#------------------------------------------------------------------------------
#$Date: 2022-02-04 04:15:01 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272543 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/43/7244337.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_7244337
loop_
_publ_author_name
'Karmakar, Himadri'
'Anga, Srinivas'
'Panda, Tarun K.'
'Chandrasekhar, Vadapalli'
_publ_section_title
;
 Aluminium alkyl complexes supported by imino-phosphanamide ligand as
 precursors for catalytic guanylation reactions of carbodiimides
;
_journal_issue                   8
_journal_name_full               'RSC Advances'
_journal_page_first              4501
_journal_page_last               4509
_journal_paper_doi               10.1039/D2RA00242F
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C39 H47 N4 P'
_chemical_formula_sum            'C39 H49 N4 P'
_chemical_formula_weight         604.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6394)
;
_audit_update_record
;
2021-11-24 deposited with the CCDC.	2022-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.570(2)
_cell_angle_beta                 100.081(2)
_cell_angle_gamma                111.127(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4611(2)
_cell_length_b                   12.4141(3)
_cell_length_c                   16.7883(4)
_cell_measurement_reflns_used    11807
_cell_measurement_temperature    249.99(10)
_cell_measurement_theta_max      28.6720
_cell_measurement_theta_min      2.9910
_cell_volume                     1734.64(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      249.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00  36.00   0.50   10.00    --    7.20 -38.00 150.00  180
  2  ω    -19.00  31.00   0.50   10.00    --    7.20 -57.00  30.00  100
  3  ω    -70.00  37.00   0.50   10.00    --    7.20 -57.00  60.00  214
  4  ω    -80.00 -54.00   0.50   10.00    --    7.20 -57.00  30.00   52
  5  ω    -87.00  17.00   0.50   10.00    --   -7.60 -57.00 120.00  208
  6  ω    -97.00  -7.00   0.50   10.00    --   -7.60 -57.00 -60.00  180
  7  ω    -62.00  20.00   0.50   10.00    --   -7.60 -82.00 -90.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0481428000
_diffrn_orient_matrix_UB_12      0.0284175000
_diffrn_orient_matrix_UB_13      0.0421101000
_diffrn_orient_matrix_UB_21      -0.0183949000
_diffrn_orient_matrix_UB_22      -0.0571764000
_diffrn_orient_matrix_UB_23      0.0073680000
_diffrn_orient_matrix_UB_31      0.0656829000
_diffrn_orient_matrix_UB_32      -0.0035105000
_diffrn_orient_matrix_UB_33      -0.0133902000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27111
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.908
_diffrn_reflns_theta_min         2.617
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         8000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0461
_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)+(0.0690P)²+0.3066P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6548
_reflns_number_total             8000
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ra00242f2.cif
_cod_data_source_block           1b
_cod_original_cell_volume        1734.64(7)
_cod_database_code               7244337
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNP
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C3(H3), C20(H20), C39(H39), C18(H18), C4(H4), C5(H5), C27(H27),
 C29(H29), C36(H36), C37(H37), C38(H38), C14(H14), C15(H15)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C33(H33A,H33B,H33C), C22(H22A,H22B,H22C),
 C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.492
_oxdiff_exptl_absorpt_empirical_full_min 0.601
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.64456(4) 0.34504(3) 0.21893(2) 0.02857(11) Uani 1 1 d . . . . .
N1 N 0.53924(13) 0.28518(10) 0.28602(7) 0.0293(2) Uani 1 1 d . . . . .
H1 H 0.5730(18) 0.3348(14) 0.3341(10) 0.035 Uiso 1 1 d . U . . .
N2 N 0.82531(14) 0.35347(11) 0.25977(7) 0.0350(3) Uani 1 1 d . . . . .
N4 N 1.03562(15) 0.30669(12) 0.22900(9) 0.0452(3) Uani 1 1 d . . . . .
N3 N 0.95096(16) 0.40171(12) 0.14908(9) 0.0450(3) Uani 1 1 d . . . . .
C1 C 0.50973(14) 0.16638(11) 0.29199(8) 0.0279(3) Uani 1 1 d . . . . .
C34 C 0.65785(15) 0.49728(11) 0.26399(8) 0.0305(3) Uani 1 1 d . . . . .
C2 C 0.40985(15) 0.06601(11) 0.22227(8) 0.0311(3) Uani 1 1 d . . . . .
C13 C 0.92484(17) 0.35404(12) 0.21570(9) 0.0357(3) Uani 1 1 d . . . . .
C7 C 0.32653(16) 0.07846(12) 0.14095(9) 0.0352(3) Uani 1 1 d . . . . .
H7 H 0.344792 0.163445 0.150248 0.042 Uiso 1 1 calc R U . . .
C6 C 0.57542(17) 0.14955(12) 0.36867(9) 0.0365(3) Uani 1 1 d . . . . .
C16 C 0.88858(17) 0.48257(13) 0.12275(9) 0.0381(3) Uani 1 1 d . . . . .
C21 C 0.77241(18) 0.44151(13) 0.04667(9) 0.0402(3) Uani 1 1 d . . . . .
C25 C 1.05048(17) 0.23628(13) 0.28543(10) 0.0396(3) Uani 1 1 d . . . . .
C35 C 0.56128(18) 0.53944(14) 0.21904(10) 0.0416(3) Uani 1 1 d . . . . .
H35 H 0.492259 0.490796 0.166712 0.050 Uiso 1 1 calc R U . . .
C3 C 0.38534(18) -0.04897(12) 0.22967(10) 0.0404(3) Uani 1 1 d . . . . .
H3 H 0.321440 -0.115835 0.183892 0.048 Uiso 1 1 calc R U . . .
C17 C 0.95333(18) 0.60274(14) 0.17236(10) 0.0427(3) Uani 1 1 d . . . . .
C20 C 0.71695(19) 0.52230(14) 0.02224(10) 0.0435(4) Uani 1 1 d . . . . .
H20 H 0.636833 0.495499 -0.027371 0.052 Uiso 1 1 calc R U . . .
C39 C 0.75999(19) 0.57217(13) 0.34210(10) 0.0436(4) Uani 1 1 d . . . . .
H39 H 0.825143 0.545551 0.373193 0.052 Uiso 1 1 calc R U . . .
C18 C 0.89531(19) 0.68064(14) 0.14449(11) 0.0454(4) Uani 1 1 d . . . . .
H18 H 0.936435 0.760722 0.176790 0.054 Uiso 1 1 calc R U . . .
C19 C 0.77770(19) 0.64238(14) 0.06981(11) 0.0444(4) Uani 1 1 d . . . . .
C30 C 0.94240(18) 0.11625(14) 0.26485(10) 0.0423(3) Uani 1 1 d . . . . .
C4 C 0.4532(2) -0.06601(13) 0.30292(11) 0.0464(4) Uani 1 1 d . . . . .
H4 H 0.437043 -0.143376 0.305969 0.056 Uiso 1 1 calc R U . . .
C5 C 0.54548(19) 0.03249(14) 0.37176(10) 0.0456(4) Uani 1 1 d . . . . .
H5 H 0.588768 0.020276 0.421538 0.055 Uiso 1 1 calc R U . . .
C26 C 1.18191(19) 0.28636(15) 0.35491(11) 0.0470(4) Uani 1 1 d . . . . .
C27 C 1.2086(2) 0.21173(17) 0.40132(12) 0.0537(4) Uani 1 1 d . . . . .
H27 H 1.296898 0.243625 0.447346 0.064 Uiso 1 1 calc R U . . .
C29 C 0.9738(2) 0.04629(15) 0.31448(12) 0.0487(4) Uani 1 1 d . . . . .
H29 H 0.902464 -0.033351 0.302479 0.058 Uiso 1 1 calc R U . . .
C10 C 0.6763(2) 0.25484(14) 0.44761(10) 0.0498(4) Uani 1 1 d . . . . .
H10 H 0.654837 0.324495 0.440717 0.060 Uiso 1 1 calc R U . . .
C36 C 0.5671(2) 0.65350(16) 0.25167(13) 0.0562(5) Uani 1 1 d . . . . .
H36 H 0.501569 0.680482 0.221258 0.067 Uiso 1 1 calc R U . . .
C8 C 0.3927(2) 0.04403(15) 0.06796(10) 0.0506(4) Uani 1 1 d . . . . .
H8A H 0.503067 0.094593 0.082004 0.076 Uiso 1 1 calc R U . . .
H8B H 0.338958 0.054569 0.018011 0.076 Uiso 1 1 calc R U . . .
H8C H 0.377781 -0.038737 0.057929 0.076 Uiso 1 1 calc R U . . .
C28 C 1.1082(2) 0.09131(17) 0.38149(12) 0.0526(4) Uani 1 1 d . . . . .
C37 C 0.6691(2) 0.72655(15) 0.32853(13) 0.0587(5) Uani 1 1 d . . . . .
H37 H 0.673246 0.803100 0.349929 0.070 Uiso 1 1 calc R U . . .
C9 C 0.1487(2) 0.00453(18) 0.11778(12) 0.0586(5) Uani 1 1 d . . . . .
H9A H 0.126552 -0.079817 0.101871 0.088 Uiso 1 1 calc R U . . .
H9B H 0.098046 0.023850 0.071358 0.088 Uiso 1 1 calc R U . . .
H9C H 0.109876 0.023136 0.165551 0.088 Uiso 1 1 calc R U . . .
C38 C 0.7655(2) 0.68627(15) 0.37404(12) 0.0590(5) Uani 1 1 d . . . . .
H38 H 0.834356 0.735653 0.426235 0.071 Uiso 1 1 calc R U . . .
C33 C 0.7999(2) 0.06426(17) 0.19072(12) 0.0595(5) Uani 1 1 d . . . . .
H33A H 0.725186 0.095987 0.203626 0.089 Uiso 1 1 calc R U . . .
H33B H 0.753033 -0.021906 0.178655 0.089 Uiso 1 1 calc R U . . .
H33C H 0.830160 0.085402 0.142397 0.089 Uiso 1 1 calc R U . . .
C22 C 1.0824(2) 0.64565(17) 0.25281(12) 0.0618(5) Uani 1 1 d . . . . .
H22A H 1.114600 0.730395 0.277569 0.093 Uiso 1 1 calc R U . . .
H22B H 1.170586 0.631311 0.240581 0.093 Uiso 1 1 calc R U . . .
H22C H 1.044510 0.602629 0.291614 0.093 Uiso 1 1 calc R U . . .
C11 C 0.6363(3) 0.23045(19) 0.52913(12) 0.0654(5) Uani 1 1 d . . . . .
H11A H 0.672451 0.171702 0.542872 0.098 Uiso 1 1 calc R U . . .
H11B H 0.524441 0.200463 0.520792 0.098 Uiso 1 1 calc R U . . .
H11C H 0.687142 0.303973 0.574536 0.098 Uiso 1 1 calc R U . . .
C14 C 1.0754(3) 0.3838(2) 0.12358(15) 0.0675(6) Uani 1 1 d . . . . .
H14 H 1.115544 0.408087 0.080288 0.081 Uiso 1 1 calc R U . . .
C24 C 0.7109(3) 0.31318(16) -0.00777(12) 0.0616(5) Uani 1 1 d . . . . .
H24A H 0.796671 0.296863 -0.021795 0.092 Uiso 1 1 calc R U . . .
H24B H 0.635727 0.301784 -0.058650 0.092 Uiso 1 1 calc R U . . .
H24C H 0.661066 0.259192 0.022469 0.092 Uiso 1 1 calc R U . . .
C15 C 1.1264(2) 0.32584(19) 0.17223(14) 0.0655(6) Uani 1 1 d . . . . .
H15 H 1.208498 0.302209 0.168897 0.079 Uiso 1 1 calc R U . . .
C23 C 0.7187(3) 0.72926(18) 0.04018(15) 0.0685(5) Uani 1 1 d . . . . .
H23A H 0.802522 0.790273 0.028555 0.103 Uiso 1 1 calc R U . . .
H23B H 0.682489 0.766339 0.083382 0.103 Uiso 1 1 calc R U . . .
H23C H 0.633389 0.686457 -0.010261 0.103 Uiso 1 1 calc R U . . .
C31 C 1.2924(2) 0.41851(17) 0.37952(16) 0.0725(6) Uani 1 1 d . . . . .
H31A H 1.347374 0.433249 0.337207 0.109 Uiso 1 1 calc R U . . .
H31B H 1.366957 0.439246 0.432880 0.109 Uiso 1 1 calc R U . . .
H31C H 1.232887 0.466762 0.384083 0.109 Uiso 1 1 calc R U . . .
C32 C 1.1466(3) 0.0104(2) 0.43009(16) 0.0781(6) Uani 1 1 d . . . . .
H32A H 1.234964 -0.002535 0.416897 0.117 Uiso 1 1 calc R U . . .
H32B H 1.057250 -0.065564 0.414604 0.117 Uiso 1 1 calc R U . . .
H32C H 1.171883 0.048074 0.489580 0.117 Uiso 1 1 calc R U . . .
C12 C 0.8480(3) 0.2886(3) 0.45670(15) 0.1049(11) Uani 1 1 d . . . . .
H12A H 0.908066 0.357214 0.505195 0.157 Uiso 1 1 calc R U . . .
H12B H 0.873337 0.308300 0.407035 0.157 Uiso 1 1 calc R U . . .
H12C H 0.872968 0.222099 0.463717 0.157 Uiso 1 1 calc R 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 C34 93.10(6) . . ?
N2 P1 N1 102.91(6) . . ?
N2 P1 C34 104.11(6) . . ?
P1 N1 H1 110.1(11) . . ?
C1 N1 P1 121.78(9) . . ?
C1 N1 H1 110.8(11) . . ?
C13 N2 P1 122.98(10) . . ?
C13 N4 C25 127.44(12) . . ?
C13 N4 C15 110.05(13) . . ?
C15 N4 C25 122.21(13) . . ?
C13 N3 C16 125.65(12) . . ?
C13 N3 C14 109.87(13) . . ?
C14 N3 C16 122.89(13) . . ?
C2 C1 N1 119.58(11) . . ?
C2 C1 C6 120.40(12) . . ?
C6 C1 N1 119.97(11) . . ?
C35 C34 P1 119.12(11) . . ?
C39 C34 P1 122.49(11) . . ?
C39 C34 C35 118.39(13) . . ?
C1 C2 C7 122.65(12) . . ?
C3 C2 C1 118.18(12) . . ?
C3 C2 C7 119.16(12) . . ?
N2 C13 N4 125.01(13) . . ?
N2 C13 N3 130.67(13) . . ?
N4 C13 N3 104.30(12) . . ?
C2 C7 H7 107.6 . . ?
C2 C7 C8 111.75(12) . . ?
C2 C7 C9 111.57(13) . . ?
C8 C7 H7 107.6 . . ?
C8 C7 C9 110.41(13) . . ?
C9 C7 H7 107.6 . . ?
C1 C6 C10 122.48(12) . . ?
C5 C6 C1 118.29(13) . . ?
C5 C6 C10 119.22(13) . . ?
C21 C16 N3 119.48(14) . . ?
C21 C16 C17 121.86(14) . . ?
C17 C16 N3 118.56(14) . . ?
C16 C21 C24 120.73(15) . . ?
C20 C21 C16 118.09(14) . . ?
C20 C21 C24 121.18(15) . . ?
C30 C25 N4 119.43(14) . . ?
C26 C25 N4 118.37(14) . . ?
C26 C25 C30 121.88(14) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 C34 120.60(15) . . ?
C36 C35 H35 119.7 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.76(13) . . ?
C4 C3 H3 119.1 . . ?
C16 C17 C22 120.77(15) . . ?
C18 C17 C16 117.81(15) . . ?
C18 C17 C22 121.42(15) . . ?
C21 C20 H20 119.1 . . ?
C21 C20 C19 121.85(15) . . ?
C19 C20 H20 119.1 . . ?
C34 C39 H39 119.7 . . ?
C38 C39 C34 120.61(15) . . ?
C38 C39 H39 119.7 . . ?
C17 C18 H18 119.0 . . ?
C19 C18 C17 121.90(15) . . ?
C19 C18 H18 119.0 . . ?
C20 C19 C23 120.67(16) . . ?
C18 C19 C20 118.45(14) . . ?
C18 C19 C23 120.87(16) . . ?
C25 C30 C33 121.24(15) . . ?
C29 C30 C25 117.55(15) . . ?
C29 C30 C33 121.19(15) . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.53(13) . . ?
C5 C4 H4 120.2 . . ?
C6 C5 H5 119.1 . . ?
C4 C5 C6 121.73(14) . . ?
C4 C5 H5 119.1 . . ?
C25 C26 C31 121.24(16) . . ?
C27 C26 C25 117.96(15) . . ?
C27 C26 C31 120.81(17) . . ?
C26 C27 H27 118.9 . . ?
C28 C27 C26 122.19(17) . . ?
C28 C27 H27 118.9 . . ?
C30 C29 H29 118.9 . . ?
C30 C29 C28 122.16(15) . . ?
C28 C29 H29 118.9 . . ?
C6 C10 H10 107.4 . . ?
C6 C10 C11 113.00(14) . . ?
C11 C10 H10 107.4 . . ?
C12 C10 C6 111.47(17) . . ?
C12 C10 H10 107.4 . . ?
C12 C10 C11 109.87(16) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 C35 120.33(16) . . ?
C37 C36 H36 119.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C27 C28 C29 118.12(15) . . ?
C27 C28 C32 120.73(18) . . ?
C29 C28 C32 121.13(18) . . ?
C36 C37 H37 120.1 . . ?
C36 C37 C38 119.90(15) . . ?
C38 C37 H37 120.1 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C39 C38 H38 119.9 . . ?
C37 C38 C39 120.18(17) . . ?
C37 C38 H38 119.9 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C14 H14 126.1 . . ?
C15 C14 N3 107.73(15) . . ?
C15 C14 H14 126.1 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N4 C15 H15 126.0 . . ?
C14 C15 N4 108.05(15) . . ?
C14 C15 H15 126.0 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C31 H31A 109.5 . . ?
C26 C31 H31B 109.5 . . ?
C26 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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
P1 N1 1.7346(11) . ?
P1 N2 1.6844(12) . ?
P1 C34 1.8390(13) . ?
N1 H1 0.838(16) . ?
N1 C1 1.4266(16) . ?
N2 C13 1.2944(18) . ?
N4 C13 1.3815(18) . ?
N4 C25 1.4336(19) . ?
N4 C15 1.390(2) . ?
N3 C13 1.3853(18) . ?
N3 C16 1.4370(19) . ?
N3 C14 1.395(2) . ?
C1 C2 1.4123(18) . ?
C1 C6 1.4172(19) . ?
C34 C35 1.3929(19) . ?
C34 C39 1.392(2) . ?
C2 C7 1.5182(19) . ?
C2 C3 1.3961(19) . ?
C7 H7 0.9800 . ?
C7 C8 1.526(2) . ?
C7 C9 1.529(2) . ?
C6 C5 1.390(2) . ?
C6 C10 1.529(2) . ?
C16 C21 1.394(2) . ?
C16 C17 1.400(2) . ?
C21 C20 1.385(2) . ?
C21 C24 1.508(2) . ?
C25 C30 1.399(2) . ?
C25 C26 1.392(2) . ?
C35 H35 0.9300 . ?
C35 C36 1.389(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(2) . ?
C17 C18 1.389(2) . ?
C17 C22 1.505(2) . ?
C20 H20 0.9300 . ?
C20 C19 1.391(2) . ?
C39 H39 0.9300 . ?
C39 C38 1.389(2) . ?
C18 H18 0.9300 . ?
C18 C19 1.388(2) . ?
C19 C23 1.508(2) . ?
C30 C29 1.388(2) . ?
C30 C33 1.499(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.380(2) . ?
C5 H5 0.9300 . ?
C26 C27 1.385(2) . ?
C26 C31 1.515(2) . ?
C27 H27 0.9300 . ?
C27 C28 1.383(3) . ?
C29 H29 0.9300 . ?
C29 C28 1.389(3) . ?
C10 H10 0.9800 . ?
C10 C11 1.540(2) . ?
C10 C12 1.496(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.372(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C28 C32 1.515(2) . ?
C37 H37 0.9300 . ?
C37 C38 1.380(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C38 H38 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C14 H14 0.9300 . ?
C14 C15 1.329(3) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C15 H15 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
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
P1 N1 C1 C2 -67.29(15) . . . . ?
P1 N1 C1 C6 115.23(12) . . . . ?
P1 N2 C13 N4 -148.51(13) . . . . ?
P1 N2 C13 N3 33.5(2) . . . . ?
P1 C34 C35 C36 179.30(13) . . . . ?
P1 C34 C39 C38 -179.57(13) . . . . ?
N1 P1 N2 C13 155.90(11) . . . . ?
N1 P1 C34 C35 -103.83(12) . . . . ?
N1 P1 C34 C39 75.48(13) . . . . ?
N1 C1 C2 C7 -2.18(19) . . . . ?
N1 C1 C2 C3 179.00(12) . . . . ?
N1 C1 C6 C5 -179.28(13) . . . . ?
N1 C1 C6 C10 1.2(2) . . . . ?
N2 P1 N1 C1 -64.94(11) . . . . ?
N2 P1 C34 C35 152.03(11) . . . . ?
N2 P1 C34 C39 -28.66(13) . . . . ?
N4 C25 C30 C29 170.85(13) . . . . ?
N4 C25 C30 C33 -7.8(2) . . . . ?
N4 C25 C26 C27 -169.85(14) . . . . ?
N4 C25 C26 C31 10.4(2) . . . . ?
N3 C16 C21 C20 -178.73(13) . . . . ?
N3 C16 C21 C24 0.5(2) . . . . ?
N3 C16 C17 C18 177.86(13) . . . . ?
N3 C16 C17 C22 -1.7(2) . . . . ?
N3 C14 C15 N4 -0.2(3) . . . . ?
C1 C2 C7 C8 110.82(15) . . . . ?
C1 C2 C7 C9 -125.02(15) . . . . ?
C1 C2 C3 C4 1.2(2) . . . . ?
C1 C6 C5 C4 -0.6(2) . . . . ?
C1 C6 C10 C11 137.18(16) . . . . ?
C1 C6 C10 C12 -98.5(2) . . . . ?
C34 P1 N1 C1 -170.18(11) . . . . ?
C34 P1 N2 C13 -107.51(12) . . . . ?
C34 C35 C36 C37 0.4(3) . . . . ?
C34 C39 C38 C37 0.2(3) . . . . ?
C2 C1 C6 C5 3.3(2) . . . . ?
C2 C1 C6 C10 -176.30(14) . . . . ?
C2 C3 C4 C5 1.4(2) . . . . ?
C13 N4 C25 C30 73.7(2) . . . . ?
C13 N4 C25 C26 -112.69(18) . . . . ?
C13 N4 C15 C14 -0.1(2) . . . . ?
C13 N3 C16 C21 -109.62(18) . . . . ?
C13 N3 C16 C17 74.0(2) . . . . ?
C13 N3 C14 C15 0.3(2) . . . . ?
C7 C2 C3 C4 -177.66(14) . . . . ?
C6 C1 C2 C7 175.29(12) . . . . ?
C6 C1 C2 C3 -3.53(19) . . . . ?
C16 N3 C13 N2 12.0(3) . . . . ?
C16 N3 C13 N4 -166.29(15) . . . . ?
C16 N3 C14 C15 166.72(18) . . . . ?
C16 C21 C20 C19 2.2(2) . . . . ?
C16 C17 C18 C19 -0.4(2) . . . . ?
C21 C16 C17 C18 1.6(2) . . . . ?
C21 C16 C17 C22 -177.96(15) . . . . ?
C21 C20 C19 C18 -1.1(2) . . . . ?
C21 C20 C19 C23 177.99(15) . . . . ?
C25 N4 C13 N2 8.2(3) . . . . ?
C25 N4 C13 N3 -173.45(15) . . . . ?
C25 N4 C15 C14 174.03(18) . . . . ?
C25 C30 C29 C28 -1.1(2) . . . . ?
C25 C26 C27 C28 -1.1(3) . . . . ?
C35 C34 C39 C38 -0.3(2) . . . . ?
C35 C36 C37 C38 -0.5(3) . . . . ?
C3 C2 C7 C8 -70.37(17) . . . . ?
C3 C2 C7 C9 53.79(18) . . . . ?
C3 C4 C5 C6 -1.7(3) . . . . ?
C17 C16 C21 C20 -2.5(2) . . . . ?
C17 C16 C21 C24 176.73(14) . . . . ?
C17 C18 C19 C20 0.2(2) . . . . ?
C17 C18 C19 C23 -178.94(16) . . . . ?
C39 C34 C35 C36 0.0(2) . . . . ?
C30 C25 C26 C27 3.6(2) . . . . ?
C30 C25 C26 C31 -176.17(16) . . . . ?
C30 C29 C28 C27 3.5(3) . . . . ?
C30 C29 C28 C32 -174.83(17) . . . . ?
C5 C6 C10 C11 -42.4(2) . . . . ?
C5 C6 C10 C12 82.0(2) . . . . ?
C26 C25 C30 C29 -2.5(2) . . . . ?
C26 C25 C30 C33 178.89(15) . . . . ?
C26 C27 C28 C29 -2.3(3) . . . . ?
C26 C27 C28 C32 175.97(17) . . . . ?
C10 C6 C5 C4 178.94(16) . . . . ?
C36 C37 C38 C39 0.2(3) . . . . ?
C33 C30 C29 C28 177.50(16) . . . . ?
C22 C17 C18 C19 179.13(15) . . . . ?
C14 N3 C13 N2 177.88(17) . . . . ?
C14 N3 C13 N4 -0.38(19) . . . . ?
C14 N3 C16 C21 86.2(2) . . . . ?
C14 N3 C16 C17 -90.2(2) . . . . ?
C24 C21 C20 C19 -176.95(15) . . . . ?
C15 N4 C13 N2 -178.11(16) . . . . ?
C15 N4 C13 N3 0.29(19) . . . . ?
C15 N4 C25 C30 -99.3(2) . . . . ?
C15 N4 C25 C26 74.3(2) . . . . ?
C31 C26 C27 C28 178.67(18) . . . . ?
