#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/02/7010238.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_7010238
loop_
_publ_author_name
'Baker, Murray V.'
'Skelton, Brian W.'
'White, Allan H.'
'Williams, Charlotte C.'
_publ_section_title
;
 Palladium carbene complexes derived from imidazolium-linked
 ortho-cyclophanes
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              111
_journal_paper_doi               10.1039/b007293l
_journal_year                    2001
_chemical_formula_sum            'C22.5 H22 I2 N4 O0.5 Pd'
_chemical_formula_weight         716.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 95.946(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   10.3800(10)
_cell_length_b                   8.9810(10)
_cell_length_c                   25.693(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2382.3(4)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      153
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .042
_diffrn_reflns_av_sigmaI/netI    .01
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26807
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.39
_exptl_absorpt_correction_T_max  .802
_exptl_absorpt_correction_T_min  .502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_description       plate
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.056
_refine_ls_extinction_coef       1001(142)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.248
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5744
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .032
_refine_ls_R_factor_gt           .031
_refine_ls_shift/su_max          .043
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .045
_refine_ls_wR_factor_ref         .044
_reflns_d_resolution_high        .733
_reflns_d_resolution_low         9.917
_reflns_Friedel_coverage         0
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              -34
_reflns_number_gt                5744
_reflns_number_total             5935
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            b007293l.txt
_cod_data_source_block           cwi
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_original_formula_sum        'C22.5 H22 I2 N4 O.5 Pd1'
_cod_database_code               7010238
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd .65622(2) .18054(3) .138078(10) .01698(13) Uani ? ? 1.00000 ? ?
I1 .69474(3) -.07205(3) .089636(10) .02767(13) Uani ? ? 1.00000 ? ?
I2 .89926(2) .27507(3) .144223(9) .02384(13) Uani ? ? 1.00000 ? ?
C1 .3942(4) .2441(5) .05068(15) .0254(17) Uani ? ? 1.00000 ? ?
C11 .3496(4) .4034(5) .04204(14) .0254(17) Uani ? ? 1.00000 ? ?
C12 .4292(4) .5265(4) .05758(14) .0226(16) Uani ? ? 1.00000 ? ?
C13 .3843(4) .6700(5) .04446(15) .0279(18) Uani ? ? 1.00000 ? ?
C14 .2624(4) .6930(6) .01729(18) .034(2) Uani ? ? 1.00000 ? ?
C15 .1838(4) .5726(6) .00333(16) .034(2) Uani ? ? 1.00000 ? ?
C16 .2277(4) .4294(5) .01561(16) .031(2) Uani ? ? 1.00000 ? ?
C2 .4733(4) .0237(4) .22697(15) .0275(18) Uani ? ? 1.00000 ? ?
N21 .3731(3) .1845(4) .10213(12) .0219(14) Uani ? ? 1.00000 ? ?
C22 .4686(4) .1384(4) .13820(14) .0212(15) Uani ? ? 1.00000 ? ?
N23 .4079(3) .0854(4) .17825(13) .0238(14) Uani ? ? 1.00000 ? ?
C24 .2737(4) .0992(5) .16699(17) .032(2) Uani ? ? 1.00000 ? ?
C25 .2523(4) .1608(6) .11971(18) .035(2) Uani ? ? 1.00000 ? ?
C3 .6289(4) .2998(5) .26435(14) .0256(17) Uani ? ? 1.00000 ? ?
C31 .5139(4) .2422(4) .29033(14) .0236(16) Uani ? ? 1.00000 ? ?
C32 .4451(4) .1119(4) .27442(14) .0235(16) Uani ? ? 1.00000 ? ?
C33 .3480(4) .0618(5) .30347(16) .0272(18) Uani ? ? 1.00000 ? ?
C34 .3172(4) .1369(6) .34760(17) .033(2) Uani ? ? 1.00000 ? ?
C35 .3833(4) .2660(5) .36316(17) .032(2) Uani ? ? 1.00000 ? ?
C36 .4813(4) .3177(5) .33464(16) .0285(18) Uani ? ? 1.00000 ? ?
C4 .5650(3) .5109(4) .08510(14) .0211(15) Uani ? ? 1.00000 ? ?
N41 .5945(3) .4023(4) .22012(12) .0209(14) Uani ? ? 1.00000 ? ?
C42 .6060(3) .3712(4) .16934(13) .0181(14) Uani ? ? 1.00000 ? ?
N43 .5663(3) .4940(3) .14250(12) .0196(13) Uani ? ? 1.00000 ? ?
C44 .5330(4) .6051(4) .17634(15) .0256(17) Uani ? ? 1.00000 ? ?
C45 .5505(4) .5472(4) .22508(15) .0252(17) Uani ? ? 1.00000 ? ?
O0 1.0071(8) .0862(12) .0312(3) .060(5) Uani ? ? .50000 ? ?
C0 1.00000 .00000 .00000 .098(9) Uani ? ? 1.00000 ? ?
H1a .34939 .18319 .02416 .03100 Uiso ? ? 1.00000 ? ?
H1b .48497 .23973 .04677 .03100 Uiso ? ? 1.00000 ? ?
H13 .43799 .75465 .05457 .03500 Uiso ? ? 1.00000 ? ?
H14 .23316 .79206 .00779 .04200 Uiso ? ? 1.00000 ? ?
H15 .09864 .58712 -.01460 .04200 Uiso ? ? 1.00000 ? ?
H16 .17215 .34589 .00556 .03900 Uiso ? ? 1.00000 ? ?
H2a .56440 .02365 .22516 .03300 Uiso ? ? 1.00000 ? ?
H2b .44495 -.07636 .23112 .03300 Uiso ? ? 1.00000 ? ?
H24 .20977 .07003 .18959 .03800 Uiso ? ? 1.00000 ? ?
H25 .16959 .18399 .10119 .04100 Uiso ? ? 1.00000 ? ?
H3a .68561 .35090 .28998 .03200 Uiso ? ? 1.00000 ? ?
H3b .67395 .21680 .25173 .03200 Uiso ? ? 1.00000 ? ?
H33 .30022 -.02584 .29197 .03400 Uiso ? ? 1.00000 ? ?
H34 .25132 .09826 .36718 .04000 Uiso ? ? 1.00000 ? ?
H35 .36136 .32013 .39332 .03900 Uiso ? ? 1.00000 ? ?
H36 .52700 .40652 .34533 .03600 Uiso ? ? 1.00000 ? ?
H4a .60499 .42501 .07139 .02500 Uiso ? ? 1.00000 ? ?
H4b .61441 .59655 .07783 .02500 Uiso ? ? 1.00000 ? ?
H44 .50338 .70288 .16694 .03100 Uiso ? ? 1.00000 ? ?
H45 .53570 .59703 .25702 .03000 Uiso ? ? 1.00000 ? ?
H0a 1.01260 -.09510 .01591 .07800 Uiso ? ? .50000 ? ?
H0b 1.06609 .01771 -.02221 .07800 Uiso ? ? .50000 ? ?
H0c .91750 .00621 -.01968 .07800 Uiso ? ? .50000 ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 90 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 88 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
I ? 0 8 -.726 1.812 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 2 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Pd ? 0 4 -1.177 1.007 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
I1 Pd I2 . . . 96.528(12) ?
I1 Pd C22 . . . 91.91(11) ?
I1 Pd C42 . . . 172.91(9) ?
I2 Pd C22 . . . 171.54(11) ?
I2 Pd C42 . . . 89.30(10) ?
C22 Pd C42 . . . 82.24(14) ?
C11 C1 N21 . . . 114.0(3) ?
C11 C1 H1a . . . 108.6(3) ?
C11 C1 H1b . . . 108.2(4) ?
N21 C1 H1a . . . 109.1(4) ?
N21 C1 H1b . . . 108.7(3) ?
H1a C1 H1b . . . 108.2(4) ?
C1 C11 C12 . . . 122.5(3) ?
C1 C11 C16 . . . 118.6(4) ?
C12 C11 C16 . . . 118.8(4) ?
C11 C12 C13 . . . 118.8(3) ?
C11 C12 C4 . . . 123.2(3) ?
C13 C12 C4 . . . 117.9(3) ?
C12 C13 C14 . . . 121.2(4) ?
C12 C13 H13 . . . 119.6(4) ?
C14 C13 H13 . . . 119.2(4) ?
C13 C14 C15 . . . 119.7(4) ?
C13 C14 H14 . . . 120.6(4) ?
C15 C14 H14 . . . 119.7(4) ?
C14 C15 C16 . . . 119.6(4) ?
C14 C15 H15 . . . 120.5(5) ?
C16 C15 H15 . . . 119.9(5) ?
C11 C16 C15 . . . 121.8(4) ?
C11 C16 H16 . . . 119.2(4) ?
C15 C16 H16 . . . 119.0(4) ?
N23 C2 C32 . . . 112.3(3) ?
N23 C2 H2a . . . 109.4(4) ?
N23 C2 H2b . . . 109.2(3) ?
C32 C2 H2a . . . 108.5(3) ?
C32 C2 H2b . . . 108.5(4) ?
H2a C2 H2b . . . 108.9(4) ?
C1 N21 C22 . . . 124.3(3) ?
C1 N21 C25 . . . 125.0(3) ?
C22 N21 C25 . . . 110.6(3) ?
Pd C22 N21 . . . 126.3(3) ?
Pd C22 N23 . . . 127.2(3) ?
N21 C22 N23 . . . 105.3(3) ?
C2 N23 C22 . . . 124.9(3) ?
C2 N23 C24 . . . 124.9(3) ?
C22 N23 C24 . . . 110.2(3) ?
N23 C24 C25 . . . 107.1(4) ?
N23 C24 H24 . . . 125.8(4) ?
C25 C24 H24 . . . 127.1(4) ?
N21 C25 C24 . . . 106.8(4) ?
N21 C25 H25 . . . 126.5(5) ?
C24 C25 H25 . . . 126.8(5) ?
C31 C3 N41 . . . 114.3(3) ?
C31 C3 H3a . . . 108.5(3) ?
C31 C3 H3b . . . 108.5(4) ?
N41 C3 H3a . . . 108.3(4) ?
N41 C3 H3b . . . 108.3(3) ?
H3a C3 H3b . . . 108.8(4) ?
C3 C31 C32 . . . 123.6(3) ?
C3 C31 C36 . . . 117.5(3) ?
C32 C31 C36 . . . 118.8(4) ?
C2 C32 C31 . . . 122.4(4) ?
C2 C32 C33 . . . 118.4(4) ?
C31 C32 C33 . . . 119.2(4) ?
C32 C33 C34 . . . 121.6(4) ?
C32 C33 H33 . . . 118.7(4) ?
C34 C33 H33 . . . 119.7(4) ?
C33 C34 C35 . . . 119.7(4) ?
C33 C34 H34 . . . 119.5(5) ?
C35 C34 H34 . . . 120.8(5) ?
C34 C35 C36 . . . 119.6(4) ?
C34 C35 H35 . . . 120.3(5) ?
C36 C35 H35 . . . 120.1(4) ?
C31 C36 C35 . . . 121.2(4) ?
C31 C36 H36 . . . 119.0(4) ?
C35 C36 H36 . . . 119.8(4) ?
C12 C4 N43 . . . 112.7(3) ?
C12 C4 H4a . . . 108.6(3) ?
C12 C4 H4b . . . 109.1(3) ?
N43 C4 H4a . . . 108.9(3) ?
N43 C4 H4b . . . 109.2(3) ?
H4a C4 H4b . . . 108.3(4) ?
C3 N41 C42 . . . 125.1(3) ?
C3 N41 C45 . . . 124.7(3) ?
C42 N41 C45 . . . 110.2(3) ?
Pd C42 N41 . . . 128.5(3) ?
Pd C42 N43 . . . 125.5(3) ?
N41 C42 N43 . . . 105.8(3) ?
C4 N43 C42 . . . 124.5(3) ?
C4 N43 C44 . . . 124.9(3) ?
C42 N43 C44 . . . 110.6(3) ?
N43 C44 C45 . . . 106.6(3) ?
N43 C44 H44 . . . 126.7(4) ?
C45 C44 H44 . . . 126.8(4) ?
N41 C45 C44 . . . 106.8(3) ?
N41 C45 H45 . . . 126.7(4) ?
C44 C45 H45 . . . 126.5(4) ?
C0 O0 H0a . . '3 755' 48.1(4) ?
C0 O0 H0b . . '3 755' 48.1(4) ?
C0 O0 H0c . . '3 755' 48.4(4) ?
H0a O0 H0b '3 755' . '3 755' 79.7(5) ?
H0a O0 H0c '3 755' . '3 755' 81.1(6) ?
H0b O0 H0c '3 755' . '3 755' 80.3(7) ?
O0 C0 H0a . . . 108.6(5) ?
O0 C0 H0b . . . 108.6(5) ?
O0 C0 H0c . . . 109.4(4) ?
O0 C0 O0 . . '3 755' 180.0000 ?
O0 C0 H0a . . '3 755' 71.4(5) ?
O0 C0 H0b . . '3 755' 71.4(5) ?
O0 C0 H0c . . '3 755' 70.6(4) ?
H0a C0 H0b . . . 109.460(3) ?
H0a C0 H0c . . . 110.985(3) ?
H0a C0 O0 . . '3 755' 71.4(5) ?
H0a C0 H0a . . '3 755' 180.0000 ?
H0a C0 H0b . . '3 755' 70.540(3) ?
H0a C0 H0c . . '3 755' 69.015(3) ?
H0b C0 H0c . . . 109.734(8) ?
H0b C0 O0 . . '3 755' 71.4(5) ?
H0b C0 H0a . . '3 755' 70.540(3) ?
H0b C0 H0b . . '3 755' 180.0000 ?
H0b C0 H0c . . '3 755' 70.266(8) ?
H0c C0 O0 . . '3 755' 70.6(5) ?
H0c C0 H0a . . '3 755' 69.015(2) ?
H0c C0 H0b . . '3 755' 70.266(8) ?
H0c C0 H0c . . '3 755' 180.0000 ?
O0 C0 H0a '3 755' . '3 755' 108.6(5) ?
O0 C0 H0b '3 755' . '3 755' 108.6(5) ?
O0 C0 H0c '3 755' . '3 755' 109.4(5) ?
H0a C0 H0b '3 755' . '3 755' 109.460(3) ?
H0a C0 H0c '3 755' . '3 755' 110.985(3) ?
H0b C0 H0c '3 755' . '3 755' 109.734(8) ?
C0 H0a O0 . . '3 755' 60.5(5) ?
C0 H0b O0 . . '3 755' 60.5(4) ?
C0 H0c O0 . . '3 755' 61.0(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd I1 . . 2.6378(4) ?
Pd I2 . . 2.6510(4) ?
Pd C22 . . 1.984(4) ?
Pd C42 . . 1.984(4) ?
C1 C11 . . 1.512(6) ?
C1 N21 . . 1.464(5) ?
C1 H1a . . .956(4) ?
C1 H1b . . .959(4) ?
C11 C12 . . 1.413(6) ?
C11 C16 . . 1.393(6) ?
C12 C13 . . 1.400(6) ?
C12 C4 . . 1.516(5) ?
C13 C14 . . 1.395(6) ?
C13 H13 . . .962(4) ?
C14 C15 . . 1.380(7) ?
C14 H14 . . .964(5) ?
C15 C16 . . 1.390(7) ?
C15 H15 . . .962(4) ?
C16 H16 . . .965(5) ?
C2 N23 . . 1.469(5) ?
C2 C32 . . 1.508(6) ?
C2 H2a . . .952(4) ?
C2 H2b . . .955(4) ?
N21 C22 . . 1.350(5) ?
N21 C25 . . 1.392(5) ?
C22 N23 . . 1.348(5) ?
N23 C24 . . 1.398(5) ?
C24 C25 . . 1.332(6) ?
C24 H24 . . .962(4) ?
C25 H25 . . .960(4) ?
C3 C31 . . 1.518(6) ?
C3 N41 . . 1.477(5) ?
C3 H3a . . .954(4) ?
C3 H3b . . .954(4) ?
C31 C32 . . 1.409(5) ?
C31 C36 . . 1.397(6) ?
C32 C33 . . 1.390(6) ?
C33 C34 . . 1.385(6) ?
C33 H33 . . .961(4) ?
C34 C35 . . 1.384(7) ?
C34 H34 . . .955(5) ?
C35 C36 . . 1.394(6) ?
C35 H35 . . .962(4) ?
C36 H36 . . .954(4) ?
C4 N43 . . 1.481(5) ?
C4 H4a . . .960(4) ?
C4 H4b . . .954(4) ?
N41 C42 . . 1.352(5) ?
N41 C45 . . 1.390(5) ?
C42 N43 . . 1.343(5) ?
N43 C44 . . 1.390(5) ?
C44 C45 . . 1.351(5) ?
C44 H44 . . .953(4) ?
C45 H45 . . .961(4) ?
O0 C0 . . 1.112(10) ?
O0 H0a . '3 755' 1.210(9) ?
O0 H0b . '3 755' 1.210(10) ?
O0 H0c . '3 755' 1.199(10) ?
C0 H0a . . .95005(9) ?
C0 H0b . . .95008(7) ?
C0 H0c . . .94995(7) ?
C0 H0a . '3 755' .95005(9) ?
C0 H0b . '3 755' .95008(7) ?
C0 H0c . '3 755' .94995(7) ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Pd C1 3.392(4) . . ?
Pd C2 3.421(4) . . ?
Pd N21 2.989(3) . . ?
Pd N23 2.999(3) . . ?
Pd C3 3.456(4) . . ?
Pd C4 3.359(4) . . ?
Pd N41 3.016(3) . . ?
Pd N43 2.972(3) . . ?
Pd H1b 2.8429(3) . . ?
Pd H2a 2.8882(3) . . ?
Pd H3b 2.9249(4) . . ?
Pd H4a 2.8018(3) . . ?
C1 C12 2.566(6) . . ?
C1 C16 2.498(6) . . ?
C1 C22 2.489(5) . . ?
C1 C25 2.533(6) . . ?
C1 H16 2.634(4) . . ?
C11 C13 2.422(6) . . ?
C11 C14 2.805(6) . . ?
C11 C15 2.431(6) . . ?
C11 N21 2.496(5) . . ?
C11 C4 2.577(5) . . ?
C11 H1a 2.030(4) . . ?
C11 H1b 2.028(4) . . ?
C11 H16 2.045(4) . . ?
C11 H4a 2.687(4) . . ?
C12 C14 2.436(6) . . ?
C12 C15 2.806(5) . . ?
C12 C16 2.415(5) . . ?
C12 N43 2.495(4) . . ?
C12 H1b 2.661(4) . . ?
C12 H13 2.053(4) . . ?
C12 H4a 2.037(4) . . ?
C12 H4b 2.038(4) . . ?
C13 C15 2.400(6) . . ?
C13 C16 2.759(6) . . ?
C13 C4 2.499(5) . . ?
C13 H14 2.060(4) . . ?
C13 H4b 2.540(4) . . ?
C14 C16 2.394(7) . . ?
C14 H13 2.045(4) . . ?
C14 H15 2.044(4) . . ?
C15 H14 2.037(5) . . ?
C15 H16 2.041(5) . . ?
C16 H1a 2.544(5) . . ?
C16 H15 2.047(4) . . ?
C2 C22 2.498(5) . . ?
C2 C24 2.542(6) . . ?
C2 C31 2.556(6) . . ?
C2 C33 2.490(6) . . ?
C2 H33 2.614(4) . . ?
N21 N23 2.145(4) . . ?
N21 C24 2.187(6) . . ?
N21 H1a 1.993(3) . . ?
N21 H1b 1.990(3) . . ?
N21 H25 2.110(3) . . ?
C22 C24 2.252(6) . . ?
C22 C25 2.255(5) . . ?
C22 C42 2.610(5) . . ?
C22 H1b 2.541(4) . . ?
C22 H2a 2.566(3) . . ?
N23 C25 2.197(5) . . ?
N23 C32 2.473(5) . . ?
N23 H2a 1.999(3) . . ?
N23 H2b 1.999(3) . . ?
N23 H24 2.111(3) . . ?
C24 H25 2.056(4) . . ?
C25 H24 2.061(5) . . ?
C3 C32 2.581(6) . . ?
C3 C36 2.492(6) . . ?
C3 C42 2.511(5) . . ?
C3 C45 2.539(6) . . ?
C3 H36 2.612(4) . . ?
C31 C33 2.413(6) . . ?
C31 C34 2.802(6) . . ?
C31 C35 2.431(6) . . ?
C31 N41 2.517(5) . . ?
C31 H2a 2.667(4) . . ?
C31 H3a 2.033(4) . . ?
C31 H3b 2.034(4) . . ?
C31 H36 2.038(4) . . ?
C32 C34 2.422(6) . . ?
C32 C35 2.798(6) . . ?
C32 C36 2.415(6) . . ?
C32 H2a 2.022(4) . . ?
C32 H2b 2.024(4) . . ?
C32 H3b 2.675(4) . . ?
C32 H33 2.034(4) . . ?
C33 C35 2.394(6) . . ?
C33 C36 2.758(6) . . ?
C33 H2b 2.529(4) . . ?
C33 H34 2.033(4) . . ?
C34 C36 2.401(6) . . ?
C34 H33 2.039(5) . . ?
C34 H35 2.046(5) . . ?
C35 H34 2.046(5) . . ?
C35 H36 2.042(5) . . ?
C36 H3a 2.532(4) . . ?
C36 H35 2.052(4) . . ?
C4 C42 2.500(5) . . ?
C4 C44 2.546(5) . . ?
C4 H13 2.633(4) . . ?
N41 N43 2.150(4) . . ?
N41 C44 2.200(5) . . ?
N41 H3a 1.994(3) . . ?
N41 H3b 1.994(3) . . ?
N41 H45 2.110(3) . . ?
C42 C44 2.247(5) . . ?
C42 C45 2.248(5) . . ?
C42 H3b 2.567(3) . . ?
C42 H4a 2.561(3) . . ?
N43 C45 2.197(5) . . ?
N43 H4a 2.009(3) . . ?
N43 H4b 2.008(3) . . ?
N43 H44 2.104(3) . . ?
C44 H45 2.071(4) . . ?
C45 H44 2.067(4) . . ?
O0 O0 2.224(14) . '3 755' ?
O0 H25 2.494(9) . '1 655' ?
O0 H0a 1.677(11) . . ?
O0 H0b 1.677(9) . . ?
O0 H0c 1.685(9) . . ?
H1a H1b 1.55128(12) . . ?
H1a H16 2.35925(17) . . ?
H1b H4a 2.13490(16) . . ?
H13 H14 2.35553(18) . . ?
H13 H4b 2.34520(16) . . ?
H14 H15 2.34561(18) . . ?
H15 H16 2.3372(2) . . ?
H2a H2b 1.55141(11) . . ?
H2a H3b 2.14648(17) . . ?
H2b H33 2.32242(17) . . ?
H3a H3b 1.55122(13) . . ?
H3a H36 2.33828(17) . . ?
H33 H34 2.3318(2) . . ?
H34 H35 2.3595(2) . . ?
H35 H36 2.34897(16) . . ?
H4a H4b 1.55146(17) . . ?
H0a H0a 1.90011(18) . '3 755' ?
H0a H0b 1.55134(11) . . ?
H0a H0b 1.09720(8) . '3 755' ?
H0a H0c 1.56571(10) . . ?
H0a H0c 1.07637(8) . '3 755' ?
H0b H0b 1.90016(14) . '3 755' ?
H0b H0c 1.09342(12) . '3 755' ?
H0b H0c 1.55388(15) . . ?
H0c H0c 1.89990(15) . '3 755' ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
