#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/24/2012489.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2012489
loop_
_publ_author_name
'Işıklan, Muhammed'
'Kılıç, Zeynel'
_publ_section_title
6-Propylamino-2,6-propylepimino-2,4,4,8,8-pentakis(pyrrolidin-1-yl)-1,3,5,7,2λ⁵,4λ⁵,6λ⁵,8λ⁵-tetraazatetraphosphorocine
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o80
_journal_page_last               o83
_journal_paper_doi               10.1107/S0108270101019151
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C26 H55 N11 P4'
_chemical_formula_sum            'C26 H55 N11 P4'
_chemical_formula_weight         645.69
_chemical_name_systematic
;
6-Propylamino-2,6-propylepimino-2,4,4,8,8-pentakis(pyrrolidin-1-yl)-
1,3,5,7,2λ⁵,4λ⁵,6λ⁵,8λ⁵-tetraazatetraphosphorocine
;
_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           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 97.73(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.405(11)
_cell_length_b                   21.545(5)
_cell_length_c                   28.893(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      10
_cell_volume                     7035(8)
_computing_cell_refinement       MolEN
_computing_data_collection       'MolEN (Fair, 1990)'
_computing_data_reduction        MolEN
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  MolEN
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .962
_diffrn_measured_fraction_theta_max .962
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .056
_diffrn_reflns_av_sigmaI/netI    .081
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14219
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .249
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .15
_refine_diff_density_max         .40
_refine_diff_density_min         -.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         13799
_refine_ls_number_restraints     783
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          .141
_refine_ls_R_factor_gt           .051
_refine_ls_shift/su_max          .004
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.055P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .111
_refine_ls_wR_factor_ref         .121
_reflns_number_gt                7479
_reflns_number_total             13799
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            da1202.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2012489
_cod_database_fobs_code          2012489
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_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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
N1 .34480(17) .69852(9) .77243(7) .0460(5) Uani d . 1 . . N
P2 .46948(6) .73132(3) .77090(2) .04268(17) Uani d . 1 A . P
N3 .49642(18) .79747(9) .79428(7) .0462(5) Uani d . 1 . . N
P4 .45722(6) .85951(3) .76682(2) .04607(18) Uani d . 1 B . P
N5 .38771(19) .85162(10) .71588(7) .0545(6) Uani d . 1 . . N
P6 .37071(6) .78798(3) .68834(2) .04692(18) Uani d . 1 . . P
N7 .24979(17) .74987(10) .69000(7) .0492(5) Uani d . 1 . . N
P8 .22970(6) .71821(3) .73847(2) .04611(18) Uani d . 1 C . P
N9 .48496(17) .74131(9) .71314(7) .0454(5) Uani d . 1 . . N
N10 .56986(19) .68315(10) .79493(8) .0541(6) Uani d . 1 . . N
C1A .5518(3) .61740(14) .80311(13) .0835(10) Uani d PD .207(17) A 1 C
H1AA .5077 .5975 .7761 .100 Uiso calc PR .207(17) A 1 H
H1AB .5115 .6107 .8302 .100 Uiso calc PR .207(17) A 1 H
C2A .6769(16) .5951(15) .8114(16) .110(3) Uani d PD .207(17) A 1 C
H2AA .7026 .5835 .7819 .132 Uiso calc PR .207(17) A 1 H
H2AB .6822 .5588 .8314 .132 Uiso calc PR .207(17) A 1 H
C3A .756(4) .6455(11) .834(2) .095(2) Uani d PD .207(17) A 1 C
H3AA .7606 .6444 .8680 .114 Uiso calc PR .207(17) A 1 H
H3AB .8352 .6430 .8255 .114 Uiso calc PR .207(17) A 1 H
C4A .6908(3) .70195(15) .81377(11) .0749(9) Uani d PD .207(17) A 1 C
H4AA .6886 .7334 .8377 .090 Uiso calc PR .207(17) A 1 H
H4AB .7307 .7192 .7891 .090 Uiso calc PR .207(17) A 1 H
C1B .5518(3) .61740(14) .80311(13) .0835(10) Uani d P .793(17) A 2 C
H1BA .5476 .5943 .7741 .100 Uiso calc PR .793(17) A 2 H
H1BB .4791 .6109 .8164 .100 Uiso calc PR .793(17) A 2 H
C2B .6551(7) .5974(3) .8362(4) .110(3) Uani d PD .793(17) A 2 C
H2BA .6752 .5544 .8309 .132 Uiso calc PR .793(17) A 2 H
H2BB .6401 .6020 .8683 .132 Uiso calc PR .793(17) A 2 H
C3B .7519(11) .6406(4) .8254(5) .095(2) Uani d PD .793(17) A 2 C
H3BA .7883 .6254 .7992 .114 Uiso calc PR .793(17) A 2 H
H3BB .8124 .6448 .8522 .114 Uiso calc PR .793(17) A 2 H
C4B .6908(3) .70195(15) .81377(11) .0749(9) Uani d P .793(17) A 2 C
H4BA .6912 .7275 .8414 .090 Uiso calc PR .793(17) A 2 H
H4BB .7282 .7246 .7907 .090 Uiso calc PR .793(17) A 2 H
N11 .37450(19) .90347(10) .79559(8) .0591(6) Uani d . 1 . . N
C5A .2665(3) .93496(18) .77607(12) .0900(11) Uani d PD .825(17) B 1 C
H5AA .2022 .9057 .7681 .108 Uiso calc PR .825(17) B 1 H
H5AB .2780 .9586 .7485 .108 Uiso calc PR .825(17) B 1 H
C6A .2428(10) .9775(5) .8160(2) .142(3) Uani d PD .825(17) B 1 C
H6AA .2724 1.0189 .8113 .170 Uiso calc PR .825(17) B 1 H
H6AB .1585 .9802 .8175 .170 Uiso calc PR .825(17) B 1 H
C7A .3051(7) .9504(5) .8604(2) .104(3) Uani d PD .825(17) B 1 C
H7AA .3267 .9823 .8837 .125 Uiso calc PR .825(17) B 1 H
H7AB .2569 .9193 .8731 .125 Uiso calc PR .825(17) B 1 H
C8A .4122(3) .92202(16) .84414(11) .0783(10) Uani d PD .825(17) B 1 C
H8AA .4763 .9519 .8459 .094 Uiso calc PR .825(17) B 1 H
H8AB .4387 .8863 .8631 .094 Uiso calc PR .825(17) B 1 H
C5B .2665(3) .93496(18) .77607(12) .0900(11) Uani d P .175(17) B 2 C
H5BA .2109 .9071 .7583 .108 Uiso calc PR .175(17) B 2 H
H5BB .2820 .9702 .7569 .108 Uiso calc PR .175(17) B 2 H
C6B .226(4) .955(2) .8212(11) .142(3) Uani d PD .175(17) B 2 C
H6BA .1658 .9868 .8162 .170 Uiso calc PR .175(17) B 2 H
H6BB .1947 .9197 .8370 .170 Uiso calc PR .175(17) B 2 H
C7B .338(3) .9786(15) .8478(15) .104(3) Uani d PD .175(17) B 2 C
H7BA .3683 1.0144 .8328 .125 Uiso calc PR .175(17) B 2 H
H7BB .3294 .9885 .8799 .125 Uiso calc PR .175(17) B 2 H
C8B .4122(3) .92202(16) .84414(11) .0783(10) Uani d P .175(17) B 2 C
H8BA .4960 .9317 .8495 .094 Uiso calc PR .175(17) B 2 H
H8BB .3949 .8901 .8659 .094 Uiso calc PR .175(17) B 2 H
N12 .5785(2) .90199(10) .76797(8) .0614(6) Uani d . 1 . . N
C9A .6850(3) .87427(17) .75484(13) .0853(10) Uani d PD .202(16) B 1 C
H9AA .6694 .8330 .7420 .102 Uiso calc PR .202(16) B 1 H
H9AB .7468 .8718 .7814 .102 Uiso calc PR .202(16) B 1 H
C10A .719(4) .9188(16) .7180(12) .144(4) Uani d PD .202(16) B 1 C
H10A .8016 .9156 .7140 .173 Uiso calc PR .202(16) B 1 H
H10B .6694 .9140 .6882 .173 Uiso calc PR .202(16) B 1 H
C11A .692(2) .978(2) .743(2) .190(5) Uani d PD .202(16) B 1 C
H11A .7419 .9821 .7727 .228 Uiso calc PR .202(16) B 1 H
H11B .6990 1.0142 .7240 .228 Uiso calc PR .202(16) B 1 H
C12A .5671(3) .96528(16) .74929(14) .0962(12) Uani d PD .202(16) B 1 C
H12A .5391 .9939 .7713 .115 Uiso calc PR .202(16) B 1 H
H12B .5150 .9669 .7199 .115 Uiso calc PR .202(16) B 1 H
C9B .6850(3) .87427(17) .75484(13) .0853(10) Uani d P .798(16) B 2 C
H9BA .6668 .8484 .7273 .102 Uiso calc PR .798(16) B 2 H
H9BB .7249 .8493 .7801 .102 Uiso calc PR .798(16) B 2 H
C10B .7600(7) .9292(4) .7449(5) .144(4) Uani d PD .798(16) B 2 C
H10C .8137 .9185 .7228 .173 Uiso calc PR .798(16) B 2 H
H10D .8053 .9449 .7733 .173 Uiso calc PR .798(16) B 2 H
C11B .6674(7) .9762(6) .7240(5) .190(5) Uani d PD .798(16) B 2 C
H11C .6967 1.0183 .7289 .228 Uiso calc PR .798(16) B 2 H
H11D .6458 .9692 .6908 .228 Uiso calc PR .798(16) B 2 H
C12B .5671(3) .96528(16) .74929(14) .0962(12) Uani d P .798(16) B 2 C
H12C .4935 .9697 .7284 .115 Uiso calc PR .798(16) B 2 H
H12D .5674 .9950 .7745 .115 Uiso calc PR .798(16) B 2 H
N13 .3827(2) .79886(13) .63406(8) .0620(7) Uani d . 1 . . N
H13 .339(2) .7788(11) .6153(9) .045(8) Uiso d . 1 . . H
N14 .1404(2) .65953(11) .72376(7) .0608(6) Uani d . 1 . . N
C13A .1425(3) .62096(17) .68396(12) .0908(11) Uani d PD .37(3) C 1 C
H13A .2112 .5940 .6880 .109 Uiso calc PR .37(3) C 1 H
H13B .1442 .6458 .6560 .109 Uiso calc PR .37(3) C 1 H
C14A .030(3) .5835(19) .6807(13) .108(5) Uani d PD .37(3) C 1 C
H14A -.0396 .6076 .6685 .130 Uiso calc PR .37(3) C 1 H
H14B .0332 .5459 .6624 .130 Uiso calc PR .37(3) C 1 H
C15A .034(3) .5703(14) .7316(12) .101(4) Uani d PD .37(3) C 1 C
H15A .0816 .5334 .7396 .121 Uiso calc PR .37(3) C 1 H
H15B -.0448 .5628 .7391 .121 Uiso calc PR .37(3) C 1 H
C16A .0879(3) .62429(17) .75916(11) .0870(11) Uani d PD .37(3) C 1 C
H16A .0282 .6484 .7720 .104 Uiso calc PR .37(3) C 1 H
H16B .1476 .6110 .7843 .104 Uiso calc PR .37(3) C 1 H
C13B .1425(3) .62096(17) .68396(12) .0908(11) Uani d P .63(3) C 2 C
H13C .2209 .6038 .6833 .109 Uiso calc PR .63(3) C 2 H
H13D .1199 .6443 .6554 .109 Uiso calc PR .63(3) C 2 H
C14B .0545(13) .5700(8) .6888(8) .108(5) Uani d PD .63(3) C 2 C
H14C -.0096 .5719 .6631 .130 Uiso calc PR .63(3) C 2 H
H14D .0926 .5299 .6881 .130 Uiso calc PR .63(3) C 2 H
C15B .0073(17) .5782(9) .7338(7) .101(4) Uani d PD .63(3) C 2 C
H15C -.0733 .5937 .7288 .121 Uiso calc PR .63(3) C 2 H
H15D .0090 .5394 .7509 .121 Uiso calc PR .63(3) C 2 H
C16B .0879(3) .62429(17) .75916(11) .0870(11) Uani d P .63(3) C 2 C
H16C .0445 .6517 .7773 .104 Uiso calc PR .63(3) C 2 H
H16D .1491 .6036 .7802 .104 Uiso calc PR .63(3) C 2 H
N15 .15265(19) .76191(11) .76978(7) .0595(6) Uani d . 1 . . N
C17A .0354(3) .7854(2) .75284(12) .0947(12) Uani d PD .509(12) C 1 C
H17A -.0075 .7573 .7304 .114 Uiso calc PR .509(12) C 1 H
H17B .0390 .8261 .7388 .114 Uiso calc PR .509(12) C 1 H
C18A -.0197(12) .7881(8) .7980(4) .098(3) Uani d PD .509(12) C 1 C
H18A -.0854 .8170 .7953 .118 Uiso calc PR .509(12) C 1 H
H18B -.0475 .7475 .8061 .118 Uiso calc PR .509(12) C 1 H
C19A .0802(13) .8100(12) .8336(7) .104(3) Uani d PD .509(12) C 1 C
H19A .0921 .8544 .8315 .125 Uiso calc PR .509(12) C 1 H
H19B .0666 .7995 .8651 .125 Uiso calc PR .509(12) C 1 H
C20A .1821(3) .77473(15) .81960(9) .0643(8) Uani d PD .509(12) C 1 C
H20A .2541 .7991 .8254 .077 Uiso calc PR .509(12) C 1 H
H20B .1936 .7363 .8371 .077 Uiso calc PR .509(12) C 1 H
C17B .0354(3) .7854(2) .75284(12) .0947(12) Uani d P .491(12) C 2 C
H17C -.0192 .7513 .7449 .114 Uiso calc PR .491(12) C 2 H
H17D .0376 .8107 .7252 .114 Uiso calc PR .491(12) C 2 H
C18B -.0026(13) .8233(7) .7915(5) .098(3) Uani d PD .491(12) C 2 C
H18C -.0863 .8178 .7933 .118 Uiso calc PR .491(12) C 2 H
H18D .0129 .8671 .7871 .118 Uiso calc PR .491(12) C 2 H
C19B .0708(14) .7990(12) .8345(7) .104(3) Uani d PD .491(12) C 2 C
H19C .0882 .8318 .8573 .125 Uiso calc PR .491(12) C 2 H
H19D .0291 .7661 .8483 .125 Uiso calc PR .491(12) C 2 H
C20B .1821(3) .77473(15) .81960(9) .0643(8) Uani d P .491(12) C 2 C
H20C .2448 .8053 .8250 .077 Uiso calc PR .491(12) C 2 H
H20D .2074 .7372 .8366 .077 Uiso calc PR .491(12) C 2 H
C21 .5032(3) .68387(14) .68630(10) .0651(8) Uani d . 1 . . C
H21A .4743 .6487 .7024 .078 Uiso calc R 1 . . H
H21B .4559 .6868 .6559 .078 Uiso calc R 1 . . H
C22 .6262(4) .6719(3) .6796(2) .158(2) Uani d . 1 . . C
H22A .6669 .6586 .7097 .190 Uiso calc R 1 . . H
H22B .6250 .6364 .6589 .190 Uiso calc R 1 . . H
C23 .6976(5) .7164(3) .6626(2) .186(3) Uani d . 1 . . C
H23A .7745 .6990 .6609 .278 Uiso calc R 1 . . H
H23B .7051 .7515 .6832 .278 Uiso calc R 1 . . H
H23C .6627 .7292 .6321 .278 Uiso calc R 1 . . H
C24 .4600(3) .84573(17) .61711(11) .0813(10) Uani d . 1 . . C
H24A .5143 .8608 .6435 .098 Uiso calc R 1 . . H
H24B .5069 .8259 .5957 .098 Uiso calc R 1 . . H
C25 .4006(4) .8977(2) .59405(17) .1232(16) Uani d . 1 . . C
H25A .3581 .9198 .6159 .148 Uiso calc R 1 . . H
H25B .3432 .8831 .5686 .148 Uiso calc R 1 . . H
C26 .4864(5) .9422(2) .57486(19) .163(2) Uani d . 1 . . C
H26A .4432 .9765 .5597 .245 Uiso calc R 1 . . H
H26B .5275 .9207 .5527 .245 Uiso calc R 1 . . H
H26C .5426 .9573 .6001 .245 Uiso calc R 1 . . H
N1' .01902(18) .73300(9) .93977(7) .0473(5) Uani d . 1 . . N
P2' .03272(6) .79705(3) .96671(2) .03945(16) Uani d . 1 . . P
N3' .15650(17) .83197(10) .97359(7) .0474(5) Uani d . 1 . . N
P4' .26129(6) .81276(3) 1.01283(2) .04435(17) Uani d . 1 D . P
N5' .22810(17) .76900(10) 1.05396(7) .0458(5) Uani d . 1 . . N
P6' .10374(6) .73303(3) 1.04896(2) .04014(16) Uani d . 1 . . P
N7' .09068(18) .67086(9) 1.01919(6) .0460(5) Uani d . 1 . . N
P8' .04384(6) .66789(3) .96510(2) .04333(17) Uani d . 1 E . P
N9' -.00204(16) .78167(9) 1.02180(6) .0400(5) Uani d . 1 . . N
N10' -.06239(18) .84547(9) .93969(7) .0476(5) Uani d . 1 . . N
C27 -.1737(2) .82553(13) .91193(10) .0594(7) Uani d D 1 . . C
H27A -.2234 .8037 .9313 .071 Uiso calc R 1 . . H
H27B -.1583 .7985 .8866 .071 Uiso calc R 1 . . H
C28 -.2315(3) .88441(17) .89340(13) .0906(11) Uani d D 1 . . C
H28A -.2758 .8781 .8627 .109 Uiso calc R 1 . . H
H28B -.2845 .9003 .9142 .109 Uiso calc R 1 . . H
C29 -.1307(3) .92750(17) .89111(13) .0949(12) Uani d D 1 . . C
H29A -.1562 .9704 .8922 .114 Uiso calc R 1 . . H
H29B -.0957 .9210 .8627 .114 Uiso calc R 1 . . H
C30 -.0443(3) .91176(13) .93338(11) .0724(9) Uani d D 1 . . C
H30A .0363 .9203 .9280 .087 Uiso calc R 1 . . H
H30B -.0611 .9351 .9604 .087 Uiso calc R 1 . . H
N11' .36406(18) .78368(11) .98481(7) .0565(6) Uani d . 1 . . N
C31A .3589(3) .77980(17) .93453(10) .0800(10) Uani d PD .427(12) D 1 C
H31A .3309 .8184 .9197 .096 Uiso calc PR .427(12) D 1 H
H31B .3073 .7463 .9220 .096 Uiso calc PR .427(12) D 1 H
C32A .4855(13) .7672(14) .9274(8) .123(3) Uani d PD .427(12) D 1 C
H32A .4885 .7407 .9004 .147 Uiso calc PR .427(12) D 1 H
H32B .5266 .8056 .9228 .147 Uiso calc PR .427(12) D 1 H
C33A .5400(14) .7354(8) .9711(5) .098(3) Uani d PD .427(12) D 1 C
H33A .5233 .6912 .9700 .117 Uiso calc PR .427(12) D 1 H
H33B .6250 .7416 .9764 .117 Uiso calc PR .427(12) D 1 H
C34A .4813(3) .76650(19) 1.00769(12) .0882(11) Uani d PD .427(12) D 1 C
H34A .4754 .7385 1.0336 .106 Uiso calc PR .427(12) D 1 H
H34B .5254 .8030 1.0194 .106 Uiso calc PR .427(12) D 1 H
C31B .3589(3) .77980(17) .93453(10) .0800(10) Uani d P .573(12) D 2 C
H31C .3470 .8205 .9203 .096 Uiso calc PR .573(12) D 2 H
H31D .2952 .7527 .9213 .096 Uiso calc PR .573(12) D 2 H
C32B .4781(9) .7534(10) .9270(6) .123(3) Uani d PD .573(12) D 2 C
H32C .4750 .7085 .9245 .147 Uiso calc PR .573(12) D 2 H
H32D .5042 .7704 .8990 .147 Uiso calc PR .573(12) D 2 H
C33B .5583(9) .7733(7) .9698(4) .098(3) Uani d PD .573(12) D 2 C
H33C .5837 .8160 .9671 .117 Uiso calc PR .573(12) D 2 H
H33D .6274 .7468 .9754 .117 Uiso calc PR .573(12) D 2 H
C34B .4813(3) .76650(19) 1.00769(12) .0882(11) Uani d P .573(12) D 2 C
H34C .4822 .7241 1.0190 .106 Uiso calc PR .573(12) D 2 H
H34D .5070 .7940 1.0337 .106 Uiso calc PR .573(12) D 2 H
N12' .3279(2) .87301(11) 1.03988(7) .0607(6) Uani d . 1 . . N
C35 .3787(3) .92183(16) 1.01382(12) .0916(11) Uani d D 1 D . C
H35A .3221 .9357 .9878 .110 Uiso calc R 1 . . H
H35B .4492 .9071 1.0019 .110 Uiso calc R 1 . . H
C36 .4085(5) .97335(19) 1.04831(15) .1216(15) Uani d D 1 . . C
H36A .4913 .9846 1.0498 .146 Uiso calc R 1 D . H
H36B .3607 1.0097 1.0391 .146 Uiso calc R 1 . . H
C37 .3834(3) .95028(16) 1.09453(13) .0853(10) Uani d D 1 D . C
H37A .3518 .9831 1.1122 .102 Uiso calc R 1 . . H
H37B .4545 .9339 1.1126 .102 Uiso calc R 1 . . H
C38 .2934(3) .89998(15) 1.08238(10) .0711(9) Uani d D 1 D . C
H38A .2968 .8693 1.1071 .085 Uiso calc R 1 . . H
H38B .2140 .9170 1.0767 .085 Uiso calc R 1 . . H
N13' .0751(2) .72003(12) 1.10119(9) .0528(7) Uani d . 1 . . N
H13' .114(2) .7277(12) 1.1205(9) .043(9) Uiso d . 1 . . H
N14' .1396(2) .62516(10) .94170(7) .0575(6) Uani d . 1 . . N
C39A .2613(3) .61582(16) .96217(11) .0769(9) Uani d PD .674(16) E 1 C
H39A .2650 .5964 .9926 .092 Uiso calc PR .674(16) E 1 H
H39B .3032 .6551 .9656 .092 Uiso calc PR .674(16) E 1 H
C40A .3142(10) .5738(6) .9286(3) .109(3) Uani d PD .674(16) E 1 C
H40A .3001 .5305 .9349 .131 Uiso calc PR .674(16) E 1 H
H40B .3986 .5807 .9298 .131 Uiso calc PR .674(16) E 1 H
C41A .2470(9) .5938(7) .8812(3) .110(4) Uani d PD .674(16) E 1 C
H41A .2858 .6289 .8686 .132 Uiso calc PR .674(16) E 1 H
H41B .2428 .5599 .8589 .132 Uiso calc PR .674(16) E 1 H
C42A .1240(3) .61166(16) .89130(10) .0843(11) Uani d PD .674(16) E 1 C
H42A .0951 .6479 .8734 .101 Uiso calc PR .674(16) E 1 H
H42B .0687 .5778 .8839 .101 Uiso calc PR .674(16) E 1 H
C39B .2613(3) .61582(16) .96217(11) .0769(9) Uani d P .326(16) E 2 C
H39C .2685 .5818 .9844 .092 Uiso calc PR .326(16) E 2 H
H39D .2947 .6531 .9774 .092 Uiso calc PR .326(16) E 2 H
C40B .319(2) .6003(10) .9193(6) .109(3) Uani d PD .326(16) E 2 C
H40C .3429 .6377 .9044 .131 Uiso calc PR .326(16) E 2 H
H40D .3879 .5741 .9273 .131 Uiso calc PR .326(16) E 2 H
C41B .2234(17) .5664(10) .8879(10) .110(4) Uani d PD .326(16) E 2 C
H41C .2418 .5625 .8562 .132 Uiso calc PR .326(16) E 2 H
H41D .2071 .5258 .9000 .132 Uiso calc PR .326(16) E 2 H
C42B .1240(3) .61166(16) .89130(10) .0843(11) Uani d P .326(16) E 2 C
H42C .1326 .6488 .8731 .101 Uiso calc PR .326(16) E 2 H
H42D .0475 .5930 .8811 .101 Uiso calc PR .326(16) E 2 H
N15' -.0785(2) .62664(10) .95272(8) .0564(6) Uani d . 1 . . N
C43A -.0746(4) .56145(16) .96743(14) .0973(12) Uani d PD .290(13) E 1 C
H43A .0008 .5512 .9855 .117 Uiso calc PR .290(13) E 1 H
H43B -.0889 .5337 .9408 .117 Uiso calc PR .290(13) E 1 H
C44A -.1734(19) .5588(10) .9968(10) .148(4) Uani d PD .290(13) E 1 C
H44A -.1434 .5686 1.0290 .178 Uiso calc PR .290(13) E 1 H
H44B -.2065 .5173 .9959 .178 Uiso calc PR .290(13) E 1 H
C45A -.268(2) .6047(15) .978(2) .154(2) Uani d PD .290(13) E 1 C
H45A -.3121 .6191 1.0027 .184 Uiso calc PR .290(13) E 1 H
H45B -.3215 .5878 .9527 .184 Uiso calc PR .290(13) E 1 H
C46A -.1903(3) .65497(16) .96260(11) .0781(9) Uani d PD .290(13) E 1 C
H46A -.2302 .6748 .9347 .094 Uiso calc PR .290(13) E 1 H
H46B -.1743 .6862 .9868 .094 Uiso calc PR .290(13) E 1 H
C43B -.0746(4) .56145(16) .96743(14) .0973(12) Uani d P .710(13) E 2 C
H43C -.0348 .5574 .9991 .117 Uiso calc PR .710(13) E 2 H
H43D -.0329 .5365 .9469 .117 Uiso calc PR .710(13) E 2 H
C44B -.1993(7) .5416(4) .9645(5) .148(4) Uani d PD .710(13) E 2 C
H44C -.2084 .5081 .9862 .178 Uiso calc PR .710(13) E 2 H
H44D -.2304 .5286 .9331 .178 Uiso calc PR .710(13) E 2 H
C45B -.2584(11) .6001(6) .9781(9) .154(2) Uani d PD .710(13) E 2 C
H45C -.2584 .6013 1.0117 .184 Uiso calc PR .710(13) E 2 H
H45D -.3398 .6014 .9631 .184 Uiso calc PR .710(13) E 2 H
C46B -.1903(3) .65497(16) .96260(11) .0781(9) Uani d P .710(13) E 2 C
H46C -.2324 .6742 .9349 .094 Uiso calc PR .710(13) E 2 H
H46D -.1761 .6858 .9872 .094 Uiso calc PR .710(13) E 2 H
C47 -.0327(2) .83818(12) 1.04840(9) .0521(7) Uani d . 1 . . C
H47A .0009 .8341 1.0809 .063 Uiso calc R 1 . . H
H47B .0016 .8747 1.0359 .063 Uiso calc R 1 . . H
C48 -.1641(3) .84632(17) 1.04517(12) .0828(10) Uani d . 1 . . C
H48A -.1973 .8109 1.0595 .099 Uiso calc R 1 . . H
H48B -.1978 .8472 1.0125 .099 Uiso calc R 1 . . H
C49 -.1988(4) .9046(2) 1.06846(15) .1306(17) Uani d . 1 . . C
H49A -.2835 .9074 1.0653 .196 Uiso calc R 1 . . H
H49B -.1678 .9399 1.0540 .196 Uiso calc R 1 . . H
H49C -.1673 .9036 1.1010 .196 Uiso calc R 1 . . H
C50 -.0032(3) .67237(17) 1.11358(10) .0812(10) Uani d . 1 . . C
H50A -.0609 .6630 1.0867 .097 Uiso calc R 1 . . H
H50B -.0456 .6878 1.1382 .097 Uiso calc R 1 . . H
C51 .0622(5) .6123(2) 1.13033(19) .150(2) Uani d . 1 . . C
H51A .0998 .5961 1.1047 .180 Uiso calc R 1 . . H
H51B .1247 .6231 1.1552 .180 Uiso calc R 1 . . H
C52 -.0063(8) .5631(3) 1.1470(2) .248(4) Uani d . 1 . . C
H52A .0443 .5285 1.1564 .372 Uiso calc R 1 . . H
H52B -.0670 .5504 1.1226 .372 Uiso calc R 1 . . H
H52C -.0421 .5776 1.1733 .372 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 '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_publ_flag
P8 N1 P2 122.07(14) yes
N3 P2 N1 120.53(12) yes
N3 P2 N10 107.78(12) ?
N1 P2 N10 106.50(12) ?
N3 P2 N9 105.18(11) yes
N1 P2 N9 106.95(11) yes
N10 P2 N9 109.64(12) ?
P4 N3 P2 121.15(13) yes
N5 P4 N3 116.48(11) yes
N5 P4 N11 106.43(13) ?
N3 P4 N11 112.06(12) ?
N5 P4 N12 112.99(13) ?
N3 P4 N12 106.08(12) ?
N11 P4 N12 101.94(13) ?
P6 N5 P4 124.88(14) yes
N5 P6 N13 110.05(14) ?
N5 P6 N7 118.27(12) yes
N13 P6 N7 106.75(13) ?
N5 P6 N9 105.16(11) yes
N13 P6 N9 109.36(13) ?
N7 P6 N9 107.01(12) yes
P8 N7 P6 117.81(12) yes
N1 P8 N7 116.79(12) yes
N1 P8 N15 105.80(12) ?
N7 P8 N15 112.83(12) ?
N1 P8 N14 112.73(13) ?
N7 P8 N14 104.95(11) ?
N15 P8 N14 103.01(13) ?
C21 N9 P2 116.24(18) ?
C21 N9 P6 114.78(17) ?
P2 N9 P6 107.86(12) yes
C1A N10 C4A 110.7(2) ?
C1A N10 P2 125.6(2) ?
C4A N10 P2 123.55(19) ?
N10 C1A C2A 100.7(13) ?
C1A C2A C3A 110(3) ?
C4A C3A C2A 100(2) ?
N10 C4A C3A 108.2(17) ?
C5A N11 C8A 111.6(2) ?
C5A N11 P4 126.1(2) ?
C8A N11 P4 121.85(19) ?
N11 C5A C6A 102.4(4) ?
C7A C6A C5A 107.5(5) ?
C8A C7A C6A 101.8(7) ?
N11 C8A C7A 105.3(3) ?
C9A N12 C12A 108.9(3) ?
C9A N12 P4 119.6(2) ?
C12A N12 P4 118.3(2) ?
N12 C9A C10A 102.9(16) ?
C11A C10A C9A 96(3) ?
C12A C11A C10A 100(2) ?
N12 C12A C11A 100(2) ?
C24 N13 P6 124.0(2) ?
C13A N14 C16A 108.3(2) ?
C13A N14 P8 125.6(2) ?
C16A N14 P8 121.03(19) ?
N14 C13A C14A 104.9(16) ?
C15A C14A C13A 97(2) ?
C14A C15A C16A 110(3) ?
N14 C16A C15A 102.0(16) ?
C17A N15 C20A 110.2(2) ?
C17A N15 P8 123.5(2) ?
C20A N15 P8 125.67(19) ?
N15 C17A C18A 101.1(6) ?
C19A C18A C17A 103.6(12) ?
C20A C19A C18A 101.6(12) ?
N15 C20A C19A 106.3(8) ?
C22 C21 N9 114.8(3) ?
C23 C22 C21 122.8(5) ?
C25 C24 N13 115.3(3) ?
C24 C25 C26 112.0(4) ?
P2' N1' P8' 122.93(13) yes
N1' P2' N3' 120.14(12) yes
N1' P2' N10' 107.94(11) ?
N3' P2' N10' 106.29(12) ?
N1' P2' N9' 105.48(10) yes
N3' P2' N9' 106.64(11) yes
N10' P2' N9' 110.19(11) ?
P4' N3' P2' 122.48(14) yes
N3' P4' N5' 116.93(12) yes
N3' P4' N11' 105.48(12) ?
N5' P4' N11' 113.47(12) ?
N3' P4' N12' 112.84(13) ?
N5' P4' N12' 104.59(12) ?
N11' P4' N12' 102.79(13) ?
P4' N5' P6' 120.77(13) yes
N7' P6' N5' 118.24(12) yes
N7' P6' N13' 110.17(13) ?
N5' P6' N13' 106.70(13) ?
N7' P6' N9' 105.06(11) yes
N5' P6' N9' 107.83(12) yes
N13' P6' N9' 108.52(13) ?
P8' N7' P6' 124.29(13) yes
N7' P8' N1' 115.73(11) yes
N7' P8' N14' 105.92(12) ?
N1' P8' N14' 113.10(12) ?
N7' P8' N15' 113.47(12) ?
N1' P8' N15' 106.39(12) ?
N14' P8' N15' 101.43(13) ?
C47 N9' P6' 117.38(15) ?
C47 N9' P2' 114.44(16) ?
P6' N9' P2' 107.84(11) yes
C30 N10' C27 110.1(2) ?
C30 N10' P2' 126.27(19) ?
C27 N10' P2' 123.03(18) ?
N10' C27 C28 104.7(2) ?
C29 C28 C27 103.9(3) ?
C28 C29 C30 104.5(3) ?
N10' C30 C29 103.6(3) ?
C31A N11' C34A 110.6(2) ?
C31A N11' P4' 125.68(19) ?
C34A N11' P4' 123.18(19) ?
N11' C31A C32A 103.7(9) ?
C33A C32A C31A 105.2(13) ?
C34A C33A C32A 102.6(13) ?
N11' C34A C33A 105.4(7) ?
C35 N12' C38 108.5(2) ?
C35 N12' P4' 120.89(19) ?
C38 N12' P4' 123.62(19) ?
N12' C35 C36 105.1(3) ?
C37 C36 C35 107.2(3) ?
C36 C37 C38 103.8(3) ?
N12' C38 C37 103.3(3) ?
C50 N13' P6' 124.6(2) ?
C39A N14' C42A 111.0(2) ?
C39A N14' P8' 124.33(19) ?
C42A N14' P8' 121.31(19) ?
N14' C39A C40A 105.3(5) ?
C39A C40A C41A 102.2(7) ?
C42A C41A C40A 105.1(7) ?
N14' C42A C41A 104.4(5) ?
C43A N15' C46A 109.5(3) ?
C43A N15' P8' 117.4(2) ?
C46A N15' P8' 117.53(19) ?
N15' C43A C44A 101.8(9) ?
C43A C44A C45A 109(2) ?
C44A C45A C46A 99.3(16) ?
N15' C46A C45A 108.5(14) ?
C48 C47 N9' 111.2(2) ?
C47 C48 C49 113.0(3) ?
N13' C50 C51 112.8(3) ?
C52 C51 C50 117.6(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 P8 . 1.587(2) yes
N1 P2 . 1.594(2) yes
P2 N3 . 1.589(2) yes
P2 N10 . 1.630(2) ?
P2 N9 . 1.715(2) yes
N3 P4 . 1.588(2) yes
P4 N5 . 1.584(2) yes
P4 N11 . 1.640(2) ?
P4 N12 . 1.655(3) ?
N5 P6 . 1.584(2) yes
P6 N13 . 1.610(2) ?
P6 N7 . 1.611(2) yes
P6 N9 . 1.724(2) yes
N7 P8 . 1.602(2) yes
P8 N15 . 1.640(2) ?
P8 N14 . 1.643(2) ?
N9 C21 . 1.490(3) ?
N10 C1A . 1.455(4) ?
N10 C4A . 1.470(4) ?
C1A C2A . 1.494(14) ?
C2A C3A . 1.505(15) ?
C3A C4A . 1.505(14) ?
C2B C3B . 1.509(11) ?
N11 C5A . 1.452(4) ?
N11 C8A . 1.466(3) ?
C5A C6A . 1.526(6) ?
C6A C7A . 1.497(9) ?
C7A C8A . 1.497(6) ?
C6B C7B . 1.496(15) ?
N12 C9A . 1.448(4) ?
N12 C12A . 1.466(4) ?
C9A C10A . 1.520(14) ?
C10A C11A . 1.511(15) ?
C11A C12A . 1.480(14) ?
C10B C11B . 1.527(10) ?
N13 C24 . 1.468(4) ?
N14 C13A . 1.421(4) ?
N14 C16A . 1.465(4) ?
C13A C14A . 1.512(13) ?
C14A C15A . 1.493(14) ?
C15A C16A . 1.493(13) ?
C14B C15B . 1.484(11) ?
N15 C17A . 1.451(4) ?
N15 C20A . 1.460(3) ?
C17A C18A . 1.524(10) ?
C18A C19A . 1.505(14) ?
C19A C20A . 1.489(11) ?
C18B C19B . 1.496(14) ?
C21 C22 . 1.464(5) ?
C22 C23 . 1.390(7) ?
C24 C25 . 1.427(5) ?
C25 C26 . 1.526(5) ?
N1' P2' . 1.582(2) yes
N1' P8' . 1.590(2) yes
P2' N3' . 1.588(2) yes
P2' N10' . 1.627(2) ?
P2' N9' . 1.724(2) yes
N3' P4' . 1.588(2) yes
P4' N5' . 1.602(2) yes
P4' N11' . 1.636(2) ?
P4' N12' . 1.647(2) ?
N5' P6' . 1.606(2) yes
P6' N7' . 1.588(2) yes
P6' N13' . 1.611(3) ?
P6' N9' . 1.707(2) yes
N7' P8' . 1.583(2) yes
P8' N14' . 1.642(2) ?
P8' N15' . 1.652(3) ?
N9' C47 . 1.506(3) ?
N10' C30 . 1.458(3) ?
N10' C27 . 1.472(3) ?
C27 C28 . 1.495(4) ?
C28 C29 . 1.486(5) ?
C29 C30 . 1.501(4) ?
N11' C31A . 1.448(3) ?
N11' C34A . 1.458(4) ?
C31A C32A . 1.511(12) ?
C32A C33A . 1.498(14) ?
C33A C34A . 1.485(10) ?
C32B C33B . 1.498(13) ?
N12' C35 . 1.458(4) ?
N12' C38 . 1.460(4) ?
C35 C36 . 1.500(4) ?
C36 C37 . 1.488(5) ?
C37 C38 . 1.502(4) ?
N13' C50 . 1.437(4) ?
N14' C39A . 1.448(4) ?
N14' C42A . 1.472(3) ?
C39A C40A . 1.511(7) ?
C40A C41A . 1.538(10) ?
C41A C42A . 1.521(8) ?
C40B C41B . 1.510(14) ?
N15' C43A . 1.466(4) ?
N15' C46A . 1.477(4) ?
C43A C44A . 1.501(13) ?
C44A C45A . 1.504(15) ?
C45A C46A . 1.505(14) ?
C44B C45B . 1.506(14) ?
C47 C48 . 1.500(4) ?
C48 C49 . 1.502(5) ?
C50 C51 . 1.539(6) ?
C51 C52 . 1.438(7) ?
