#------------------------------------------------------------------------------
#$Date: 2025-03-04 22:09:08 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298249 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/74/7717449.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_7717449
loop_
_publ_author_name
'Wang, Wenlong'
'Li, Cunyao'
'Wang, Wenhao'
'Qiu, Yuqin'
'Liu, Hongguang'
'Lu, Jinlong'
'Zhan, Yizhou'
'Yan, Li'
'Ding, Yunjie'
_publ_section_title
;
 Modular synthesis of triphenylphosphine-derived cage ligands for
 rhodium-catalyzed hydroformylation applications.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              207
_journal_page_last               214
_journal_paper_doi               10.1039/d4dt02627f
_journal_volume                  54
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C66 H72 N6 P2'
_chemical_formula_sum            'C66 H72 N6 P2'
_chemical_formula_weight         1011.23
_space_group_crystal_system      tetragonal
_space_group_IT_number           91
_space_group_name_Hall           'P 4w 2c'
_space_group_name_H-M_alt        'P 41 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-15 deposited with the CCDC.	2024-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1786(5)
_cell_length_b                   17.1786(5)
_cell_length_c                   24.7552(6)
_cell_measurement_reflns_used    7894
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.4280
_cell_measurement_theta_min      2.5300
_cell_volume                     7305.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  33.00   1.00    2.00    --  -40.98  38.00  60.00   99
  2  ω     -7.00  47.00   1.00    2.00    --   40.98 -38.00 150.00   54
  3  ω     35.00 106.00   1.00    3.00    --  106.95 -95.00  60.00   71
  4  ω     51.00 109.00   1.00    3.00    --  106.95 -95.00 150.00   58
  5  ω     30.00  62.00   1.00    2.00    --   40.98-125.00 -30.00   32
  6  ω     27.00 103.00   1.00    3.00    --  106.95 -95.00 -30.00   76
  7  ω     25.00  73.00   1.00    2.00    --   40.98-125.00-180.00   48
  8  ω     85.00 175.00   1.00    3.00    --  106.95  45.00-180.00   90
  9  ω     99.00 162.00   1.00    3.00    --  106.95 125.00   0.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0812406000
_diffrn_orient_matrix_UB_12      -0.0097605000
_diffrn_orient_matrix_UB_13      0.0255709000
_diffrn_orient_matrix_UB_21      -0.0085280000
_diffrn_orient_matrix_UB_22      0.0892333000
_diffrn_orient_matrix_UB_23      0.0031969000
_diffrn_orient_matrix_UB_31      -0.0370879000
_diffrn_orient_matrix_UB_32      0.0006127000
_diffrn_orient_matrix_UB_33      -0.0565531000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25027
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.759
_diffrn_reflns_theta_min         2.572
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.919
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 1968 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1116P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.1946
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                5907
_reflns_number_total             7230
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02627f2.cif
_cod_data_source_block           8-2
_cod_depositor_comments
'Adding full bibliography for 7717449--7717451.cif.'
_cod_original_cell_volume        7305.3(4)
_cod_database_code               7717449
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C32(H32A,H32B), C33(H33A,
 H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C13(H13), C15(H15), C17(H17), C20(H20), C21(H21),
 C25(H25), C27(H27), C28(H28), C30(H30)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2020-08-05
_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 1.924
_oxdiff_exptl_absorpt_empirical_full_min 0.446
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'
'-x, y, -z'
'x, -y, -z+1/2'
'y, x, -z+3/4'
'-y, -x, -z+1/4'
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 0.45460(7) 0.18479(6) 0.28794(4) 0.0407(3) Uani 1 1 d . . . . .
N1 N 0.2601(3) 0.1128(2) 0.59646(15) 0.0644(13) Uani 1 1 d . . . . .
N2 N 0.3807(3) 0.0296(2) 0.53957(13) 0.0529(10) Uani 1 1 d . . . . .
N3 N 0.6246(2) 0.5417(2) 0.33330(12) 0.0392(7) Uani 1 1 d . . . . .
C1 C 0.3667(4) 0.0205(3) 0.59775(17) 0.0639(16) Uani 1 1 d . . . . .
H1 H 0.396621 0.059762 0.617547 0.077 Uiso 1 1 calc R U . . .
C2 C 0.3935(4) -0.0605(3) 0.61491(18) 0.0665(16) Uani 1 1 d . . . . .
H2A H 0.368881 -0.099144 0.592018 0.080 Uiso 1 1 calc R U . . .
H2B H 0.449335 -0.064579 0.610046 0.080 Uiso 1 1 calc R U . . .
C3 C 0.3733(5) -0.0771(4) 0.6737(2) 0.088(2) Uani 1 1 d . . . . .
H3A H 0.387179 -0.130381 0.682356 0.105 Uiso 1 1 calc R U . . .
H3B H 0.403212 -0.042912 0.696933 0.105 Uiso 1 1 calc R U . . .
C4 C 0.2879(6) -0.0651(4) 0.6841(2) 0.099(3) Uani 1 1 d . . . . .
H4A H 0.277401 -0.073441 0.722179 0.119 Uiso 1 1 calc R U . . .
H4B H 0.258367 -0.103181 0.663752 0.119 Uiso 1 1 calc R U . . .
C5 C 0.2611(5) 0.0167(3) 0.6683(2) 0.095(3) Uani 1 1 d . . . . .
H5A H 0.286420 0.055021 0.691094 0.113 Uiso 1 1 calc R U . . .
H5B H 0.205290 0.021273 0.673384 0.113 Uiso 1 1 calc R U . . .
C6 C 0.2818(4) 0.0321(3) 0.60863(17) 0.0643(16) Uani 1 1 d . . . . .
H6 H 0.251523 -0.003143 0.585606 0.077 Uiso 1 1 calc R U . . .
C7 C 0.2320(3) 0.1260(3) 0.55030(17) 0.0564(12) Uani 1 1 d . . . . .
H7 H 0.220421 0.083856 0.528089 0.068 Uiso 1 1 calc R U . . .
C8 C 0.2166(3) 0.2049(3) 0.53005(17) 0.0525(12) Uani 1 1 d . . . . .
C9 C 0.1994(3) 0.2149(3) 0.47600(17) 0.0542(12) Uani 1 1 d . . . . .
H9 H 0.194657 0.171736 0.453535 0.065 Uiso 1 1 calc R U . . .
C10 C 0.1892(3) 0.2901(3) 0.45490(17) 0.0531(12) Uani 1 1 d . . . . .
H10 H 0.177541 0.296640 0.418498 0.064 Uiso 1 1 calc R U . . .
C11 C 0.1964(3) 0.3548(3) 0.48842(15) 0.0422(10) Uani 1 1 d . . . . .
C12 C 0.2137(3) 0.3455(3) 0.54308(14) 0.0405(9) Uani 1 1 d . . . . .
C13 C 0.2238(3) 0.2702(3) 0.56318(15) 0.0465(11) Uani 1 1 d . . . . .
H13 H 0.235723 0.263400 0.599529 0.056 Uiso 1 1 calc R U . . .
C14 C 0.2235(3) 0.4137(3) 0.58041(15) 0.0466(10) Uani 1 1 d . . . . .
H14A H 0.273528 0.437046 0.574510 0.070 Uiso 1 1 calc R U . . .
H14B H 0.219816 0.396267 0.617174 0.070 Uiso 1 1 calc R U . . .
H14C H 0.183398 0.451256 0.573407 0.070 Uiso 1 1 calc R U . . .
C15 C 0.4010(3) 0.0978(3) 0.52459(17) 0.0527(12) Uani 1 1 d . . . . .
H15 H 0.409644 0.135925 0.550578 0.063 Uiso 1 1 calc R U . . .
C16 C 0.4110(3) 0.1174(3) 0.46726(15) 0.0443(10) Uani 1 1 d . . . . .
C17 C 0.4091(3) 0.0622(3) 0.42631(15) 0.0491(11) Uani 1 1 d . . . . .
H17 H 0.399516 0.010532 0.435294 0.059 Uiso 1 1 calc R U . . .
C18 C 0.4210(3) 0.0816(3) 0.37181(16) 0.0477(11) Uani 1 1 d . . . . .
C19 C 0.4361(3) 0.1598(3) 0.35897(14) 0.0408(9) Uani 1 1 d . . . . .
C20 C 0.4370(3) 0.2152(3) 0.40016(14) 0.0406(9) Uani 1 1 d . . . . .
H20 H 0.446147 0.267149 0.391547 0.049 Uiso 1 1 calc R U . . .
C21 C 0.4248(3) 0.1949(3) 0.45310(15) 0.0449(10) Uani 1 1 d . . . . .
H21 H 0.425747 0.233030 0.479767 0.054 Uiso 1 1 calc R U . . .
C22 C 0.4157(4) 0.0193(3) 0.32943(19) 0.0633(15) Uani 1 1 d . . . . .
H22A H 0.372676 0.030161 0.305853 0.095 Uiso 1 1 calc R U . . .
H22B H 0.407994 -0.030257 0.346496 0.095 Uiso 1 1 calc R U . . .
H22C H 0.463050 0.018248 0.308844 0.095 Uiso 1 1 calc R U . . .
C23 C 0.4848(3) 0.2867(2) 0.29491(14) 0.0374(9) Uani 1 1 d . . . . .
C24 C 0.5644(2) 0.3037(2) 0.30243(13) 0.0370(9) Uani 1 1 d . . . . .
C25 C 0.5868(2) 0.3809(3) 0.30967(13) 0.0372(9) Uani 1 1 d . . . . .
H25 H 0.639244 0.392150 0.314927 0.045 Uiso 1 1 calc R U . . .
C26 C 0.5336(2) 0.4417(2) 0.30929(12) 0.0330(8) Uani 1 1 d . . . . .
C27 C 0.4543(2) 0.4247(2) 0.30068(13) 0.0351(8) Uani 1 1 d . . . . .
H27 H 0.417838 0.464590 0.299509 0.042 Uiso 1 1 calc R U . . .
C28 C 0.4312(2) 0.3481(2) 0.29399(15) 0.0388(9) Uani 1 1 d . . . . .
H28 H 0.378734 0.337163 0.288745 0.047 Uiso 1 1 calc R U . . .
C29 C 0.6252(3) 0.2405(3) 0.30457(18) 0.0497(11) Uani 1 1 d . . . . .
H29A H 0.676006 0.263307 0.301321 0.074 Uiso 1 1 calc R U . . .
H29B H 0.616939 0.204632 0.275390 0.074 Uiso 1 1 calc R U . . .
H29C H 0.621386 0.213340 0.338353 0.074 Uiso 1 1 calc R U . . .
C30 C 0.5564(2) 0.5228(2) 0.31753(14) 0.0372(9) Uani 1 1 d . . . . .
H30 H 0.520093 0.561841 0.311082 0.045 Uiso 1 1 calc R U . . .
C31 C 0.6386(3) 0.6232(3) 0.34458(15) 0.0406(9) Uani 1 1 d . . . . .
H31 H 0.603015 0.655010 0.322888 0.049 Uiso 1 1 calc R U . . .
C32 C 0.7223(3) 0.6440(3) 0.33033(17) 0.0472(10) Uani 1 1 d . . . . .
H32A H 0.757339 0.609124 0.349228 0.057 Uiso 1 1 calc R U . . .
H32B H 0.730181 0.636771 0.291861 0.057 Uiso 1 1 calc R U . . .
C33 C 0.7419(3) 0.7272(3) 0.34516(19) 0.0537(12) Uani 1 1 d . . . . .
H33A H 0.710357 0.762499 0.323800 0.064 Uiso 1 1 calc R U . . .
H33B H 0.796171 0.737398 0.336952 0.064 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
C19 P1 C11 101.71(19) . 7 ?
C23 P1 C11 101.11(19) . 7 ?
C23 P1 C19 100.47(18) . . ?
C7 N1 C6 116.9(4) . . ?
C15 N2 C1 115.3(4) . . ?
C30 N3 C31 117.2(4) . . ?
N2 C1 H1 109.3 . . ?
N2 C1 C2 108.7(4) . . ?
N2 C1 C6 108.8(4) . . ?
C2 C1 H1 109.3 . . ?
C6 C1 H1 109.3 . . ?
C6 C1 C2 111.4(4) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C3 C2 C1 111.6(5) . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
C2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 C2 111.1(5) . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
C3 C4 C5 112.1(6) . . ?
H4A C4 H4B 107.9 . . ?
C5 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
C4 C5 H5A 109.8 . . ?
C4 C5 H5B 109.8 . . ?
C4 C5 C6 109.5(5) . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
N1 C6 C1 109.6(4) . . ?
N1 C6 C5 107.5(4) . . ?
N1 C6 H6 109.2 . . ?
C1 C6 C5 112.0(5) . . ?
C1 C6 H6 109.2 . . ?
C5 C6 H6 109.2 . . ?
N1 C7 H7 118.5 . . ?
N1 C7 C8 122.9(5) . . ?
C8 C7 H7 118.5 . . ?
C9 C8 C7 118.9(4) . . ?
C9 C8 C13 119.3(5) . . ?
C13 C8 C7 121.7(4) . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.1(4) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 P1 121.4(3) . 7 ?
C10 C11 C12 120.3(4) . . ?
C12 C11 P1 118.3(3) . 7 ?
C11 C12 C13 118.6(4) . . ?
C11 C12 C14 122.1(4) . . ?
C13 C12 C14 119.3(3) . . ?
C8 C13 H13 119.2 . . ?
C12 C13 C8 121.6(4) . . ?
C12 C13 H13 119.2 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 H15 119.2 . . ?
N2 C15 C16 121.5(4) . . ?
C16 C15 H15 119.2 . . ?
C17 C16 C15 123.1(4) . . ?
C17 C16 C21 118.1(4) . . ?
C21 C16 C15 118.7(4) . . ?
C16 C17 H17 118.8 . . ?
C16 C17 C18 122.4(4) . . ?
C18 C17 H17 118.8 . . ?
C17 C18 C19 118.1(4) . . ?
C17 C18 C22 119.5(4) . . ?
C19 C18 C22 122.3(4) . . ?
C18 C19 P1 118.1(3) . . ?
C20 C19 P1 122.6(3) . . ?
C20 C19 C18 119.3(4) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.5(4) . . ?
C21 C20 H20 119.3 . . ?
C16 C21 H21 119.7 . . ?
C20 C21 C16 120.5(4) . . ?
C20 C21 H21 119.7 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P1 119.0(3) . . ?
C28 C23 P1 122.1(3) . . ?
C28 C23 C24 118.9(4) . . ?
C23 C24 C29 121.8(4) . . ?
C25 C24 C23 118.8(4) . . ?
C25 C24 C29 119.3(4) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 C24 122.2(4) . . ?
C26 C25 H25 118.9 . . ?
C25 C26 C27 118.8(4) . . ?
C25 C26 C30 122.7(4) . . ?
C27 C26 C30 118.5(4) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 C26 119.5(4) . . ?
C28 C27 H27 120.2 . . ?
C23 C28 H28 119.2 . . ?
C27 C28 C23 121.7(4) . . ?
C27 C28 H28 119.2 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C26 122.1(4) . . ?
N3 C30 H30 119.0 . . ?
C26 C30 H30 119.0 . . ?
N3 C31 C31 108.9(3) . 7 ?
N3 C31 H31 109.3 . . ?
N3 C31 C32 109.8(4) . . ?
C31 C31 H31 109.3 7 . ?
C32 C31 C31 110.2(3) . 7 ?
C32 C31 H31 109.3 . . ?
C31 C32 H32A 109.2 . . ?
C31 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 C31 112.1(4) . . ?
C33 C32 H32A 109.2 . . ?
C33 C32 H32B 109.2 . . ?
C32 C33 C33 110.8(3) . 7 ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C33 C33 H33A 109.5 7 . ?
C33 C33 H33B 109.5 7 . ?
H33A C33 H33B 108.1 . . ?
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 C11 1.845(5) 7 ?
P1 C19 1.837(4) . ?
P1 C23 1.834(4) . ?
N1 C6 1.467(7) . ?
N1 C7 1.261(6) . ?
N2 C1 1.469(5) . ?
N2 C15 1.277(6) . ?
N3 C30 1.277(5) . ?
N3 C31 1.447(6) . ?
C1 H1 0.9800 . ?
C1 C2 1.525(7) . ?
C1 C6 1.497(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.523(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.502(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.530(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.542(6) . ?
C6 H6 0.9800 . ?
C7 H7 0.9300 . ?
C7 C8 1.470(7) . ?
C8 C9 1.381(6) . ?
C8 C13 1.395(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.404(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.393(6) . ?
C11 C12 1.395(5) . ?
C12 C13 1.397(6) . ?
C12 C14 1.502(6) . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15 0.9300 . ?
C15 C16 1.469(5) . ?
C16 C17 1.388(6) . ?
C16 C21 1.397(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.405(6) . ?
C18 C19 1.405(6) . ?
C18 C22 1.501(6) . ?
C19 C20 1.395(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.373(5) . ?
C21 H21 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.410(6) . ?
C23 C28 1.400(6) . ?
C24 C25 1.393(6) . ?
C24 C29 1.508(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.387(6) . ?
C26 C27 1.409(6) . ?
C26 C30 1.462(6) . ?
C27 H27 0.9300 . ?
C27 C28 1.384(6) . ?
C28 H28 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30 0.9300 . ?
C31 C31 1.552(7) 7 ?
C31 H31 0.9800 . ?
C31 C32 1.524(6) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.513(7) . ?
C33 C33 1.520(9) 7 ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
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 C11 C12 C13 -179.0(3) 7 . . . ?
P1 C11 C12 C14 -0.5(6) 7 . . . ?
P1 C19 C20 C21 -178.5(4) . . . . ?
P1 C23 C24 C25 -177.7(3) . . . . ?
P1 C23 C24 C29 0.4(5) . . . . ?
P1 C23 C28 C27 178.3(3) . . . . ?
N1 C7 C8 C9 168.2(5) . . . . ?
N1 C7 C8 C13 -7.5(8) . . . . ?
N2 C1 C2 C3 -174.3(5) . . . . ?
N2 C1 C6 N1 -65.5(5) . . . . ?
N2 C1 C6 C5 175.3(4) . . . . ?
N2 C15 C16 C17 -8.4(8) . . . . ?
N2 C15 C16 C21 173.0(5) . . . . ?
N3 C31 C32 C33 -175.8(4) . . . . ?
C1 N2 C15 C16 -175.0(5) . . . . ?
C1 C2 C3 C4 54.4(7) . . . . ?
C2 C1 C6 N1 174.6(4) . . . . ?
C2 C1 C6 C5 55.4(6) . . . . ?
C2 C3 C4 C5 -55.9(7) . . . . ?
C3 C4 C5 C6 55.8(8) . . . . ?
C4 C5 C6 N1 -176.0(7) . . . . ?
C4 C5 C6 C1 -55.6(8) . . . . ?
C6 N1 C7 C8 -172.3(5) . . . . ?
C6 C1 C2 C3 -54.4(6) . . . . ?
C7 N1 C6 C1 95.6(6) . . . . ?
C7 N1 C6 C5 -142.5(6) . . . . ?
C7 C8 C9 C10 -176.1(5) . . . . ?
C7 C8 C13 C12 176.1(5) . . . . ?
C8 C9 C10 C11 0.1(8) . . . . ?
C9 C8 C13 C12 0.4(8) . . . . ?
C9 C10 C11 P1 179.1(4) . . . 7 ?
C9 C10 C11 C12 -0.2(7) . . . . ?
C10 C11 C12 C13 0.3(7) . . . . ?
C10 C11 C12 C14 178.8(4) . . . . ?
C11 P1 C19 C18 84.5(4) 7 . . . ?
C11 P1 C19 C20 -96.0(4) 7 . . . ?
C11 P1 C23 C24 -165.6(3) 7 . . . ?
C11 P1 C23 C28 15.6(4) 7 . . . ?
C11 C12 C13 C8 -0.5(7) . . . . ?
C13 C8 C9 C10 -0.3(8) . . . . ?
C14 C12 C13 C8 -179.0(4) . . . . ?
C15 N2 C1 C2 -144.6(5) . . . . ?
C15 N2 C1 C6 93.9(5) . . . . ?
C15 C16 C17 C18 -178.1(5) . . . . ?
C15 C16 C21 C20 177.8(5) . . . . ?
C16 C17 C18 C19 0.6(8) . . . . ?
C16 C17 C18 C22 -178.2(5) . . . . ?
C17 C16 C21 C20 -0.8(7) . . . . ?
C17 C18 C19 P1 178.2(4) . . . . ?
C17 C18 C19 C20 -1.3(7) . . . . ?
C18 C19 C20 C21 1.1(7) . . . . ?
C19 P1 C23 C24 90.1(3) . . . . ?
C19 P1 C23 C28 -88.7(3) . . . . ?
C19 C20 C21 C16 0.0(7) . . . . ?
C21 C16 C17 C18 0.5(8) . . . . ?
C22 C18 C19 P1 -3.1(7) . . . . ?
C22 C18 C19 C20 177.4(5) . . . . ?
C23 P1 C19 C18 -171.7(4) . . . . ?
C23 P1 C19 C20 7.8(4) . . . . ?
C23 C24 C25 C26 -0.5(5) . . . . ?
C24 C23 C28 C27 -0.5(6) . . . . ?
C24 C25 C26 C27 -0.7(5) . . . . ?
C24 C25 C26 C30 179.2(3) . . . . ?
C25 C26 C27 C28 1.4(5) . . . . ?
C25 C26 C30 N3 -10.4(5) . . . . ?
C26 C27 C28 C23 -0.8(5) . . . . ?
C27 C26 C30 N3 169.6(3) . . . . ?
C28 C23 C24 C25 1.1(5) . . . . ?
C28 C23 C24 C29 179.2(4) . . . . ?
C29 C24 C25 C26 -178.6(3) . . . . ?
C30 N3 C31 C31 92.4(5) . . . 7 ?
C30 N3 C31 C32 -146.8(3) . . . . ?
C30 C26 C27 C28 -178.6(3) . . . . ?
C31 N3 C30 C26 -174.8(3) . . . . ?
C31 C31 C32 C33 -55.8(5) 7 . . . ?
C31 C32 C33 C33 56.6(6) . . . 7 ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.989 -0.504 -0.083 2181.2 491.4 ?
2 0.328 0.405 0.183 24.5 0.0 ?
3 0.328 0.595 0.317 24.5 0.0 ?
4 0.405 0.328 0.567 24.5 0.0 ?
5 0.405 0.672 0.933 24.5 0.0 ?
6 0.595 0.328 0.433 24.5 0.0 ?
7 0.595 0.672 0.067 24.5 0.0 ?
8 0.672 0.405 0.817 24.5 0.0 ?
9 0.672 0.595 0.683 24.5 0.0 ?
