#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:16:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180069 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/15/7051579.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_7051579
loop_
_publ_author_name
'Jin, Guoxia'
'Jones, Cameron'
'Junk, Peter C.'
'Lippert, Kai-Alexander'
'Rose, Richard P.'
'Stasch, Andreas'
_publ_section_title
;
 Synthesis and characterisation of bulky guanidines and
 phosphaguanidines: precursors for low oxidation state metallacycles
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              64
_journal_paper_doi               10.1039/b809120j
_journal_volume                  33
_journal_year                    2009
_chemical_formula_sum            'C68 H110 N6'
_chemical_formula_weight         1011.62
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.467(3)
_cell_length_b                   22.956(5)
_cell_length_c                   19.774(4)
_cell_measurement_temperature    150(2)
_cell_volume                     6516(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_sigmaI/netI    0.1032
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16169
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         11404
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0620P)²+4.3021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1828
_reflns_number_gt                6796
_reflns_number_total             11404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809120j.txt
_cod_data_source_block           compound8
_cod_original_cell_volume        6516(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7051579
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.23666(15) 0.50554(11) 0.53539(12) 0.0259(6) Uani 1 1 d . . .
H1 H 0.2163 0.5384 0.5119 0.031 Uiso 1 1 calc R . .
C1 C 0.31168(18) 0.51031(14) 0.60142(14) 0.0246(7) Uani 1 1 d . . .
N2 N 0.36939(15) 0.46254(11) 0.62342(12) 0.0260(6) Uani 1 1 d . . .
C2 C 0.18836(18) 0.45380(14) 0.50072(15) 0.0290(7) Uani 1 1 d . . .
N3 N 0.32723(15) 0.55689(11) 0.64068(12) 0.0241(6) Uani 1 1 d . . .
C3 C 0.18469(19) 0.44078(15) 0.42997(16) 0.0339(8) Uani 1 1 d . . .
N4 N -0.11638(15) 0.88953(11) 0.48255(12) 0.0270(6) Uani 1 1 d . . .
C4 C 0.1369(2) 0.39107(16) 0.39618(18) 0.0440(9) Uani 1 1 d . . .
H4 H 0.1330 0.3815 0.3484 0.053 Uiso 1 1 calc R . .
N5 N -0.26225(15) 0.93035(11) 0.45911(12) 0.0271(6) Uani 1 1 d . . .
C5 C 0.0950(2) 0.35532(17) 0.4312(2) 0.0510(10) Uani 1 1 d . . .
H5 H 0.0643 0.3208 0.4079 0.061 Uiso 1 1 calc R . .
N6 N -0.23586(15) 0.83075(11) 0.49074(12) 0.0275(6) Uani 1 1 d . . .
H6 H -0.1944 0.8065 0.5196 0.033 Uiso 1 1 calc R . .
C6 C 0.0975(2) 0.36912(16) 0.4994(2) 0.0462(9) Uani 1 1 d . . .
H6A H 0.0674 0.3443 0.5223 0.055 Uiso 1 1 calc R . .
C7 C 0.14298(19) 0.41857(14) 0.53556(16) 0.0330(8) Uani 1 1 d . . .
C8 C 0.2307(2) 0.47985(16) 0.39093(16) 0.0393(8) Uani 1 1 d . . .
H8 H 0.2774 0.5047 0.4285 0.047 Uiso 1 1 calc R . .
C9 C 0.2825(3) 0.44512(19) 0.3517(2) 0.0649(12) Uani 1 1 d . . .
H9A H 0.2376 0.4231 0.3114 0.097 Uiso 1 1 calc R . .
H9B H 0.3261 0.4180 0.3860 0.097 Uiso 1 1 calc R . .
H9C H 0.3171 0.4719 0.3325 0.097 Uiso 1 1 calc R . .
C10 C 0.1592(3) 0.5201(2) 0.3380(2) 0.0716(13) Uani 1 1 d . . .
H10A H 0.1896 0.5442 0.3123 0.107 Uiso 1 1 calc R . .
H10B H 0.1321 0.5454 0.3649 0.107 Uiso 1 1 calc R . .
H10C H 0.1098 0.4968 0.3026 0.107 Uiso 1 1 calc R . .
C11 C 0.1389(2) 0.43573(16) 0.60830(17) 0.0403(9) Uani 1 1 d . . .
H11 H 0.1949 0.4602 0.6344 0.048 Uiso 1 1 calc R . .
C12 C 0.0529(3) 0.4733(2) 0.5967(2) 0.0753(14) Uani 1 1 d . . .
H12A H 0.0552 0.5082 0.5689 0.113 Uiso 1 1 calc R . .
H12B H 0.0517 0.4848 0.6441 0.113 Uiso 1 1 calc R . .
H12C H -0.0034 0.4509 0.5697 0.113 Uiso 1 1 calc R . .
C13 C 0.1417(3) 0.3835(2) 0.6570(2) 0.0745(13) Uani 1 1 d . . .
H13A H 0.1513 0.3972 0.7062 0.112 Uiso 1 1 calc R . .
H13B H 0.1931 0.3577 0.6590 0.112 Uiso 1 1 calc R . .
H13C H 0.0827 0.3622 0.6370 0.112 Uiso 1 1 calc R . .
C14 C 0.3950(2) 0.42934(14) 0.56941(16) 0.0337(8) Uani 1 1 d . . .
H14 H 0.3505 0.4416 0.5202 0.040 Uiso 1 1 calc R . .
C15 C 0.4926(2) 0.44439(17) 0.57211(18) 0.0446(9) Uani 1 1 d . . .
H15A H 0.4982 0.4867 0.5687 0.067 Uiso 1 1 calc R . .
H15B H 0.5030 0.4256 0.5313 0.067 Uiso 1 1 calc R . .
H15C H 0.5392 0.4305 0.6181 0.067 Uiso 1 1 calc R . .
C16 C 0.3818(2) 0.36427(16) 0.5750(2) 0.0532(10) Uani 1 1 d . . .
H16A H 0.4235 0.3503 0.6229 0.080 Uiso 1 1 calc R . .
H16B H 0.3961 0.3441 0.5368 0.080 Uiso 1 1 calc R . .
H16C H 0.3170 0.3564 0.5690 0.080 Uiso 1 1 calc R . .
C17 C 0.4349(2) 0.45743(14) 0.69990(15) 0.0330(8) Uani 1 1 d . . .
H17 H 0.4703 0.4206 0.7023 0.040 Uiso 1 1 calc R . .
C18 C 0.5082(2) 0.50524(15) 0.72769(16) 0.0405(9) Uani 1 1 d . . .
H18A H 0.5321 0.5152 0.6897 0.061 Uiso 1 1 calc R . .
H18B H 0.5596 0.4914 0.7711 0.061 Uiso 1 1 calc R . .
H18C H 0.4801 0.5398 0.7402 0.061 Uiso 1 1 calc R . .
C19 C 0.3841(2) 0.44885(16) 0.75196(16) 0.0438(9) Uani 1 1 d . . .
H19A H 0.3482 0.4840 0.7522 0.066 Uiso 1 1 calc R . .
H19B H 0.4296 0.4416 0.8012 0.066 Uiso 1 1 calc R . .
H19C H 0.3418 0.4155 0.7360 0.066 Uiso 1 1 calc R . .
C20 C 0.26526(18) 0.60477(13) 0.61774(14) 0.0252(7) Uani 1 1 d . . .
C21 C 0.26506(18) 0.64058(13) 0.55955(14) 0.0251(7) Uani 1 1 d . . .
C22 C 0.20384(19) 0.68734(13) 0.53899(15) 0.0259(7) Uani 1 1 d . . .
H22 H 0.2032 0.7109 0.4993 0.031 Uiso 1 1 calc R . .
C23 C 0.14324(18) 0.70122(13) 0.57417(14) 0.0255(7) Uani 1 1 d . . .
C24 C 0.14882(19) 0.66677(14) 0.63376(15) 0.0288(7) Uani 1 1 d . . .
H24 H 0.1098 0.6760 0.6597 0.035 Uiso 1 1 calc R . .
C25 C 0.20884(19) 0.61944(13) 0.65699(15) 0.0273(7) Uani 1 1 d . . .
C26 C 0.33725(19) 0.63109(14) 0.52473(15) 0.0286(7) Uani 1 1 d . . .
H26 H 0.3432 0.5881 0.5192 0.034 Uiso 1 1 calc R . .
C27 C 0.4321(2) 0.65358(16) 0.57665(19) 0.0458(9) Uani 1 1 d . . .
H27A H 0.4273 0.6952 0.5859 0.069 Uiso 1 1 calc R . .
H27B H 0.4785 0.6478 0.5545 0.069 Uiso 1 1 calc R . .
H27C H 0.4510 0.6321 0.6227 0.069 Uiso 1 1 calc R . .
C28 C 0.3112(2) 0.65836(17) 0.44969(17) 0.0476(10) Uani 1 1 d . . .
H28A H 0.2490 0.6450 0.4181 0.071 Uiso 1 1 calc R . .
H28B H 0.3566 0.6468 0.4285 0.071 Uiso 1 1 calc R . .
H28C H 0.3110 0.7009 0.4540 0.071 Uiso 1 1 calc R . .
C29 C 0.2172(2) 0.58543(15) 0.72478(16) 0.0351(8) Uani 1 1 d . . .
H29 H 0.2236 0.5433 0.7145 0.042 Uiso 1 1 calc R . .
C30 C 0.3075(3) 0.60388(17) 0.78763(17) 0.0519(10) Uani 1 1 d . . .
H30A H 0.3605 0.5995 0.7723 0.078 Uiso 1 1 calc R . .
H30B H 0.3169 0.5792 0.8302 0.078 Uiso 1 1 calc R . .
H30C H 0.3024 0.6447 0.8003 0.078 Uiso 1 1 calc R . .
C31 C 0.1339(3) 0.59097(18) 0.7483(2) 0.0581(11) Uani 1 1 d . . .
H31A H 0.1291 0.6313 0.7628 0.087 Uiso 1 1 calc R . .
H31B H 0.1425 0.5649 0.7895 0.087 Uiso 1 1 calc R . .
H31C H 0.0768 0.5803 0.7075 0.087 Uiso 1 1 calc R . .
C32 C 0.07706(18) 0.75080(13) 0.54985(15) 0.0260(7) Uani 1 1 d . . .
C33 C 0.04034(18) 0.76867(13) 0.47753(15) 0.0269(7) Uani 1 1 d . . .
H33 H 0.0596 0.7491 0.4432 0.032 Uiso 1 1 calc R . .
C34 C -0.02364(18) 0.81426(13) 0.45317(14) 0.0257(7) Uani 1 1 d . . .
C35 C -0.05370(18) 0.84195(13) 0.50408(15) 0.0249(7) Uani 1 1 d . . .
C36 C -0.01524(18) 0.82643(13) 0.57835(14) 0.0244(7) Uani 1 1 d . . .
C37 C 0.04887(18) 0.78088(13) 0.59907(15) 0.0264(7) Uani 1 1 d . . .
H37 H 0.0744 0.7699 0.6490 0.032 Uiso 1 1 calc R . .
C38 C -0.0573(2) 0.83592(14) 0.37508(14) 0.0283(7) Uani 1 1 d . . .
H38 H -0.1252 0.8448 0.3595 0.034 Uiso 1 1 calc R . .
C39 C -0.0457(2) 0.79215(16) 0.32099(16) 0.0412(9) Uani 1 1 d . . .
H39A H -0.0758 0.8073 0.2713 0.062 Uiso 1 1 calc R . .
H39B H -0.0746 0.7551 0.3253 0.062 Uiso 1 1 calc R . .
H39C H 0.0208 0.7860 0.3315 0.062 Uiso 1 1 calc R . .
C40 C -0.0075(2) 0.89265(16) 0.37175(16) 0.0398(9) Uani 1 1 d . . .
H40A H -0.0175 0.9212 0.4050 0.060 Uiso 1 1 calc R . .
H40B H -0.0325 0.9080 0.3219 0.060 Uiso 1 1 calc R . .
H40C H 0.0594 0.8852 0.3862 0.060 Uiso 1 1 calc R . .
C41 C -0.0386(2) 0.86107(14) 0.63488(15) 0.0307(7) Uani 1 1 d . . .
H41 H -0.1064 0.8710 0.6130 0.037 Uiso 1 1 calc R . .
C42 C 0.0159(2) 0.91859(17) 0.65042(19) 0.0520(10) Uani 1 1 d . . .
H42A H 0.0829 0.9103 0.6719 0.078 Uiso 1 1 calc R . .
H42B H -0.0021 0.9420 0.6845 0.078 Uiso 1 1 calc R . .
H42C H 0.0019 0.9402 0.6048 0.078 Uiso 1 1 calc R . .
C43 C -0.0224(3) 0.82802(18) 0.70532(17) 0.0565(11) Uani 1 1 d . . .
H43A H -0.0563 0.7910 0.6941 0.085 Uiso 1 1 calc R . .
H43B H -0.0449 0.8514 0.7369 0.085 Uiso 1 1 calc R . .
H43C H 0.0443 0.8204 0.7303 0.085 Uiso 1 1 calc R . .
C44 C -0.20146(19) 0.88360(13) 0.47764(14) 0.0249(7) Uani 1 1 d . . .
C45 C -0.2374(2) 0.98336(14) 0.42769(16) 0.0330(8) Uani 1 1 d . . .
H45 H -0.2900 1.0113 0.4193 0.040 Uiso 1 1 calc R . .
C46 C -0.2348(2) 0.97098(15) 0.35272(16) 0.0405(8) Uani 1 1 d . . .
H46A H -0.1819 0.9455 0.3579 0.061 Uiso 1 1 calc R . .
H46B H -0.2280 1.0077 0.3299 0.061 Uiso 1 1 calc R . .
H46C H -0.2928 0.9518 0.3221 0.061 Uiso 1 1 calc R . .
C47 C -0.1495(2) 1.01555(15) 0.47577(18) 0.0420(8) Uani 1 1 d . . .
H47A H -0.1479 1.0176 0.5257 0.063 Uiso 1 1 calc R . .
H47B H -0.1499 1.0551 0.4570 0.063 Uiso 1 1 calc R . .
H47C H -0.0944 0.9946 0.4754 0.063 Uiso 1 1 calc R . .
C48 C -0.3289(2) 0.93861(14) 0.49598(16) 0.0322(7) Uani 1 1 d . . .
H48 H -0.3333 0.9002 0.5184 0.039 Uiso 1 1 calc R . .
C49 C -0.4267(2) 0.95249(18) 0.44203(19) 0.0517(10) Uani 1 1 d . . .
H49A H -0.4271 0.9913 0.4213 0.078 Uiso 1 1 calc R . .
H49B H -0.4705 0.9516 0.4673 0.078 Uiso 1 1 calc R . .
H49C H -0.4453 0.9234 0.4029 0.078 Uiso 1 1 calc R . .
C50 C -0.2967(3) 0.98237(17) 0.55815(19) 0.0532(10) Uani 1 1 d . . .
H50A H -0.2349 0.9712 0.5928 0.080 Uiso 1 1 calc R . .
H50B H -0.3409 0.9829 0.5830 0.080 Uiso 1 1 calc R . .
H50C H -0.2935 1.0212 0.5387 0.080 Uiso 1 1 calc R . .
C51 C -0.33070(19) 0.81067(13) 0.46308(15) 0.0261(7) Uani 1 1 d . . .
C52 C -0.38010(19) 0.80623(14) 0.38775(15) 0.0289(7) Uani 1 1 d . . .
C53 C -0.4731(2) 0.78914(15) 0.36359(16) 0.0368(8) Uani 1 1 d . . .
H53 H -0.5085 0.7871 0.3128 0.044 Uiso 1 1 calc R . .
C54 C -0.5146(2) 0.77503(15) 0.41232(18) 0.0415(9) Uani 1 1 d . . .
H54 H -0.5784 0.7641 0.3949 0.050 Uiso 1 1 calc R . .
C55 C -0.4638(2) 0.77685(15) 0.48600(17) 0.0370(8) Uani 1 1 d . . .
H55 H -0.4923 0.7654 0.5189 0.044 Uiso 1 1 calc R . .
C56 C -0.3714(2) 0.79509(14) 0.51333(15) 0.0292(7) Uani 1 1 d . . .
C57 C -0.3312(2) 0.81449(14) 0.33441(15) 0.0324(8) Uani 1 1 d . . .
H57 H -0.2835 0.8458 0.3541 0.039 Uiso 1 1 calc R . .
C58 C -0.3956(2) 0.83275(18) 0.25869(16) 0.0510(10) Uani 1 1 d . . .
H58A H -0.4373 0.8004 0.2352 0.077 Uiso 1 1 calc R . .
H58B H -0.3585 0.8432 0.2297 0.077 Uiso 1 1 calc R . .
H58C H -0.4326 0.8664 0.2623 0.077 Uiso 1 1 calc R . .
C59 C -0.2798(2) 0.75828(16) 0.33145(17) 0.0425(9) Uani 1 1 d . . .
H59A H -0.3248 0.7264 0.3141 0.064 Uiso 1 1 calc R . .
H59B H -0.2349 0.7490 0.3803 0.064 Uiso 1 1 calc R . .
H59C H -0.2468 0.7634 0.2981 0.064 Uiso 1 1 calc R . .
C60 C -0.3157(2) 0.79619(15) 0.59431(15) 0.0376(8) Uani 1 1 d . . .
H60 H -0.2629 0.8241 0.6032 0.045 Uiso 1 1 calc R . .
C61 C -0.3716(3) 0.81678(19) 0.63921(18) 0.0606(12) Uani 1 1 d . . .
H61A H -0.4030 0.8535 0.6191 0.091 Uiso 1 1 calc R . .
H61B H -0.3295 0.8228 0.6899 0.091 Uiso 1 1 calc R . .
H61C H -0.4182 0.7873 0.6374 0.091 Uiso 1 1 calc R . .
C62 C -0.2739(3) 0.73616(18) 0.62012(19) 0.0622(12) Uani 1 1 d . . .
H62A H -0.3242 0.7081 0.6135 0.093 Uiso 1 1 calc R . .
H62B H -0.2337 0.7381 0.6718 0.093 Uiso 1 1 calc R . .
H62C H -0.2372 0.7238 0.5916 0.093 Uiso 1 1 calc R . .
C63 C -0.7234(3) 0.8433(2) 0.4750(2) 0.0844(14) Uiso 1 1 d D . .
H63A H -0.7640 0.8091 0.4664 0.127 Uiso 1 1 calc R . .
H63B H -0.6909 0.8429 0.4409 0.127 Uiso 1 1 calc R . .
H63C H -0.7611 0.8787 0.4675 0.127 Uiso 1 1 calc R . .
C64 C -0.6530(4) 0.8420(3) 0.5522(2) 0.1025(17) Uiso 1 1 d D B .
H64A H -0.6128 0.8074 0.5571 0.123 Uiso 1 1 calc R . .
H64B H -0.6127 0.8767 0.5592 0.123 Uiso 1 1 calc R . .
C65 C -0.6874(3) 0.8404(2) 0.6120(2) 0.0898(15) Uiso 1 1 d D . .
H65A H -0.7397 0.8124 0.6000 0.108 Uiso 1 1 calc R A 1
H65B H -0.7113 0.8794 0.6177 0.108 Uiso 1 1 calc R A 1
C66 C -0.6120(11) 0.8229(16) 0.6824(8) 0.104(2) Uiso 0.228(6) 1 d PD B 1
H66A H -0.5750 0.7904 0.6743 0.125 Uiso 0.228(6) 1 calc PR B 1
H66B H -0.5697 0.8561 0.7036 0.125 Uiso 0.228(6) 1 calc PR B 1
C67 C -0.6591(17) 0.8043(10) 0.7326(10) 0.103(2) Uiso 0.228(6) 1 d PD B 1
H67A H -0.6107 0.7923 0.7796 0.124 Uiso 0.228(6) 1 calc PR B 1
H67B H -0.6980 0.7697 0.7114 0.124 Uiso 0.228(6) 1 calc PR B 1
C68 C -0.7195(15) 0.8500(10) 0.7475(12) 0.0885(19) Uiso 0.228(6) 1 d PD B 1
H68A H -0.7832 0.8352 0.7332 0.133 Uiso 0.228(6) 1 calc PR B 1
H68B H -0.7197 0.8852 0.7193 0.133 Uiso 0.228(6) 1 calc PR B 1
H68C H -0.6949 0.8595 0.7995 0.133 Uiso 0.228(6) 1 calc PR B 1
C66A C -0.6194(5) 0.8363(5) 0.6858(3) 0.104(2) Uiso 0.772(6) 1 d PD B 2
H66C H -0.5730 0.8675 0.6917 0.125 Uiso 0.772(6) 1 calc PR B 2
H66D H -0.5864 0.7987 0.6896 0.125 Uiso 0.772(6) 1 calc PR B 2
C67A C -0.6481(5) 0.8398(4) 0.7494(4) 0.103(2) Uiso 0.772(6) 1 d PD B 2
H67C H -0.5916 0.8350 0.7940 0.124 Uiso 0.772(6) 1 calc PR B 2
H67D H -0.6720 0.8796 0.7507 0.124 Uiso 0.772(6) 1 calc PR B 2
C68A C -0.7182(4) 0.7983(3) 0.7531(3) 0.0885(19) Uiso 0.772(6) 1 d PD B 2
H68D H -0.7734 0.8004 0.7079 0.133 Uiso 0.772(6) 1 calc PR B 2
H68E H -0.7356 0.8081 0.7946 0.133 Uiso 0.772(6) 1 calc PR B 2
H68F H -0.6924 0.7588 0.7593 0.133 Uiso 0.772(6) 1 calc PR 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'
N N 0.0061 0.0033 '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
C1 N1 C2 128.2(2) . . ?
N3 C1 N2 121.1(2) . . ?
N3 C1 N1 122.2(3) . . ?
N2 C1 N1 116.7(3) . . ?
C1 N2 C17 120.2(2) . . ?
C1 N2 C14 119.8(2) . . ?
C17 N2 C14 115.5(2) . . ?
C7 C2 C3 121.3(3) . . ?
C7 C2 N1 120.5(3) . . ?
C3 C2 N1 118.1(3) . . ?
C1 N3 C20 119.9(2) . . ?
C4 C3 C2 118.0(3) . . ?
C4 C3 C8 120.4(3) . . ?
C2 C3 C8 121.6(3) . . ?
C44 N4 C35 120.4(3) . . ?
C5 C4 C3 120.8(3) . . ?
C44 N5 C48 119.9(2) . . ?
C44 N5 C45 119.5(2) . . ?
C48 N5 C45 116.0(2) . . ?
C6 C5 C4 120.6(3) . . ?
C44 N6 C51 128.1(2) . . ?
C5 C6 C7 121.2(3) . . ?
C6 C7 C2 117.9(3) . . ?
C6 C7 C11 120.6(3) . . ?
C2 C7 C11 121.3(3) . . ?
C10 C8 C3 110.5(3) . . ?
C10 C8 C9 110.6(3) . . ?
C3 C8 C9 112.5(3) . . ?
C7 C11 C13 113.1(3) . . ?
C7 C11 C12 110.2(3) . . ?
C13 C11 C12 110.9(3) . . ?
N2 C14 C16 111.9(3) . . ?
N2 C14 C15 112.6(3) . . ?
C16 C14 C15 112.2(3) . . ?
N2 C17 C19 111.9(2) . . ?
N2 C17 C18 116.4(3) . . ?
C19 C17 C18 110.6(3) . . ?
C25 C20 C21 119.7(3) . . ?
C25 C20 N3 119.6(2) . . ?
C21 C20 N3 120.5(2) . . ?
C22 C21 C20 118.9(2) . . ?
C22 C21 C26 120.7(3) . . ?
C20 C21 C26 120.2(2) . . ?
C21 C22 C23 122.8(3) . . ?
C24 C23 C22 116.7(3) . . ?
C24 C23 C32 121.7(2) . . ?
C22 C23 C32 121.5(3) . . ?
C25 C24 C23 123.1(3) . . ?
C24 C25 C20 118.6(3) . . ?
C24 C25 C29 121.4(2) . . ?
C20 C25 C29 119.9(3) . . ?
C28 C26 C21 114.1(2) . . ?
C28 C26 C27 110.8(3) . . ?
C21 C26 C27 109.1(2) . . ?
C25 C29 C31 115.0(3) . . ?
C25 C29 C30 109.0(3) . . ?
C31 C29 C30 110.2(3) . . ?
C37 C32 C33 117.4(3) . . ?
C37 C32 C23 120.8(2) . . ?
C33 C32 C23 121.8(2) . . ?
C32 C33 C34 122.8(3) . . ?
C33 C34 C35 118.2(2) . . ?
C33 C34 C38 121.8(2) . . ?
C35 C34 C38 120.0(3) . . ?
C34 C35 C36 120.5(3) . . ?
C34 C35 N4 120.3(2) . . ?
C36 C35 N4 119.0(2) . . ?
C37 C36 C35 118.3(2) . . ?
C37 C36 C41 120.9(2) . . ?
C35 C36 C41 120.7(3) . . ?
C32 C37 C36 122.8(3) . . ?
C34 C38 C39 114.3(3) . . ?
C34 C38 C40 109.6(2) . . ?
C39 C38 C40 109.8(2) . . ?
C36 C41 C43 114.1(3) . . ?
C36 C41 C42 109.5(2) . . ?
C43 C41 C42 110.8(3) . . ?
N4 C44 N5 120.8(3) . . ?
N4 C44 N6 122.0(3) . . ?
N5 C44 N6 117.3(2) . . ?
N5 C45 C46 111.1(3) . . ?
N5 C45 C47 116.5(2) . . ?
C46 C45 C47 110.8(2) . . ?
N5 C48 C50 113.8(3) . . ?
N5 C48 C49 111.9(2) . . ?
C50 C48 C49 111.6(3) . . ?
C52 C51 C56 121.5(3) . . ?
C52 C51 N6 120.2(2) . . ?
C56 C51 N6 118.3(2) . . ?
C53 C52 C51 118.0(3) . . ?
C53 C52 C57 120.9(3) . . ?
C51 C52 C57 120.9(3) . . ?
C54 C53 C52 121.1(3) . . ?
C55 C54 C53 120.1(3) . . ?
C54 C55 C56 121.4(3) . . ?
C55 C56 C51 117.9(3) . . ?
C55 C56 C60 121.0(3) . . ?
C51 C56 C60 121.1(3) . . ?
C58 C57 C52 114.0(3) . . ?
C58 C57 C59 110.8(3) . . ?
C52 C57 C59 108.7(3) . . ?
C56 C60 C62 110.0(3) . . ?
C56 C60 C61 113.5(3) . . ?
C62 C60 C61 110.2(3) . . ?
C65 C64 C63 118.3(4) . . ?
C66A C65 C64 117.9(5) . . ?
C66A C65 C66 13.2(17) . . ?
C64 C65 C66 111.4(8) . . ?
C67 C66 C65 106.8(11) . . ?
C66 C67 C68 115.0(14) . . ?
C65 C66A C67A 121.1(6) . . ?
C68A C67A C66A 117.9(8) . . ?
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
N1 C1 1.391(3) . ?
N1 C2 1.434(4) . ?
C1 N3 1.290(4) . ?
C1 N2 1.378(4) . ?
N2 C17 1.478(3) . ?
N2 C14 1.481(4) . ?
C2 C7 1.408(4) . ?
C2 C3 1.411(4) . ?
N3 C20 1.417(4) . ?
C3 C4 1.388(5) . ?
C3 C8 1.522(4) . ?
N4 C44 1.290(3) . ?
N4 C35 1.417(4) . ?
C4 C5 1.381(5) . ?
N5 C44 1.383(4) . ?
N5 C48 1.480(3) . ?
N5 C45 1.481(4) . ?
C5 C6 1.372(5) . ?
N6 C44 1.387(4) . ?
N6 C51 1.437(4) . ?
C6 C7 1.386(5) . ?
C7 C11 1.515(4) . ?
C8 C10 1.520(5) . ?
C8 C9 1.531(5) . ?
C11 C13 1.527(5) . ?
C11 C12 1.528(5) . ?
C14 C16 1.518(5) . ?
C14 C15 1.530(4) . ?
C17 C19 1.522(4) . ?
C17 C18 1.526(4) . ?
C20 C25 1.408(4) . ?
C20 C21 1.413(4) . ?
C21 C22 1.388(4) . ?
C21 C26 1.530(4) . ?
C22 C23 1.396(4) . ?
C23 C24 1.395(4) . ?
C23 C32 1.486(4) . ?
C24 C25 1.391(4) . ?
C25 C29 1.515(4) . ?
C26 C28 1.520(4) . ?
C26 C27 1.533(4) . ?
C29 C31 1.528(4) . ?
C29 C30 1.543(5) . ?
C32 C37 1.389(4) . ?
C32 C33 1.390(4) . ?
C33 C34 1.397(4) . ?
C34 C35 1.408(4) . ?
C34 C38 1.518(4) . ?
C35 C36 1.409(4) . ?
C36 C37 1.393(4) . ?
C36 C41 1.521(4) . ?
C38 C39 1.526(4) . ?
C38 C40 1.527(4) . ?
C41 C43 1.523(4) . ?
C41 C42 1.535(5) . ?
C45 C46 1.525(4) . ?
C45 C47 1.528(4) . ?
C48 C50 1.521(4) . ?
C48 C49 1.525(4) . ?
C51 C52 1.402(4) . ?
C51 C56 1.406(4) . ?
C52 C53 1.392(4) . ?
C52 C57 1.521(4) . ?
C53 C54 1.381(4) . ?
C54 C55 1.375(4) . ?
C55 C56 1.391(4) . ?
C56 C60 1.510(4) . ?
C57 C58 1.516(4) . ?
C57 C59 1.528(4) . ?
C60 C62 1.527(5) . ?
C60 C61 1.527(4) . ?
C63 C64 1.510(5) . ?
C64 C65 1.468(5) . ?
C65 C66A 1.450(7) . ?
C65 C66 1.501(10) . ?
C66 C67 1.494(10) . ?
C67 C68 1.505(10) . ?
C66A C67A 1.482(7) . ?
C67A C68A 1.466(7) . ?
