#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:30:44 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195014 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/51/1545182.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_1545182
loop_
_publ_author_name
'Dutkiewicz, Michał S.'
'Apostolidis, Christos'
'Walter, Olaf'
'Arnold, Polly L.'
_publ_section_title
;
 Reduction chemistry of neptunium cyclopentadienide complexes: from
 structure to understanding
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2553
_journal_paper_doi               10.1039/C7SC00034K
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C32 H35 K1.5 Np1.5 O0.5'
_chemical_formula_weight         841.75
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-12-22 deposited with the CCDC.
2017-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6093(10)
_cell_length_b                   14.7125(10)
_cell_length_c                   9.0155(5)
_cell_measurement_reflns_used    7796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.26
_cell_volume                     2998.8(3)
_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-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            27617
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.568
_diffrn_reflns_theta_min         1.651
_exptl_absorpt_coefficient_mu    5.406
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'intense red-brown'
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       quader
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.044
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details
;
 Flack x determined using 2856 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.000(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         7071
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0352P)²+13.1553P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                6479
_reflns_number_total             7071
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7sc00034k2.cif
_cod_data_source_block           mdit67
_cod_depositor_comments
'Adding full bibliography for 1545181--1545185.cif.'
_cod_original_formula_sum        'C32 H35 K1.50 Np1.50 O0.50'
_cod_database_code               1545182
_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   0.797
_shelx_estimated_absorpt_t_max   0.881
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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 0.69506(2) 0.92067(3) 0.39594(4) 0.01667(10) Uani 1 1 d . . . . .
Np2 Np 1.0000 0.86673(4) 1.0000 0.01712(13) Uani 1 2 d S T P . .
K1 K 0.5000 1.1385(2) 0.5000 0.0221(7) Uani 1 2 d S T P . .
K2 K 0.80981(11) 1.09698(16) 0.9138(3) 0.0257(5) Uani 1 1 d . . . . .
C1 C 0.6359(3) 0.7639(6) 0.3010(11) 0.037(3) Uani 1 1 d G . . . .
H1 H 0.5967 0.7573 0.3361 0.17(2) Uiso 1 1 calc R U . . .
C2 C 0.6529(4) 0.8076(6) 0.1675(9) 0.040(3) Uani 1 1 d G . . . .
H2 H 0.6270 0.8354 0.0976 0.17(2) Uiso 1 1 calc R U . . .
C3 C 0.7155(4) 0.8025(6) 0.1568(8) 0.039(3) Uani 1 1 d G . . . .
H3 H 0.7387 0.8263 0.0785 0.17(2) Uiso 1 1 calc R U . . .
C4 C 0.7371(3) 0.7557(6) 0.2837(10) 0.034(3) Uani 1 1 d G . . . .
H4 H 0.7774 0.7426 0.3052 0.17(2) Uiso 1 1 calc R U . . .
C5 C 0.6880(4) 0.7318(6) 0.3728(8) 0.041(3) Uani 1 1 d G . . . .
H5 H 0.6896 0.6999 0.4644 0.17(2) Uiso 1 1 calc R U . . .
C6 C 0.8140(4) 0.8950(6) 0.4910(10) 0.045(4) Uani 1 1 d G . . . .
H6 H 0.8406 0.8672 0.4237 0.17(2) Uiso 1 1 calc R U . . .
C7 C 0.7777(5) 0.8490(5) 0.5949(12) 0.048(4) Uani 1 1 d G . . . .
H7 H 0.7758 0.7851 0.6092 0.17(2) Uiso 1 1 calc R U . . .
C8 C 0.7448(4) 0.9153(9) 0.6736(8) 0.052(4) Uani 1 1 d G . . . .
H8 H 0.7170 0.9036 0.7498 0.17(2) Uiso 1 1 calc R U . . .
C9 C 0.7607(4) 1.0023(6) 0.6184(11) 0.046(4) Uani 1 1 d G . . . .
H9 H 0.7455 1.0589 0.6512 0.17(2) Uiso 1 1 calc R U . . .
C10 C 0.8035(4) 0.9897(5) 0.5056(10) 0.040(3) Uani 1 1 d G . . . .
H10 H 0.8218 1.0365 0.4496 0.17(2) Uiso 1 1 calc R U . . .
C11 C 0.5815(5) 0.9400(8) 0.5161(16) 0.068(6) Uani 1 1 d G . . . .
H11 H 0.5642 0.8881 0.5610 0.17(2) Uiso 1 1 calc R U . . .
C12 C 0.6167(6) 1.0066(11) 0.5891(11) 0.078(7) Uani 1 1 d G . . . .
H12 H 0.6271 1.0069 0.6913 0.17(2) Uiso 1 1 calc R U . . .
C13 C 0.6335(5) 1.0725(7) 0.482(2) 0.074(7) Uani 1 1 d G . . . .
H13 H 0.6572 1.1247 0.5006 0.17(2) Uiso 1 1 calc R U . . .
C14 C 0.6087(6) 1.0467(9) 0.3434(14) 0.074(7) Uani 1 1 d G . . . .
H14 H 0.6129 1.0786 0.2525 0.17(2) Uiso 1 1 calc R U . . .
C15 C 0.5766(4) 0.9648(9) 0.3643(14) 0.063(5) Uani 1 1 d G . . . .
H15 H 0.5555 0.9323 0.2898 0.17(2) Uiso 1 1 calc R U . . .
C16 C 0.7471(4) 1.1120(5) 0.2111(8) 0.035(3) Uani 1 1 d G . . . .
H16 H 0.7721 1.1350 0.2875 0.17(2) Uiso 1 1 calc R U . . .
C17 C 0.7079(4) 1.1638(4) 0.1213(10) 0.041(4) Uani 1 1 d G . . . .
H17 H 0.7019 1.2277 0.1271 0.17(2) Uiso 1 1 calc R U . . .
C18 C 0.6790(3) 1.1036(6) 0.0214(9) 0.038(3) Uani 1 1 d G . . . .
H18 H 0.6503 1.1200 -0.0515 0.17(2) Uiso 1 1 calc R U . . .
C19 C 0.7004(4) 1.0144(5) 0.0494(9) 0.034(3) Uani 1 1 d G . . . .
H19 H 0.6886 0.9608 -0.0014 0.17(2) Uiso 1 1 calc R U . . .
C20 C 0.7425(3) 1.0196(4) 0.1666(8) 0.019(2) Uani 1 1 d G . . . .
H20 H 0.7639 0.9700 0.2081 0.17(2) Uiso 1 1 calc R U . . .
C21 C 1.0314(5) 0.8029(8) 1.2890(11) 0.071(6) Uani 1 1 d G . . . .
H21 H 1.0646 0.8337 1.3301 0.17(2) Uiso 1 1 calc R U . . .
C22 C 1.0334(4) 0.7249(8) 1.1963(13) 0.063(5) Uani 1 1 d G . . . .
H22 H 1.0681 0.6944 1.1646 0.17(2) Uiso 1 1 calc R U . . .
C23 C 0.9743(5) 0.7004(6) 1.1594(10) 0.047(4) Uani 1 1 d G . . . .
H23 H 0.9626 0.6507 1.0987 0.17(2) Uiso 1 1 calc R U . . .
C24 C 0.9359(3) 0.7633(7) 1.2293(11) 0.046(4) Uani 1 1 d G . . . .
H24 H 0.8939 0.7631 1.2235 0.17(2) Uiso 1 1 calc R U . . .
C25 C 0.9712(6) 0.8266(6) 1.3093(9) 0.048(4) Uani 1 1 d G . . . .
H25 H 0.9569 0.8762 1.3665 0.17(2) Uiso 1 1 calc R U . . .
C26 C 0.9155(6) 0.9799(12) 0.8365(13) 0.074(6) Uani 1 1 d G . . . .
H26 H 0.9228 0.9857 0.7333 0.17(2) Uiso 1 1 calc R U . . .
C27 C 0.8814(4) 0.9108(8) 0.905(2) 0.067(6) Uani 1 1 d G . . . .
H27 H 0.8618 0.8622 0.8553 0.17(2) Uiso 1 1 calc R U . . .
C28 C 0.8816(6) 0.9271(13) 1.0600(17) 0.125(12) Uani 1 1 d G . . . .
H28 H 0.8622 0.8913 1.1327 0.17(2) Uiso 1 1 calc R U . . .
C29 C 0.9158(8) 1.0063(14) 1.0877(17) 0.168(19) Uani 1 1 d G . . . .
H29 H 0.9234 1.0327 1.1820 0.17(2) Uiso 1 1 calc R U . . .
C30 C 0.9368(5) 1.0389(7) 0.949(3) 0.114(12) Uani 1 1 d G . . . .
H30 H 0.9609 1.0911 0.9352 0.17(2) Uiso 1 1 calc R U . . .
O1 O 0.4563(11) 0.852(2) 0.104(3) 0.029(7) Uiso 0.25 1 d D . P A 1
C41 C 0.5000 0.872(3) 0.0000 0.053(11) Uiso 0.5 2 d DS . P A 1
C42 C 0.5000 0.967(3) 0.0000 0.052(11) Uiso 0.5 2 d DS . P A 1
C43 C 0.441(2) 0.770(3) 0.170(5) 0.109(16) Uiso 0.25 1 d D . P A 1
C44 C 0.428(2) 0.717(3) 0.294(4) 0.102(15) Uiso 0.25 1 d D . P A 1
O1X O 0.4665(18) 0.664(3) 0.378(4) 0.074(14) Uiso 0.25 1 d D . P B 2
C41X C 0.5000 0.691(3) 0.5000 0.053(12) Uiso 0.5 2 d DS . P B 2
C42X C 0.530(2) 0.613(3) 0.544(5) 0.033(11) Uiso 0.25 1 d D . P B 2
C43X C 0.428(2) 0.717(3) 0.294(4) 0.102(15) Uiso 0.25 1 d . . P B 2
C44X C 0.441(2) 0.770(3) 0.170(5) 0.109(16) Uiso 0.25 1 d . . P B 2
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'
O O 0.0106 0.0060 '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'
K K 0.2009 0.2494 '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
C14 Np1 C8 117.8(4) . .
C14 Np1 C13 30.04(9) . .
C8 Np1 C13 88.3(5) . .
C14 Np1 C20 78.0(2) . .
C8 Np1 C20 122.8(2) . .
C13 Np1 C20 89.1(4) . .
C14 Np1 C9 102.2(4) . .
C8 Np1 C9 29.92(8) . .
C13 Np1 C9 73.2(3) . .
C20 Np1 C9 96.0(3) . .
C14 Np1 C15 29.91(9) . .
C8 Np1 C15 119.5(3) . .
C13 Np1 C15 49.22(11) . .
C20 Np1 C15 100.4(4) . .
C9 Np1 C15 119.2(3) . .
C14 Np1 C7 147.5(4) . .
C8 Np1 C7 29.76(8) . .
C13 Np1 C7 117.6(4) . .
C20 Np1 C7 114.8(3) . .
C9 Np1 C7 48.91(9) . .
C15 Np1 C7 143.0(4) . .
C14 Np1 C5 128.5(4) . .
C8 Np1 C5 93.6(3) . .
C13 Np1 C5 143.3(3) . .
C20 Np1 C5 119.5(2) . .
C9 Np1 C5 121.2(3) . .
C15 Np1 C5 99.8(3) . .
C7 Np1 C5 73.1(2) . .
C14 Np1 C12 49.11(11) . .
C8 Np1 C12 72.7(3) . .
C13 Np1 C12 29.67(9) . .
C20 Np1 C12 118.8(4) . .
C9 Np1 C12 72.0(3) . .
C15 Np1 C12 48.77(11) . .
C7 Np1 C12 101.3(3) . .
C5 Np1 C12 117.4(4) . .
C14 Np1 C1 99.6(4) . .
C8 Np1 C1 116.6(3) . .
C13 Np1 C1 121.0(3) . .
C20 Np1 C1 113.2(2) . .
C9 Np1 C1 146.5(3) . .
C15 Np1 C1 72.7(3) . .
C7 Np1 C1 101.6(3) . .
C5 Np1 C1 29.44(8) . .
C12 Np1 C1 105.1(4) . .
C14 Np1 C4 140.4(4) . .
C8 Np1 C4 99.6(3) . .
C13 Np1 C4 169.0(3) . .
C20 Np1 C4 93.0(2) . .
C9 Np1 C4 117.2(2) . .
C15 Np1 C4 119.8(3) . .
C7 Np1 C4 71.1(3) . .
C5 Np1 C4 29.43(8) . .
C12 Np1 C4 146.7(4) . .
C1 Np1 C4 48.48(10) . .
C14 Np1 C2 92.1(4) . .
C8 Np1 C2 142.0(3) . .
C13 Np1 C2 121.3(3) . .
C20 Np1 C2 83.9(2) . .
C9 Np1 C2 165.4(2) . .
C15 Np1 C2 75.0(3) . .
C7 Np1 C2 118.0(2) . .
C5 Np1 C2 48.45(10) . .
C12 Np1 C2 120.7(3) . .
C1 Np1 C2 29.35(8) . .
C4 Np1 C2 48.37(9) . .
C22 Np2 C22 85.2(5) . 2_757
C22 Np2 C21 28.90(8) . .
C22 Np2 C21 113.0(4) 2_757 .
C22 Np2 C21 113.0(5) . 2_757
C22 Np2 C21 28.9(4) 2_757 2_757
C21 Np2 C21 141.6(5) . 2_757
C22 Np2 C28 110.7(3) . .
C22 Np2 C28 95.8(8) 2_757 .
C21 Np2 C28 99.0(4) . .
C21 Np2 C28 92.7(5) 2_757 .
C22 Np2 C28 95.8(9) . 2_757
C22 Np2 C28 110.7(10) 2_757 2_757
C21 Np2 C28 92.7(10) . 2_757
C21 Np2 C28 99.0(10) 2_757 2_757
C28 Np2 C28 144.0(7) . 2_757
C22 Np2 C27 126.5(4) . .
C22 Np2 C27 74.7(6) 2_757 .
C21 Np2 C27 124.8(4) . .
C21 Np2 C27 65.0(4) 2_757 .
C28 Np2 C27 28.54(9) . .
C28 Np2 C27 137.7(11) 2_757 .
C22 Np2 C27 74.7(8) . 2_757
C22 Np2 C27 126.5(11) 2_757 2_757
C21 Np2 C27 65.0(9) . 2_757
C21 Np2 C27 124.8(11) 2_757 2_757
C28 Np2 C27 137.7(13) . 2_757
C28 Np2 C27 28.54(13) 2_757 2_757
C27 Np2 C27 154.0(7) . 2_757
C22 Np2 C23 28.65(8) . .
C22 Np2 C23 68.6(3) 2_757 .
C21 Np2 C23 47.07(9) . .
C21 Np2 C23 97.2(4) 2_757 .
C28 Np2 C23 88.7(4) . .
C28 Np2 C23 123.0(9) 2_757 .
C27 Np2 C23 98.5(4) . .
C27 Np2 C23 103.4(8) 2_757 .
C22 Np2 C23 68.6(6) . 2_757
C22 Np2 C23 28.6(3) 2_757 2_757
C21 Np2 C23 97.2(6) . 2_757
C21 Np2 C23 47.1(4) 2_757 2_757
C28 Np2 C23 123.0(7) . 2_757
C28 Np2 C23 88.7(9) 2_757 2_757
C27 Np2 C23 103.4(6) . 2_757
C27 Np2 C23 98.5(11) 2_757 2_757
C23 Np2 C23 64.8(3) . 2_757
C22 Np2 C29 121.1(8) . 2_757
C22 Np2 C29 121.4(10) 2_757 2_757
C21 Np2 C29 108.7(10) . 2_757
C21 Np2 C29 98.2(10) 2_757 2_757
C28 Np2 C29 116.4(5) . 2_757
C28 Np2 C29 28.4(4) 2_757 2_757
C27 Np2 C29 111.6(8) . 2_757
C27 Np2 C29 46.7(6) 2_757 2_757
C23 Np2 C29 149.7(7) . 2_757
C23 Np2 C29 109.1(8) 2_757 2_757
C22 Np2 C29 121.4(5) . .
C22 Np2 C29 121.1(6) 2_757 .
C21 Np2 C29 98.2(4) . .
C21 Np2 C29 108.7(3) 2_757 .
C28 Np2 C29 28.39(9) . .
C28 Np2 C29 116.4(9) 2_757 .
C27 Np2 C29 46.70(10) . .
C27 Np2 C29 111.6(11) 2_757 .
C23 Np2 C29 109.1(6) . .
C23 Np2 C29 149.7(7) 2_757 .
C29 Np2 C29 90.4(8) 2_757 .
C22 K1 C22 132(4) 4_657 3_454
C22 K1 C14 65.6(11) 4_657 2_656
C22 K1 C14 139.8(16) 3_454 2_656
C22 K1 C14 139.8(14) 4_657 .
C22 K1 C14 65.6(14) 3_454 .
C14 K1 C14 129.2(7) 2_656 .
C22 K1 C21 26(2) 4_657 4_657
C22 K1 C21 105.9(19) 3_454 4_657
C14 K1 C21 83.0(7) 2_656 4_657
C14 K1 C21 141.1(4) . 4_657
C22 K1 C21 105.9(17) 4_657 3_454
C22 K1 C21 26(2) 3_454 3_454
C14 K1 C21 141.1(8) 2_656 3_454
C14 K1 C21 83.0(3) . 3_454
C21 K1 C21 80.2(5) 4_657 3_454
C22 K1 C13 81.0(9) 4_657 2_656
C22 K1 C13 113.9(15) 3_454 2_656
C14 K1 C13 25.95(17) 2_656 2_656
C14 K1 C13 129.6(10) . 2_656
C21 K1 C13 89.2(8) 4_657 2_656
C21 K1 C13 118.8(8) 3_454 2_656
C22 K1 C13 113.9(13) 4_657 .
C22 K1 C13 81.0(11) 3_454 .
C14 K1 C13 129.6(9) 2_656 .
C14 K1 C13 25.95(7) . .
C21 K1 C13 118.8(3) 4_657 .
C21 K1 C13 89.2(4) 3_454 .
C13 K1 C13 144.4(8) 2_656 .
C22 K1 C23 25.7(7) 4_657 4_657
C22 K1 C23 132(3) 3_454 4_657
C14 K1 C23 80.3(12) 2_656 4_657
C14 K1 C23 114.2(14) . 4_657
C21 K1 C23 42.0(18) 4_657 4_657
C21 K1 C23 108.3(13) 3_454 4_657
C13 K1 C23 101.6(12) 2_656 4_657
C13 K1 C23 88.3(14) . 4_657
C22 K1 C23 132(4) 4_657 3_454
C22 K1 C23 25.7(6) 3_454 3_454
C14 K1 C23 114.2(19) 2_656 3_454
C14 K1 C23 80.3(17) . 3_454
C21 K1 C23 108(2) 4_657 3_454
C21 K1 C23 42(2) 3_454 3_454
C13 K1 C23 88.3(19) 2_656 3_454
C13 K1 C23 101.6(16) . 3_454
C23 K1 C23 147(4) 4_657 3_454
C22 K1 C15 140(2) 4_657 .
C22 K1 C15 82.0(18) 3_454 .
C14 K1 C15 104.2(7) 2_656 .
C14 K1 C15 25.16(7) . .
C21 K1 C15 158.3(2) 4_657 .
C21 K1 C15 104.3(4) 3_454 .
C13 K1 C15 106.3(9) 2_656 .
C13 K1 C15 41.32(8) . .
C23 K1 C15 118.2(17) 4_657 .
C23 K1 C15 87.6(19) 3_454 .
C22 K1 C15 82.0(15) 4_657 2_656
C22 K1 C15 140(2) 3_454 2_656
C14 K1 C15 25.2(4) 2_656 2_656
C14 K1 C15 104.2(5) . 2_656
C21 K1 C15 104.3(5) 4_657 2_656
C21 K1 C15 158.3(7) 3_454 2_656
C13 K1 C15 41.3(5) 2_656 2_656
C13 K1 C15 106.3(6) . 2_656
C23 K1 C15 87.6(14) 4_657 2_656
C23 K1 C15 118(2) 3_454 2_656
C15 K1 C15 79.6(5) . 2_656
C20 K2 C30 107.6(10) 1_556 .
C20 K2 C19 27.4(4) 1_556 1_556
C30 K2 C19 128.7(8) . 1_556
C20 K2 C26 111.5(10) 1_556 .
C30 K2 C26 27.18(9) . .
C19 K2 C26 120.9(9) 1_556 .
C20 K2 C16 27.2(8) 1_556 1_556
C30 K2 C16 112.0(5) . 1_556
C19 K2 C16 44.5(5) 1_556 1_556
C26 K2 C16 128.0(3) . 1_556
C20 K2 C4 123.4(14) 1_556 4_656
C30 K2 C4 126.4(10) . 4_656
C19 K2 C4 104.8(12) 1_556 4_656
C26 K2 C4 124.0(10) . 4_656
C16 K2 C4 106.8(10) 1_556 4_656
C20 K2 C18 44.2(6) 1_556 1_556
C30 K2 C18 151.7(7) . 1_556
C19 K2 C18 26.7(4) 1_556 1_556
C26 K2 C18 147.1(9) . 1_556
C16 K2 C18 43.7(3) 1_556 1_556
C4 K2 C18 80.5(12) 4_656 1_556
C20 K2 C17 44.1(6) 1_556 1_556
C30 K2 C17 136.8(8) . 1_556
C19 K2 C17 43.8(6) 1_556 1_556
C26 K2 C17 154.0(7) . 1_556
C16 K2 C17 26.5(6) 1_556 1_556
C4 K2 C17 81.8(12) 4_656 1_556
C18 K2 C17 26.2(4) 1_556 1_556
C20 K2 C3 115.5(14) 1_556 4_656
C30 K2 C3 117.8(11) . 4_656
C19 K2 C3 108.7(14) 1_556 4_656
C26 K2 C3 130.0(11) . 4_656
C16 K2 C3 91.3(10) 1_556 4_656
C4 K2 C3 26.22(9) 4_656 4_656
C18 K2 C3 82.0(14) 1_556 4_656
C17 K2 C3 71.7(14) 1_556 4_656
C20 K2 C29 81.3(11) 1_556 .
C30 K2 C29 26.52(9) . .
C19 K2 C29 104.5(9) 1_556 .
C26 K2 C29 43.58(10) . .
C16 K2 C29 87.1(4) 1_556 .
C4 K2 C29 148.9(11) 4_656 .
C18 K2 C29 125.3(7) 1_556 .
C17 K2 C29 113.3(7) 1_556 .
C3 K2 C29 130.2(11) 4_656 .
C20 K2 C27 87.3(10) 1_556 .
C30 K2 C27 43.44(10) . .
C19 K2 C27 94.7(9) 1_556 .
C26 K2 C27 26.28(9) . .
C16 K2 C27 108.9(4) 1_556 .
C4 K2 C27 143.2(10) 4_656 .
C18 K2 C27 121.2(8) 1_556 .
C17 K2 C27 131.4(9) 1_556 .
C3 K2 C27 156.2(11) 4_656 .
C29 K2 C27 42.53(10) . .
C20 K2 C9 107.2(9) 1_556 .
C30 K2 C9 106.9(4) . .
C19 K2 C9 83.2(6) 1_556 .
C26 K2 C9 80.2(4) . .
C16 K2 C9 127.1(2) 1_556 .
C4 K2 C9 74.7(9) 4_656 .
C18 K2 C9 87.0(6) 1_556 .
C17 K2 C9 112.4(8) 1_556 .
C3 K2 C9 100.9(10) 4_656 .
C29 K2 C9 119.2(3) . .
C27 K2 C9 77.1(3) . .
C5 C1 C2 108.0 . .
C5 C1 Np1 75.1(3) . .
C2 C1 Np1 75.8(3) . .
C5 C1 K2 73.5(3) . 4_646
C2 C1 K2 75.0(3) . 4_646
Np1 C1 K2 127.1(2) . 4_646
C3 C2 C1 108.0 . .
C3 C2 Np1 75.4(3) . .
C1 C2 Np1 74.9(3) . .
C3 C2 K2 71.3(3) . 4_646
C1 C2 K2 80.4(3) . 4_646
Np1 C2 K2 129.3(2) . 4_646
C2 C3 C4 108.0 . .
C2 C3 Np1 75.3(3) . .
C4 C3 Np1 74.9(3) . .
C2 C3 K2 83.4(4) . 4_646
C4 C3 K2 75.9(4) . 4_646
Np1 C3 K2 136.1(2) . 4_646
C3 C4 C5 108.0 . .
C3 C4 Np1 75.8(3) . .
C5 C4 Np1 75.0(3) . .
C3 C4 K2 77.8(4) . 4_646
C5 C4 K2 82.7(4) . 4_646
Np1 C4 K2 137.8(2) . 4_646
C1 C5 C4 108.0 . .
C1 C5 Np1 75.5(3) . .
C4 C5 Np1 75.6(3) . .
C1 C5 K2 81.9(3) . 4_646
C4 C5 K2 71.7(3) . 4_646
Np1 C5 K2 131.6(2) . 4_646
C7 C6 C10 108.0 . .
C7 C6 Np1 73.3(3) . .
C10 C6 Np1 74.9(4) . .
C6 C7 C8 108.0 . .
C6 C7 Np1 77.5(3) . .
C8 C7 Np1 73.2(4) . .
C9 C8 C7 108.0 . .
C9 C8 Np1 76.0(4) . .
C7 C8 Np1 77.1(4) . .
C8 C9 C10 108.0 . .
C8 C9 Np1 74.1(3) . .
C10 C9 Np1 77.8(3) . .
C8 C9 K2 100.8(5) . .
C10 C9 K2 114.8(5) . .
Np1 C9 K2 167.4(4) . .
C6 C10 C9 108.0 . .
C6 C10 Np1 76.1(4) . .
C9 C10 Np1 72.8(3) . .
C15 C11 C12 108.0 . .
C15 C11 Np1 73.7(4) . .
C12 C11 Np1 74.8(4) . .
C15 C11 K1 72.8(4) . .
C12 C11 K1 74.5(4) . .
Np1 C11 K1 123.9(3) . .
C13 C12 C11 108.0 . .
C13 C12 Np1 73.3(4) . .
C11 C12 Np1 75.8(4) . .
C13 C12 K1 70.0(4) . .
C11 C12 K1 81.5(4) . .
Np1 C12 K1 127.7(3) . .
C12 C13 C14 108.0 . .
C12 C13 Np1 77.0(4) . .
C14 C13 Np1 74.3(4) . .
C12 C13 K1 85.1(4) . .
C14 C13 K1 75.9(4) . .
Np1 C13 K1 138.3(4) . .
C13 C14 C15 108.0 . .
C13 C14 Np1 75.6(4) . .
C15 C14 Np1 76.5(4) . .
C13 C14 K1 78.1(4) . .
C15 C14 K1 84.4(4) . .
Np1 C14 K1 140.6(4) . .
C11 C15 C14 108.0 . .
C11 C15 Np1 76.8(4) . .
C14 C15 Np1 73.5(4) . .
C11 C15 K1 83.1(4) . .
C14 C15 K1 70.5(4) . .
Np1 C15 K1 130.4(3) . .
C20 C16 C17 108.0 . .
C20 C16 K2 73.5(3) . 1_554
C17 C16 K2 80.2(3) . 1_554
C18 C17 C16 108.0 . .
C18 C17 K2 76.2(3) . 1_554
C16 C17 K2 73.3(3) . 1_554
C17 C18 C19 108.0 . .
C17 C18 K2 77.5(3) . 1_554
C19 C18 K2 72.8(3) . 1_554
C20 C19 C18 108.0 . .
C20 C19 K2 74.5(3) . 1_554
C18 C19 K2 80.6(3) . 1_554
C19 C20 C16 108.0 . .
C19 C20 Np1 105.5(4) . .
C16 C20 Np1 108.8(4) . .
C19 C20 K2 78.1(3) . 1_554
C16 C20 K2 79.3(3) . 1_554
Np1 C20 K2 169.0(2) . 1_554
C25 C21 C22 108.0 . .
C25 C21 Np2 78.7(4) . .
C22 C21 Np2 74.8(4) . .
C25 C21 K1 83.7(4) . 3_546
C22 C21 K1 75.2(4) . 3_546
Np2 C21 K1 138.2(3) . 3_546
C23 C22 C21 108.0 . .
C23 C22 Np2 78.1(4) . .
C21 C22 Np2 76.3(4) . .
C23 C22 K1 82.5(4) . 3_546
C21 C22 K1 78.7(4) . 3_546
Np2 C22 K1 141.6(3) . 3_546
C24 C23 C22 108.0 . .
C24 C23 Np2 78.2(4) . .
C22 C23 Np2 73.2(4) . .
C24 C23 K1 82.5(4) . 3_546
C22 C23 K1 71.9(4) . 3_546
Np2 C23 K1 132.1(3) . 3_546
C23 C24 C25 108.0 . .
C23 C24 Np2 73.7(4) . .
C25 C24 Np2 75.0(3) . .
C23 C24 K1 72.8(4) . 3_546
C25 C24 K1 75.7(4) . 3_546
Np2 C24 K1 125.2(2) . 3_546
C21 C25 C24 108.0 . .
C21 C25 Np2 72.9(4) . .
C24 C25 Np2 77.1(3) . .
C21 C25 K1 71.1(4) . 3_546
C24 C25 K1 79.9(4) . 3_546
Np2 C25 K1 128.1(3) . 3_546
C27 C26 C30 108.0 . .
C27 C26 Np2 74.3(4) . .
C30 C26 Np2 76.7(4) . .
C27 C26 K2 82.8(5) . .
C30 C26 K2 75.6(5) . .
Np2 C26 K2 136.1(4) . .
C28 C27 C26 108.0 . .
C28 C27 Np2 75.4(4) . .
C26 C27 Np2 77.5(4) . .
C28 C27 K2 80.1(4) . .
C26 C27 K2 70.9(4) . .
Np2 C27 K2 131.1(4) . .
C27 C28 C29 108.0 . .
C27 C28 Np2 76.0(4) . .
C29 C28 Np2 77.2(4) . .
C27 C28 K2 74.5(4) . .
C29 C28 K2 73.2(4) . .
Np2 C28 K2 128.5(4) . .
C30 C29 C28 108.0 . .
C30 C29 Np2 77.1(4) . .
C28 C29 Np2 74.4(4) . .
C30 C29 K2 71.2(5) . .
C28 C29 K2 81.3(4) . .
Np2 C29 K2 131.3(4) . .
C29 C30 C26 108.0 . .
C29 C30 Np2 74.8(4) . .
C26 C30 Np2 75.3(4) . .
C29 C30 K2 82.3(5) . .
C26 C30 K2 77.2(5) . .
Np2 C30 K2 136.3(4) . .
C41 O1 C43 130(4) . .
O1 C41 O1 156(5) 2_655 .
O1 C41 C42 102(2) 2_655 .
O1 C41 C42 102(2) . .
O1 C43 C44 153(5) . .
C42X O1X C41X 68.2(15) 2_656 .
O1X C41X O1X 147(5) . 2_656
O1X C41X C42X 105(4) . .
O1X C41X C42X 44(3) 2_656 .
O1X C41X C42X 44(3) . 2_656
O1X C41X C42X 105(4) 2_656 2_656
C42X C41X C42X 69(5) . 2_656
O1X C42X C41X 68.2(15) 2_656 .
O1X C42X C42X 114(4) 2_656 2_656
C41X C42X C42X 56(2) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Np1 C14 2.731(10) .
Np1 C8 2.738(8) .
Np1 C13 2.747(10) .
Np1 C20 2.753(7) .
Np1 C9 2.762(9) .
Np1 C15 2.769(9) .
Np1 C7 2.788(9) .
Np1 C5 2.791(9) .
Np1 C12 2.796(10) .
Np1 C1 2.797(9) .
Np1 C4 2.800(8) .
Np1 C2 2.809(9) .
Np2 C22 2.835(9) .
Np2 C22 2.84(2) 2_757
Np2 C21 2.855(9) .
Np2 C21 2.855(9) 2_757
Np2 C28 2.876(11) .
Np2 C28 2.876(15) 2_757
Np2 C27 2.884(10) .
Np2 C27 2.884(7) 2_757
Np2 C23 2.898(9) .
Np2 C23 2.90(2) 2_757
Np2 C29 2.91(3) 2_757
Np2 C29 2.912(11) .
K1 C22 3.12(9) 4_657
K1 C22 3.12(9) 3_454
K1 C14 3.148(15) 2_656
K1 C14 3.148(10) .
K1 C21 3.161(10) 4_657
K1 C21 3.161(10) 3_454
K1 C13 3.176(8) 2_656
K1 C13 3.176(11) .
K1 C23 3.25(8) 4_657
K1 C23 3.25(7) 3_454
K1 C15 3.324(11) .
K1 C15 3.32(3) 2_656
K2 C20 2.98(4) 1_556
K2 C30 3.011(11) .
K2 C19 3.02(5) 1_556
K2 C26 3.031(11) .
K2 C16 3.049(8) 1_556
K2 C4 3.117(11) 4_656
K2 C18 3.12(5) 1_556
K2 C17 3.14(4) 1_556
K2 C3 3.14(2) 4_656
K2 C29 3.151(11) .
K2 C27 3.183(11) .
K2 C9 3.197(9) .
C1 C5 1.4200 .
C1 C2 1.4200 .
C1 K2 3.364(9) 4_646
C2 C3 1.4200 .
C2 K2 3.295(9) 4_646
C3 C4 1.4200 .
C3 K2 3.142(9) 4_646
C4 C5 1.4200 .
C4 K2 3.118(9) 4_646
C5 K2 3.258(9) 4_646
C6 C7 1.4200 .
C6 C10 1.4200 .
C7 C8 1.4200 .
C8 C9 1.4200 .
C9 C10 1.4200 .
C11 C15 1.4200 .
C11 C12 1.4200 .
C12 C13 1.4200 .
C13 C14 1.4200 .
C14 C15 1.4200 .
C16 C20 1.4200 .
C16 C17 1.4200 .
C16 K2 3.049(8) 1_554
C17 C18 1.4200 .
C17 K2 3.138(8) 1_554
C18 C19 1.4200 .
C18 K2 3.121(9) 1_554
C19 C20 1.4200 .
C19 K2 3.022(9) 1_554
C20 K2 2.976(8) 1_554
C21 C25 1.4200 .
C21 C22 1.4200 .
C21 K1 3.161(10) 3_546
C22 C23 1.4200 .
C22 K1 3.116(10) 3_546
C23 C24 1.4200 .
C23 K1 3.251(9) 3_546
C24 C25 1.4200 .
C24 K1 3.374(10) 3_546
C25 K1 3.321(10) 3_546
C26 C27 1.4200 .
C26 C30 1.4200 .
C27 C28 1.4200 .
C28 C29 1.4200 .
C29 C30 1.4200 .
O1 C41 1.394(15) .
O1 C43 1.394(16) .
C41 O1 1.394(15) 2_655
C41 C42 1.395(17) .
C43 C44 1.395(16) .
O1X C42X 1.03(6) 2_656
O1X C41X 1.387(16) .
C41X O1X 1.387(16) 2_656
C41X C42X 1.388(17) .
C41X C42X 1.388(17) 2_656
C42X O1X 1.03(6) 2_656
C42X C42X 1.56(9) 2_656
