#------------------------------------------------------------------------------
#$Date: 2023-05-05 05:13:46 +0300 (Fri, 05 May 2023) $
#$Revision: 283295 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/21/7712153.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_7712153
loop_
_publ_author_name
'Kudo, Eiji'
'Oba, Yuki'
'Yamamoto, Koji'
'Murahashi, Tetsuro'
_publ_section_title
;
 Di- and trinuclear sandwich complexes of a cross-conjugated fulvene.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1568
_journal_page_last               1573
_journal_paper_doi               10.1039/d2dt03521a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C44 H40 N4 Pd3, 2(B F4), 1[CH3CN]'
_chemical_formula_sum            'C46 H43 B2 F8 N5 Pd3'
_chemical_formula_weight         1158.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-28
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2022-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.5900(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2396(6)
_cell_length_b                   18.0521(7)
_cell_length_c                   15.9775(7)
_cell_measurement_reflns_used    45129
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.03
_cell_volume                     4712.9(3)
_computing_cell_refinement       'RAPID AUTO (Rigaku, ????)'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO (Rigaku, ????)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69046
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.029
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.230
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10667
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0560
_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)+(0.0952P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7513
_reflns_number_total             10667
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt03521a2.cif
_cod_data_source_block           shelxl_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7712149--7712153.cif.'
_cod_database_code               7712153
_shelx_shelxl_version_number     2018/3
_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_max   0.831
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups
2. Restrained distances
 B1-F1 = B1-F2 = B1-F3 = B1-F4
 1.37 with sigma of 0.02
 B2-F5 = B2-F6 = B2-F7 = B2-F8
 1.37 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B2 \\sim F5 \\sim F6 \\sim F7 \\sim F8: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(B2) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim
Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36)
4.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 128 electrons were 
found in a volume of 484Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
1[CH3CN] per Asymmetric Unit 
which account for 88 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Pd1 Pd 0.65105(2) 0.75465(2) 0.81871(3) 0.03978(13) Uani 1 1 d . . . . .
Pd2 Pd 0.79539(2) 0.77151(2) 0.92435(3) 0.03688(12) Uani 1 1 d . . . . .
Pd3 Pd 0.67784(2) 0.56198(2) 1.04445(3) 0.03791(13) Uani 1 1 d . . . . .
F1 F 0.4187(7) 0.7573(7) 0.4212(13) 0.311(9) Uani 1 1 d D . . . .
F2 F 0.2950(4) 0.7981(5) 0.4197(6) 0.202(5) Uani 1 1 d D . . . .
F3 F 0.3171(15) 0.7670(6) 0.2945(6) 0.384(13) Uani 1 1 d D . . . .
F4 F 0.3049(6) 0.6822(4) 0.3940(6) 0.196(4) Uani 1 1 d D . . . .
F5 F 0.3820(7) 0.5093(7) 0.6888(7) 0.227(4) Uani 1 1 d D U . . .
F6 F 0.4818(7) 0.4247(7) 0.7029(11) 0.312(9) Uani 1 1 d D U . . .
F7 F 0.4755(6) 0.5207(9) 0.6287(8) 0.289(7) Uani 1 1 d D U . . .
F8 F 0.5093(9) 0.5353(8) 0.7739(11) 0.384(12) Uani 1 1 d D U . . .
N1 N 0.5369(3) 0.7258(3) 0.7287(4) 0.0566(13) Uani 1 1 d . . . . .
N2 N 0.9193(3) 0.7691(3) 1.0001(3) 0.0488(11) Uani 1 1 d . . . . .
N3 N 0.5614(3) 0.5774(3) 1.0572(3) 0.0497(11) Uani 1 1 d . . . . .
N4 N 0.7106(3) 0.4865(3) 1.1487(4) 0.0612(14) Uani 1 1 d . . . . .
C1 C 0.6567(3) 0.6309(3) 0.9268(3) 0.0378(11) Uani 1 1 d . . . . .
H1 H 0.628215 0.588586 0.897009 0.045 Uiso 1 1 calc R U . . .
C2 C 0.6218(3) 0.7052(3) 0.9265(3) 0.0388(11) Uani 1 1 d . . . . .
H2 H 0.567967 0.720820 0.893920 0.047 Uiso 1 1 calc R U . . .
C3 C 0.6841(3) 0.7489(3) 0.9843(3) 0.0400(11) Uani 1 1 d . . . . .
H3 H 0.677501 0.798863 0.999412 0.048 Uiso 1 1 calc R U . . .
C4 C 0.7584(3) 0.7075(3) 1.0170(3) 0.0356(10) Uani 1 1 d . . . . .
H4 H 0.809209 0.724953 1.055561 0.043 Uiso 1 1 calc R U . . .
C5 C 0.7410(3) 0.6333(3) 0.9795(3) 0.0364(10) Uani 1 1 d . . . . .
C6 C 0.7861(3) 0.5656(3) 1.0062(3) 0.0325(10) Uani 1 1 d . . . . .
C7 C 0.8699(3) 0.5690(3) 1.0755(3) 0.0347(10) Uani 1 1 d . . . . .
C8 C 0.8829(3) 0.5664(3) 1.1648(4) 0.0453(13) Uani 1 1 d . . . . .
H8 H 0.837403 0.566314 1.186071 0.054 Uiso 1 1 calc R U . . .
C9 C 0.9615(4) 0.5640(3) 1.2243(4) 0.0525(14) Uani 1 1 d . . . . .
H9 H 0.968778 0.560597 1.285708 0.063 Uiso 1 1 calc R U . . .
C10 C 1.0282(3) 0.5665(3) 1.1969(4) 0.0496(14) Uani 1 1 d . . . . .
H10 H 1.081709 0.564984 1.238376 0.059 Uiso 1 1 calc R U . . .
C11 C 1.0169(3) 0.5714(3) 1.1073(4) 0.0499(14) Uani 1 1 d . . . . .
H11 H 1.062814 0.574429 1.086800 0.060 Uiso 1 1 calc R U . . .
C12 C 0.9380(3) 0.5717(3) 1.0474(4) 0.0433(12) Uani 1 1 d . . . . .
H12 H 0.930692 0.573785 0.985946 0.052 Uiso 1 1 calc R U . . .
C13 C 0.7755(3) 0.5030(3) 0.9433(3) 0.0366(11) Uani 1 1 d . . . . .
C14 C 0.7817(3) 0.4296(3) 0.9733(4) 0.0418(12) Uani 1 1 d . . . . .
H14 H 0.792260 0.420168 1.034380 0.050 Uiso 1 1 calc R U . . .
C15 C 0.7729(3) 0.3711(3) 0.9164(4) 0.0534(15) Uani 1 1 d . . . . .
H15 H 0.776872 0.321770 0.938132 0.064 Uiso 1 1 calc R U . . .
C16 C 0.7579(3) 0.3842(4) 0.8264(5) 0.0586(17) Uani 1 1 d . . . . .
H16 H 0.751218 0.343637 0.786776 0.070 Uiso 1 1 calc R U . . .
C17 C 0.7528(4) 0.4551(4) 0.7953(4) 0.0595(16) Uani 1 1 d . . . . .
H17 H 0.744159 0.463873 0.734355 0.071 Uiso 1 1 calc R U . . .
C18 C 0.7604(3) 0.5143(3) 0.8526(4) 0.0459(13) Uani 1 1 d . . . . .
H18 H 0.755232 0.563432 0.830072 0.055 Uiso 1 1 calc R U . . .
C19 C 0.7047(3) 0.7876(3) 0.7135(4) 0.0462(13) Uani 1 1 d . . . . .
H19 H 0.662153 0.764119 0.668184 0.055 Uiso 1 1 calc R U . . .
C20 C 0.6958(4) 0.8504(3) 0.7589(4) 0.0499(13) Uani 1 1 d . . . . .
H20 H 0.646799 0.877894 0.749685 0.060 Uiso 1 1 calc R U . . .
C21 C 0.7752(4) 0.8670(3) 0.8235(4) 0.0503(14) Uani 1 1 d . . . . .
H21 H 0.785806 0.906482 0.864888 0.060 Uiso 1 1 calc R U . . .
C22 C 0.8325(3) 0.8164(3) 0.8154(4) 0.0451(12) Uani 1 1 d . . . . .
H22 H 0.889018 0.816314 0.848617 0.054 Uiso 1 1 calc R U . . .
C23 C 0.7908(3) 0.7627(3) 0.7464(4) 0.0415(12) Uani 1 1 d . . . . .
C24 C 0.8259(3) 0.7011(3) 0.7239(3) 0.0410(11) Uani 1 1 d . . . . .
C25 C 0.7807(3) 0.6410(3) 0.6650(3) 0.0420(12) Uani 1 1 d . . . . .
C26 C 0.7001(3) 0.6221(3) 0.6602(4) 0.0486(13) Uani 1 1 d . . . . .
H26 H 0.674410 0.646605 0.696941 0.058 Uiso 1 1 calc R U . . .
C27 C 0.6581(4) 0.5675(4) 0.6017(5) 0.0682(19) Uani 1 1 d . . . . .
H27 H 0.603689 0.554798 0.598397 0.082 Uiso 1 1 calc R U . . .
C28 C 0.6955(5) 0.5322(4) 0.5487(5) 0.0705(19) Uani 1 1 d . . . . .
H28 H 0.666386 0.495908 0.507587 0.085 Uiso 1 1 calc R U . . .
C29 C 0.7766(5) 0.5493(4) 0.5551(5) 0.0666(18) Uani 1 1 d . . . . .
H29 H 0.802599 0.523864 0.519312 0.080 Uiso 1 1 calc R U . . .
C30 C 0.8184(4) 0.6028(3) 0.6132(4) 0.0500(13) Uani 1 1 d . . . . .
H30 H 0.873565 0.613740 0.617954 0.060 Uiso 1 1 calc R U . . .
C31 C 0.9166(3) 0.6923(3) 0.7626(3) 0.0424(12) Uani 1 1 d . . . . .
C32 C 0.9502(3) 0.6294(3) 0.8122(4) 0.0496(13) Uani 1 1 d . . . . .
H32 H 0.915328 0.590138 0.817407 0.060 Uiso 1 1 calc R U . . .
C33 C 1.0331(3) 0.6242(3) 0.8535(4) 0.0573(16) Uani 1 1 d . . . . .
H33 H 1.054906 0.581908 0.888523 0.069 Uiso 1 1 calc R U . . .
C34 C 1.0851(4) 0.6796(4) 0.8447(5) 0.0621(17) Uani 1 1 d . . . . .
H34 H 1.142293 0.676079 0.874570 0.075 Uiso 1 1 calc R U . . .
C35 C 1.0535(4) 0.7397(4) 0.7925(5) 0.0660(19) Uani 1 1 d . . . . .
H35 H 1.089438 0.776826 0.784305 0.079 Uiso 1 1 calc R U . . .
C36 C 0.9691(4) 0.7470(3) 0.7512(4) 0.0538(15) Uani 1 1 d . . . . .
H36 H 0.947887 0.789088 0.715499 0.065 Uiso 1 1 calc R U . . .
C37 C 0.4762(4) 0.7071(5) 0.6855(6) 0.082(2) Uani 1 1 d . . . . .
C38 C 0.3947(6) 0.6817(7) 0.6296(9) 0.153(5) Uani 1 1 d . . . . .
H38A H 0.353657 0.719254 0.629693 0.184 Uiso 1 1 calc R U . . .
H38B H 0.381121 0.635029 0.652847 0.184 Uiso 1 1 calc R U . . .
H38C H 0.395284 0.674160 0.569017 0.184 Uiso 1 1 calc R U . . .
C39 C 0.9870(4) 0.7745(4) 1.0322(5) 0.0652(18) Uani 1 1 d . . . . .
C40 C 1.0764(5) 0.7793(7) 1.0741(8) 0.131(4) Uani 1 1 d . . . . .
H40A H 1.088666 0.793940 1.136035 0.157 Uiso 1 1 calc R U . . .
H40B H 1.098680 0.816315 1.043103 0.157 Uiso 1 1 calc R U . . .
H40C H 1.101138 0.730981 1.070974 0.157 Uiso 1 1 calc R U . . .
C41 C 0.5009(3) 0.5868(3) 1.0678(4) 0.0517(14) Uani 1 1 d . . . . .
C42 C 0.4229(4) 0.6023(4) 1.0817(6) 0.072(2) Uani 1 1 d . . . . .
H42A H 0.390958 0.636426 1.035880 0.086 Uiso 1 1 calc R U . . .
H42B H 0.432834 0.624963 1.139898 0.086 Uiso 1 1 calc R U . . .
H42C H 0.392433 0.556007 1.078511 0.086 Uiso 1 1 calc R U . . .
C43 C 0.7377(5) 0.4550(4) 1.2134(6) 0.077(2) Uani 1 1 d . . . . .
C44 C 0.7744(7) 0.4148(6) 1.2973(7) 0.127(4) Uani 1 1 d . . . . .
H44A H 0.751220 0.364765 1.292312 0.152 Uiso 1 1 calc R U . . .
H44B H 0.762644 0.441360 1.345299 0.152 Uiso 1 1 calc R U . . .
H44C H 0.833795 0.411447 1.309814 0.152 Uiso 1 1 calc R U . . .
B1 B 0.3327(9) 0.7524(7) 0.3805(9) 0.145(6) Uani 1 1 d D . . . .
B2 B 0.4640(9) 0.4946(10) 0.7038(10) 0.177(9) Uani 1 1 d D 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Pd Pd -0.9988 1.0072 '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
_geom_angle_publ_flag
N1 Pd1 Pd2 172.03(15) . . ?
N1 Pd1 C2 92.2(2) . . ?
N1 Pd1 C3 123.84(19) . . ?
N1 Pd1 C19 94.1(2) . . ?
N1 Pd1 C20 106.0(2) . . ?
C2 Pd1 Pd2 86.99(14) . . ?
C2 Pd1 C3 33.99(18) . . ?
C2 Pd1 C19 167.04(19) . . ?
C2 Pd1 C20 150.7(2) . . ?
C3 Pd1 Pd2 57.52(12) . . ?
C19 Pd1 Pd2 85.17(15) . . ?
C19 Pd1 C3 142.0(2) . . ?
C20 Pd1 Pd2 78.02(16) . . ?
C20 Pd1 C3 119.2(2) . . ?
C20 Pd1 C19 36.0(2) . . ?
N2 Pd2 Pd1 169.89(13) . . ?
N2 Pd2 C3 123.74(18) . . ?
N2 Pd2 C4 93.63(19) . . ?
N2 Pd2 C21 108.6(2) . . ?
N2 Pd2 C22 88.0(2) . . ?
C3 Pd2 Pd1 60.91(12) . . ?
C4 Pd2 Pd1 87.12(13) . . ?
C4 Pd2 C3 35.71(18) . . ?
C4 Pd2 C21 151.42(19) . . ?
C4 Pd2 C22 168.6(2) . . ?
C21 Pd2 Pd1 74.19(16) . . ?
C21 Pd2 C3 115.89(19) . . ?
C22 Pd2 Pd1 89.34(15) . . ?
C22 Pd2 C3 147.09(19) . . ?
C22 Pd2 C21 35.6(2) . . ?
N3 Pd3 C1 96.08(18) . . ?
N3 Pd3 C5 127.85(19) . . ?
N3 Pd3 C6 166.05(18) . . ?
N4 Pd3 N3 91.89(19) . . ?
N4 Pd3 C1 170.77(19) . . ?
N4 Pd3 C5 136.47(19) . . ?
N4 Pd3 C6 102.06(18) . . ?
C5 Pd3 C1 38.45(17) . . ?
C6 Pd3 C1 70.03(17) . . ?
C6 Pd3 C5 39.11(18) . . ?
C37 N1 Pd1 175.1(6) . . ?
C39 N2 Pd2 170.4(6) . . ?
C41 N3 Pd3 176.8(5) . . ?
C43 N4 Pd3 167.8(6) . . ?
Pd3 C1 H1 83.7 . . ?
C2 C1 Pd3 118.5(3) . . ?
C2 C1 H1 125.9 . . ?
C5 C1 Pd3 69.6(3) . . ?
C5 C1 H1 125.9 . . ?
C5 C1 C2 108.2(4) . . ?
Pd1 C2 H2 82.8 . . ?
C1 C2 Pd1 100.4(3) . . ?
C1 C2 H2 126.8 . . ?
C3 C2 Pd1 88.2(3) . . ?
C3 C2 C1 106.4(4) . . ?
C3 C2 H2 126.8 . . ?
Pd1 C3 H3 102.8 . . ?
Pd2 C3 Pd1 61.57(12) . . ?
Pd2 C3 H3 96.5 . . ?
C2 C3 Pd1 57.8(3) . . ?
C2 C3 Pd2 111.5(3) . . ?
C2 C3 H3 124.7 . . ?
C2 C3 C4 110.7(5) . . ?
C4 C3 Pd1 106.3(3) . . ?
C4 C3 Pd2 60.3(3) . . ?
C4 C3 H3 124.7 . . ?
Pd2 C4 H4 81.5 . . ?
C3 C4 Pd2 84.0(3) . . ?
C3 C4 H4 126.7 . . ?
C3 C4 C5 106.7(4) . . ?
C5 C4 Pd2 106.3(3) . . ?
C5 C4 H4 126.7 . . ?
C1 C5 Pd3 72.0(3) . . ?
C1 C5 C4 107.9(4) . . ?
C1 C5 C6 120.0(4) . . ?
C4 C5 Pd3 114.9(3) . . ?
C6 C5 Pd3 70.0(3) . . ?
C6 C5 C4 129.7(4) . . ?
C5 C6 Pd3 70.9(3) . . ?
C5 C6 C7 118.7(4) . . ?
C5 C6 C13 120.6(4) . . ?
C7 C6 Pd3 120.5(3) . . ?
C13 C6 Pd3 103.9(3) . . ?
C13 C6 C7 114.0(4) . . ?
C8 C7 C6 124.0(4) . . ?
C8 C7 C12 117.6(4) . . ?
C12 C7 C6 118.3(4) . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 121.0(5) . . ?
C9 C8 H8 119.5 . . ?
C8 C9 H9 119.3 . . ?
C10 C9 C8 121.4(6) . . ?
C10 C9 H9 119.3 . . ?
C9 C10 H10 120.6 . . ?
C9 C10 C11 118.9(5) . . ?
C11 C10 H10 120.6 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.7(5) . . ?
C12 C11 H11 120.1 . . ?
C7 C12 C11 121.4(5) . . ?
C7 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C14 C13 C6 120.6(5) . . ?
C14 C13 C18 117.3(5) . . ?
C18 C13 C6 122.1(5) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 C13 121.5(6) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.8(6) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 120.1(6) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.1(6) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 H18 119.4 . . ?
C17 C18 C13 121.2(6) . . ?
C17 C18 H18 119.4 . . ?
Pd1 C19 H19 92.9 . . ?
C20 C19 Pd1 71.5(3) . . ?
C20 C19 H19 125.4 . . ?
C20 C19 C23 109.2(5) . . ?
C23 C19 Pd1 105.1(3) . . ?
C23 C19 H19 125.4 . . ?
Pd1 C20 H20 93.4 . . ?
C19 C20 Pd1 72.6(3) . . ?
C19 C20 H20 126.1 . . ?
C19 C20 C21 107.7(5) . . ?
C21 C20 Pd1 103.3(4) . . ?
C21 C20 H20 126.1 . . ?
Pd2 C21 H21 97.0 . . ?
C20 C21 Pd2 103.9(4) . . ?
C20 C21 H21 125.2 . . ?
C22 C21 Pd2 67.6(3) . . ?
C22 C21 C20 109.6(5) . . ?
C22 C21 H21 125.2 . . ?
Pd2 C22 H22 93.6 . . ?
C21 C22 Pd2 76.8(3) . . ?
C21 C22 H22 125.9 . . ?
C21 C22 C23 108.2(5) . . ?
C23 C22 Pd2 98.9(3) . . ?
C23 C22 H22 125.9 . . ?
C22 C23 C19 105.1(5) . . ?
C24 C23 C19 129.2(5) . . ?
C24 C23 C22 125.6(5) . . ?
C23 C24 C25 125.0(5) . . ?
C23 C24 C31 118.0(5) . . ?
C25 C24 C31 117.0(5) . . ?
C26 C25 C24 121.4(5) . . ?
C30 C25 C24 119.4(5) . . ?
C30 C25 C26 119.2(5) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 C25 120.1(6) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.7(6) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.4(7) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 C28 120.0(6) . . ?
C30 C29 H29 120.0 . . ?
C25 C30 H30 119.7 . . ?
C29 C30 C25 120.5(6) . . ?
C29 C30 H30 119.7 . . ?
C32 C31 C24 120.6(5) . . ?
C36 C31 C24 120.6(5) . . ?
C36 C31 C32 118.8(5) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 C31 120.5(5) . . ?
C33 C32 H32 119.8 . . ?
C32 C33 H33 119.6 . . ?
C32 C33 C34 120.8(6) . . ?
C34 C33 H33 119.6 . . ?
C33 C34 H34 120.3 . . ?
C35 C34 C33 119.3(6) . . ?
C35 C34 H34 120.3 . . ?
C34 C35 H35 119.5 . . ?
C34 C35 C36 120.9(6) . . ?
C36 C35 H35 119.5 . . ?
C31 C36 C35 119.5(5) . . ?
C31 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
N1 C37 C38 178.8(11) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N2 C39 C40 178.5(8) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N3 C41 C42 177.7(7) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 C44 178.8(9) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
F2 B1 F1 110.1(11) . . ?
F2 B1 F3 113.3(14) . . ?
F2 B1 F4 104.4(12) . . ?
F3 B1 F1 107.2(15) . . ?
F3 B1 F4 111.7(10) . . ?
F4 B1 F1 110.2(12) . . ?
F6 B2 F5 114.6(14) . . ?
F6 B2 F7 103.0(16) . . ?
F6 B2 F8 117.3(14) . . ?
F7 B2 F5 102.1(12) . . ?
F8 B2 F5 109.0(15) . . ?
F8 B2 F7 109.5(14) . . ?
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
Pd1 Pd2 2.5409(6) . ?
Pd1 N1 2.099(5) . ?
Pd1 C2 2.138(5) . ?
Pd1 C3 2.525(5) . ?
Pd1 C19 2.242(5) . ?
Pd1 C20 2.229(5) . ?
Pd2 N2 2.093(5) . ?
Pd2 C3 2.437(5) . ?
Pd2 C4 2.129(5) . ?
Pd2 C21 2.308(5) . ?
Pd2 C22 2.192(5) . ?
Pd3 N3 2.100(5) . ?
Pd3 N4 2.087(5) . ?
Pd3 C1 2.186(5) . ?
Pd3 C5 2.154(5) . ?
Pd3 C6 2.142(4) . ?
F1 B1 1.421(14) . ?
F2 B1 1.323(13) . ?
F3 B1 1.339(13) . ?
F4 B1 1.397(13) . ?
F5 B2 1.382(13) . ?
F6 B2 1.301(15) . ?
F7 B2 1.360(13) . ?
F8 B2 1.358(15) . ?
N1 C37 1.107(8) . ?
N2 C39 1.120(8) . ?
N3 C41 1.122(7) . ?
N4 C43 1.140(9) . ?
C1 H1 0.9500 . ?
C1 C2 1.471(7) . ?
C1 C5 1.430(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.412(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.431(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.458(7) . ?
C5 C6 1.438(7) . ?
C6 C7 1.516(6) . ?
C6 C13 1.483(7) . ?
C7 C8 1.373(7) . ?
C7 C12 1.384(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.385(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.355(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.384(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.391(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.403(7) . ?
C13 C18 1.403(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.368(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.398(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.367(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(8) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C19 C20 1.380(8) . ?
C19 C23 1.479(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.458(9) . ?
C21 H21 0.9500 . ?
C21 C22 1.381(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.471(8) . ?
C23 C24 1.368(7) . ?
C24 C25 1.484(7) . ?
C24 C31 1.495(7) . ?
C25 C26 1.410(7) . ?
C25 C30 1.388(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.391(9) . ?
C27 H27 0.9500 . ?
C27 C28 1.375(10) . ?
C28 H28 0.9500 . ?
C28 C29 1.403(10) . ?
C29 H29 0.9500 . ?
C29 C30 1.374(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.400(7) . ?
C31 C36 1.391(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.374(8) . ?
C33 H33 0.9500 . ?
C33 C34 1.380(8) . ?
C34 H34 0.9500 . ?
C34 C35 1.371(9) . ?
C35 H35 0.9500 . ?
C35 C36 1.399(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.477(11) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.474(10) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.458(8) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.478(12) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 C2 C3 Pd2 -31.5(3) . . . . ?
Pd1 C2 C3 C4 -96.7(4) . . . . ?
Pd1 C3 C4 Pd2 42.5(2) . . . . ?
Pd1 C3 C4 C5 -62.8(4) . . . . ?
Pd1 C19 C20 C21 98.8(4) . . . . ?
Pd1 C19 C23 C22 -75.4(4) . . . . ?
Pd1 C19 C23 C24 100.8(6) . . . . ?
Pd1 C20 C21 Pd2 7.0(4) . . . . ?
Pd1 C20 C21 C22 77.8(5) . . . . ?
Pd2 C3 C4 C5 -105.3(4) . . . . ?
Pd2 C4 C5 Pd3 -167.6(2) . . . . ?
Pd2 C4 C5 C1 -89.6(4) . . . . ?
Pd2 C4 C5 C6 108.5(5) . . . . ?
Pd2 C21 C22 C23 95.2(4) . . . . ?
Pd2 C22 C23 C19 80.4(4) . . . . ?
Pd2 C22 C23 C24 -96.0(5) . . . . ?
Pd3 C1 C2 Pd1 163.0(2) . . . . ?
Pd3 C1 C2 C3 71.8(5) . . . . ?
Pd3 C1 C5 C4 -111.1(4) . . . . ?
Pd3 C1 C5 C6 52.9(4) . . . . ?
Pd3 C5 C6 C7 -115.0(4) . . . . ?
Pd3 C5 C6 C13 95.3(4) . . . . ?
Pd3 C6 C7 C8 3.2(6) . . . . ?
Pd3 C6 C7 C12 -179.6(4) . . . . ?
Pd3 C6 C13 C14 -71.1(5) . . . . ?
Pd3 C6 C13 C18 109.9(4) . . . . ?
C1 C2 C3 Pd1 100.3(4) . . . . ?
C1 C2 C3 Pd2 68.8(4) . . . . ?
C1 C2 C3 C4 3.7(6) . . . . ?
C1 C5 C6 Pd3 -53.8(4) . . . . ?
C1 C5 C6 C7 -168.8(4) . . . . ?
C1 C5 C6 C13 41.5(6) . . . . ?
C2 C1 C5 Pd3 114.4(4) . . . . ?
C2 C1 C5 C4 3.4(5) . . . . ?
C2 C1 C5 C6 167.3(4) . . . . ?
C2 C3 C4 Pd2 103.6(4) . . . . ?
C2 C3 C4 C5 -1.6(6) . . . . ?
C3 C4 C5 Pd3 -79.1(4) . . . . ?
C3 C4 C5 C1 -1.1(5) . . . . ?
C3 C4 C5 C6 -163.0(5) . . . . ?
C4 C5 C6 Pd3 106.2(5) . . . . ?
C4 C5 C6 C7 -8.8(7) . . . . ?
C4 C5 C6 C13 -158.5(5) . . . . ?
C5 C1 C2 Pd1 86.9(4) . . . . ?
C5 C1 C2 C3 -4.3(5) . . . . ?
C5 C6 C7 C8 86.9(6) . . . . ?
C5 C6 C7 C12 -95.9(6) . . . . ?
C5 C6 C13 C14 -146.9(5) . . . . ?
C5 C6 C13 C18 34.0(6) . . . . ?
C6 C7 C8 C9 175.0(5) . . . . ?
C6 C7 C12 C11 -176.9(5) . . . . ?
C6 C13 C14 C15 -179.5(4) . . . . ?
C6 C13 C18 C17 178.3(5) . . . . ?
C7 C6 C13 C14 62.0(6) . . . . ?
C7 C6 C13 C18 -117.1(5) . . . . ?
C7 C8 C9 C10 2.1(9) . . . . ?
C8 C7 C12 C11 0.4(8) . . . . ?
C8 C9 C10 C11 -0.2(9) . . . . ?
C9 C10 C11 C12 -1.6(8) . . . . ?
C10 C11 C12 C7 1.5(9) . . . . ?
C12 C7 C8 C9 -2.2(8) . . . . ?
C13 C6 C7 C8 -121.4(5) . . . . ?
C13 C6 C7 C12 55.7(6) . . . . ?
C13 C14 C15 C16 0.5(8) . . . . ?
C14 C13 C18 C17 -0.8(7) . . . . ?
C14 C15 C16 C17 0.6(8) . . . . ?
C15 C16 C17 C18 -1.7(9) . . . . ?
C16 C17 C18 C13 1.8(9) . . . . ?
C18 C13 C14 C15 -0.4(7) . . . . ?
C19 C20 C21 Pd2 -68.7(5) . . . . ?
C19 C20 C21 C22 2.2(6) . . . . ?
C19 C23 C24 C25 -6.0(9) . . . . ?
C19 C23 C24 C31 175.3(5) . . . . ?
C20 C19 C23 C22 -0.1(6) . . . . ?
C20 C19 C23 C24 176.0(5) . . . . ?
C20 C21 C22 Pd2 -97.4(4) . . . . ?
C20 C21 C22 C23 -2.2(6) . . . . ?
C21 C22 C23 C19 1.4(6) . . . . ?
C21 C22 C23 C24 -174.9(5) . . . . ?
C22 C23 C24 C25 169.5(5) . . . . ?
C22 C23 C24 C31 -9.3(8) . . . . ?
C23 C19 C20 Pd1 -100.0(4) . . . . ?
C23 C19 C20 C21 -1.2(6) . . . . ?
C23 C24 C25 C26 -31.0(8) . . . . ?
C23 C24 C25 C30 148.8(5) . . . . ?
C23 C24 C31 C32 122.5(6) . . . . ?
C23 C24 C31 C36 -56.5(7) . . . . ?
C24 C25 C26 C27 177.4(5) . . . . ?
C24 C25 C30 C29 -177.0(5) . . . . ?
C24 C31 C32 C33 -174.9(6) . . . . ?
C24 C31 C36 C35 176.1(6) . . . . ?
C25 C24 C31 C32 -56.3(7) . . . . ?
C25 C24 C31 C36 124.7(6) . . . . ?
C25 C26 C27 C28 0.1(10) . . . . ?
C26 C25 C30 C29 2.8(8) . . . . ?
C26 C27 C28 C29 1.8(11) . . . . ?
C27 C28 C29 C30 -1.4(11) . . . . ?
C28 C29 C30 C25 -0.9(9) . . . . ?
C30 C25 C26 C27 -2.4(8) . . . . ?
C31 C24 C25 C26 147.7(5) . . . . ?
C31 C24 C25 C30 -32.5(7) . . . . ?
C31 C32 C33 C34 -2.0(10) . . . . ?
C32 C31 C36 C35 -2.9(9) . . . . ?
C32 C33 C34 C35 -1.5(11) . . . . ?
C33 C34 C35 C36 2.7(12) . . . . ?
C34 C35 C36 C31 -0.5(11) . . . . ?
C36 C31 C32 C33 4.1(9) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 187.6 52.2 '2 CH3CN'
2 0.000 0.500 0.500 187.6 52.2 '2 CH3CN'
3 0.474 0.607 0.458 27.0 6.0 ?
4 0.474 0.893 0.958 27.0 6.0 ?
5 0.526 0.107 0.042 27.0 6.1 ?
6 0.526 0.393 0.542 27.0 6.1 ?
