C28 C30 C31 113.4(7) . .
C1 C30 C32 109.7(7) . .
C28 C30 C32 108.9(7) . .
C31 C30 C32 105.6(7) . .
C30 C31 H31A 109.5 . .
C30 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C30 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
O1 C33 H33A 109.5 . .
O1 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
O1 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C35 O2 C34 113.9(9) . .
C35 O2 K1 110.1(6) . .
C34 O2 K1 109.5(6) . .
C36 O3 C37 112.8(9) . .
C36 O3 K1 116.9(6) . .
C37 O3 K1 121.8(7) . .
O2 C34 K1 47.4(4) . .
O2 C34 H34A 109.5 . .
K1 C34 H34A 152.9 . .
O2 C34 H34B 109.5 . .
K1 C34 H34B 73.7 . .
H34A C34 H34B 109.5 . .
O2 C34 H34C 109.5 . .
K1 C34 H34C 93.9 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
O2 C35 C36 108.6(9) . .
O2 C35 K1 47.4(5) . .
C36 C35 K1 80.3(6) . .
O2 C35 H35A 110.0 . .
C36 C35 H35A 110.0 . .
K1 C35 H35A 157.2 . .
O2 C35 H35B 110.0 . .
C36 C35 H35B 110.0 . .
K1 C35 H35B 85.8 . .
H35A C35 H35B 108.4 . .
O3 C36 C35 110.7(10) . .
O3 C36 K1 42.6(5) . .
C35 C36 K1 75.3(6) . .
O3 C36 H36A 109.5 . .
C35 C36 H36A 109.5 . .
K1 C36 H36A 146.3 . .
O3 C36 H36B 109.5 . .
C35 C36 H36B 109.5 . .
K1 C36 H36B 101.0 . .
H36A C36 H36B 108.1 . .
O3 C37 H37A 109.5 . .
O3 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
O3 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Np1 O1 2.297(6) .
Np1 O1 2.448(5) 3_575
Np1 C29 2.666(8) .
Np1 C1 2.761(7) .
Np1 C20 2.779(7) .
Np1 C19 2.801(7) .
Np1 N1 2.843(6) .
Np1 C2 2.865(8) .
Np1 N2 2.867(6) .
Np1 C18 2.928(7) .
Np1 C17 2.989(8) .
Np1 C4 3.021(8) .
K1 O3 2.685(7) .
K1 O2 2.722(7) .
K1 N2 2.894(7) .
K1 N1 2.920(6) .
K1 C29 3.045(9) .
K1 C24 3.196(9) .
K1 C28 3.207(9) .
K1 C12 3.328(8) .
K1 C11 3.333(9) .
K1 C13 3.357(8) .
K1 C9 3.369(9) .
K1 C10 3.387(10) .
O1 C33 1.451(10) .
O1 Np1 2.448(5) 3_575
N1 C1 1.376(10) .
N1 C4 1.382(10) .
N2 C17 1.361(10) .
N2 C20 1.384(10) .
C1 C2 1.396(11) .
C1 C30 1.501(11) .
C2 C3 1.414(12) .
C2 H2 0.9500 .
C3 C4 1.391(12) .
C3 H3 0.9500 .
C4 C5 1.517(12) .
C5 C6 1.506(11) .
C5 C8 1.521(11) .
C5 C7 1.550(11) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C13 1.375(11) .
C8 C9 1.384(12) .
C9 C10 1.405(12) .
C9 H9 0.9500 .
C10 C11 1.385(12) .
C10 H10 0.9500 .
C11 C12 1.392(12) .
C11 H11 0.9500 .
C12 C13 1.414(11) .
C12 C14 1.546(11) .
C13 H13 0.9500 .
C14 C16 1.522(11) .
C14 C17 1.528(12) .
C14 C15 1.534(10) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 C18 1.409(12) .
C18 C19 1.402(11) .
C18 H18 0.9500 .
C19 C20 1.382(11) .
C19 H19 0.9500 .
C20 C21 1.506(11) .
C21 C23 1.539(12) .
C21 C24 1.544(12) .
C21 C22 1.555(10) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C24 C25 1.408(11) .
C24 C29 1.432(11) .
C25 C26 1.363(12) .
C25 H25 0.9500 .
C26 C27 1.406(12) .
C26 H26 0.9500 .
C27 C28 1.380(12) .
C27 H27 0.9500 .
C28 C29 1.411(11) .
C28 C30 1.531(11) .
C30 C31 1.535(12) .
C30 C32 1.557(12) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
O2 C35 1.410(13) .
O2 C34 1.446(13) .
O3 C36 1.386(12) .
O3 C37 1.394(15) .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C35 C36 1.483(17) .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C36 H36A 0.9900 .
C36 H36B 0.9900 .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
