#------------------------------------------------------------------------------
#$Date: 2021-11-06 19:46:11 +0100 (Sat 06 de Nov de 2021) $
#$Revision: 270353 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/90/7129032.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_7129032
loop_
_publ_author_name
'Frenette, Brandon L.'
'Omaña, Alvaro A'
'Ferguson, Michael J.'
'Zhou, Yuqiao'
'Rivard, Eric'
_publ_section_title
;
 Access to adducts of parent iminoborane isomers, HBNH and
 NBH₂, using frustrated Lewis pair chelation.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10895
_journal_page_last               10898
_journal_paper_doi               10.1039/d1cc04923b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C H2 Cl2, C31 H52 B2 N3 P'
_chemical_formula_sum            'C32 H54 B2 Cl2 N3 P'
_chemical_formula_weight         604.27
_chemical_name_common            PB(NBH2)-DMAP
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2021-09-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                98.954(2)
_cell_angle_beta                 98.334(2)
_cell_angle_gamma                99.920(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5926(12)
_cell_length_b                   11.0351(14)
_cell_length_c                   16.641(2)
_cell_measurement_reflns_used    4652
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      22.64
_cell_measurement_theta_min      2.19
_cell_volume                     1687.1(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30383
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.179
_diffrn_reflns_theta_min         1.259
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9132
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,  J. Appl. Cryst. 48 (2015) 3-10'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       fragment
_exptl_crystal_F_000             652
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes/DCM at -40C'
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0430
_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)+(0.0477P)²+0.3880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5428
_reflns_number_total             7484
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc04923b2.cif
_cod_data_source_block           PB(NBH2)-DMAP
_cod_depositor_comments
'Adding full bibliography for 7129027--7129035.cif.'
_cod_database_code               7129032
_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.
;
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.952
_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. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(C32B)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C19(H19)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C32A(H32A,H32B), C32B(H32C,H32D)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C25(H25), C26(H26), C28(H28), C29(H29)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_olex2_date_sample_data_collection 2021-07-20
_olex2_date_sample_submission    2021-07-20
_olex2_exptl_crystal_mounting_method
'A suitable crystal was coated in Paratone oil and mounted on a loop.'
_olex2_submission_original_sample_id riv21a1
_olex2_submission_special_instructions 'No special instructions were received'
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
Cl1A Cl 0.1433(5) 0.1303(4) 0.4020(2) 0.0590(8) Uani 0.609(18) 1 d . . P A 1
Cl1B Cl 0.1375(8) 0.1621(14) 0.4064(5) 0.0883(18) Uani 0.391(18) 1 d . . P A 2
Cl2A Cl 0.4182(5) 0.2819(8) 0.3908(4) 0.0837(14) Uani 0.609(18) 1 d . . P A 1
Cl2B Cl 0.4147(9) 0.2534(10) 0.3778(6) 0.0854(19) Uani 0.391(18) 1 d . . P A 2
P1 P 0.48041(5) 0.39556(4) 0.79019(3) 0.02173(11) Uani 1 1 d . . . . .
N1 N 0.64543(14) 0.37888(12) 0.80133(8) 0.0211(3) Uani 1 1 d . . . . .
N2 N 0.87373(14) 0.56000(12) 0.86036(8) 0.0231(3) Uani 1 1 d . . . . .
N3 N 1.21034(16) 0.83834(14) 0.83415(9) 0.0325(4) Uani 1 1 d . . . . .
C1 C 0.39719(17) 0.25821(15) 0.71485(10) 0.0220(3) Uani 1 1 d . . . . .
C2 C 0.50453(17) 0.19438(15) 0.69300(9) 0.0219(3) Uani 1 1 d . . . . .
C3 C 0.45749(19) 0.08113(16) 0.63670(10) 0.0275(4) Uani 1 1 d . . . . .
H3 H 0.526220 0.034154 0.620426 0.033 Uiso 1 1 calc R U . . .
C4 C 0.3129(2) 0.03587(16) 0.60412(10) 0.0309(4) Uani 1 1 d . . . . .
H4 H 0.284253 -0.041565 0.566348 0.037 Uiso 1 1 calc R U . . .
C5 C 0.20968(19) 0.10240(17) 0.62607(11) 0.0317(4) Uani 1 1 d . . . . .
H5 H 0.111058 0.071303 0.602917 0.038 Uiso 1 1 calc R U . . .
C6 C 0.25118(18) 0.21394(17) 0.68173(10) 0.0281(4) Uani 1 1 d . . . . .
H6 H 0.181522 0.260246 0.697418 0.034 Uiso 1 1 calc R U . . .
C7 C 0.40306(18) 0.39870(16) 0.88490(10) 0.0275(4) Uani 1 1 d . . . . .
H7 H 0.454449 0.477274 0.923845 0.033 Uiso 1 1 calc R U . . .
C8 C 0.4321(2) 0.29028(19) 0.92624(12) 0.0417(5) Uani 1 1 d . . . . .
H8A H 0.387950 0.211113 0.888586 0.063 Uiso 1 1 calc R U . . .
H8B H 0.390992 0.294092 0.976957 0.063 Uiso 1 1 calc R U . . .
H8C H 0.536077 0.295543 0.939922 0.063 Uiso 1 1 calc R U . . .
C9 C 0.2430(2) 0.4030(2) 0.87204(12) 0.0433(5) Uani 1 1 d . . . . .
H9A H 0.227437 0.474800 0.846365 0.065 Uiso 1 1 calc R U . . .
H9B H 0.210888 0.411369 0.925552 0.065 Uiso 1 1 calc R U . . .
H9C H 0.188243 0.325606 0.835974 0.065 Uiso 1 1 calc R U . . .
C10 C 0.4512(2) 0.53752(16) 0.75021(11) 0.0298(4) Uani 1 1 d . . . . .
H10 H 0.524830 0.552038 0.714107 0.036 Uiso 1 1 calc R U . . .
C11 C 0.3069(2) 0.52788(19) 0.69417(13) 0.0423(5) Uani 1 1 d . . . . .
H11A H 0.292501 0.457058 0.648238 0.063 Uiso 1 1 calc R U . . .
H11B H 0.306643 0.605367 0.672323 0.063 Uiso 1 1 calc R U . . .
H11C H 0.229057 0.515051 0.726045 0.063 Uiso 1 1 calc R U . . .
C12 C 0.4858(2) 0.65481(17) 0.81800(13) 0.0450(5) Uani 1 1 d . . . . .
H12A H 0.413710 0.649321 0.854085 0.067 Uiso 1 1 calc R U . . .
H12B H 0.484739 0.729135 0.792638 0.067 Uiso 1 1 calc R U . . .
H12C H 0.581271 0.661003 0.850642 0.067 Uiso 1 1 calc R U . . .
C13 C 0.74454(18) 0.15603(16) 0.77864(10) 0.0253(4) Uani 1 1 d . . . . .
H13 H 0.734917 0.084550 0.731839 0.030 Uiso 1 1 calc R U . . .
C14 C 0.90627(19) 0.19047(18) 0.81327(12) 0.0340(4) Uani 1 1 d . . . . .
H14A H 0.957484 0.227165 0.772470 0.041 Uiso 1 1 calc R U . . .
H14B H 0.923770 0.254598 0.864272 0.041 Uiso 1 1 calc R U . . .
C15 C 0.9665(2) 0.0769(2) 0.83279(13) 0.0428(5) Uani 1 1 d . . . . .
H15A H 0.956751 0.015771 0.781010 0.051 Uiso 1 1 calc R U . . .
H15B H 1.070115 0.103627 0.856597 0.051 Uiso 1 1 calc R U . . .
C16 C 0.8884(2) 0.0144(2) 0.89340(12) 0.0426(5) Uani 1 1 d . . . . .
H16A H 0.909729 0.071159 0.947820 0.051 Uiso 1 1 calc R U . . .
H16B H 0.923524 -0.063180 0.900648 0.051 Uiso 1 1 calc R U . . .
C17 C 0.7265(2) -0.01747(18) 0.86272(12) 0.0384(5) Uani 1 1 d . . . . .
H17A H 0.677790 -0.050239 0.905694 0.046 Uiso 1 1 calc R U . . .
H17B H 0.704170 -0.083811 0.812661 0.046 Uiso 1 1 calc R U . . .
C18 C 0.66922(19) 0.09755(16) 0.84236(11) 0.0284(4) Uani 1 1 d . . . . .
H18A H 0.564703 0.072808 0.820691 0.034 Uiso 1 1 calc R U . . .
H18B H 0.683427 0.160660 0.893631 0.034 Uiso 1 1 calc R U . . .
C19 C 0.76161(18) 0.31005(16) 0.66624(10) 0.0251(4) Uani 1 1 d . . . . .
H19 H 0.849947 0.370000 0.697688 0.030 Uiso 1 1 calc R U . . .
C20 C 0.68251(19) 0.38227(17) 0.60861(10) 0.0286(4) Uani 1 1 d . . . . .
H20A H 0.596016 0.324686 0.574837 0.034 Uiso 1 1 calc R U . . .
H20B H 0.649876 0.450084 0.642709 0.034 Uiso 1 1 calc R U . . .
C21 C 0.7742(2) 0.43938(18) 0.55090(12) 0.0367(4) Uani 1 1 d . . . . .
H21A H 0.715672 0.481497 0.514335 0.044 Uiso 1 1 calc R U . . .
H21B H 0.856072 0.503186 0.584050 0.044 Uiso 1 1 calc R U . . .
C22 C 0.8309(2) 0.3396(2) 0.49846(12) 0.0388(5) Uani 1 1 d . . . . .
H22A H 0.749875 0.283389 0.458896 0.047 Uiso 1 1 calc R U . . .
H22B H 0.898481 0.379974 0.466353 0.047 Uiso 1 1 calc R U . . .
C23 C 0.9074(2) 0.2631(2) 0.55238(12) 0.0394(5) Uani 1 1 d . . . . .
H23A H 0.996608 0.317003 0.585896 0.047 Uiso 1 1 calc R U . . .
H23B H 0.934797 0.193888 0.516615 0.047 Uiso 1 1 calc R U . . .
C24 C 0.8132(2) 0.20898(18) 0.60976(11) 0.0326(4) Uani 1 1 d . . . . .
H24A H 0.868141 0.161992 0.644482 0.039 Uiso 1 1 calc R U . . .
H24B H 0.728316 0.149208 0.576007 0.039 Uiso 1 1 calc R U . . .
C25 C 0.98155(18) 0.61579(15) 0.92360(10) 0.0256(4) Uani 1 1 d . . . . .
H25 H 0.979892 0.589585 0.975253 0.031 Uiso 1 1 calc R U . . .
C26 C 1.09253(18) 0.70733(16) 0.91789(11) 0.0272(4) Uani 1 1 d . . . . .
H26 H 1.165181 0.743072 0.964809 0.033 Uiso 1 1 calc R U . . .
C27 C 1.09996(18) 0.74929(15) 0.84245(11) 0.0253(4) Uani 1 1 d . . . . .
C28 C 0.98596(19) 0.69154(16) 0.77719(11) 0.0294(4) Uani 1 1 d . . . . .
H28 H 0.984010 0.715632 0.724726 0.035 Uiso 1 1 calc R U . . .
C29 C 0.87777(19) 0.60079(16) 0.78883(10) 0.0277(4) Uani 1 1 d . . . . .
H29 H 0.801557 0.564884 0.743768 0.033 Uiso 1 1 calc R U . . .
C30 C 1.3144(2) 0.90713(18) 0.90603(13) 0.0404(5) Uani 1 1 d . . . . .
H30A H 1.264545 0.949426 0.945943 0.061 Uiso 1 1 calc R U . . .
H30B H 1.384218 0.969483 0.888916 0.061 Uiso 1 1 calc R U . . .
H30C H 1.364634 0.848855 0.931678 0.061 Uiso 1 1 calc R U . . .
C31 C 1.2198(2) 0.87815(19) 0.75556(12) 0.0386(5) Uani 1 1 d . . . . .
H31A H 1.203105 0.804391 0.711527 0.058 Uiso 1 1 calc R U . . .
H31B H 1.315643 0.928495 0.758234 0.058 Uiso 1 1 calc R U . . .
H31C H 1.147015 0.928417 0.743896 0.058 Uiso 1 1 calc R U . . .
C32A C 0.3024(14) 0.2269(10) 0.4530(6) 0.060(3) Uani 0.609(18) 1 d . . P A 1
H32A H 0.352914 0.180719 0.490502 0.072 Uiso 0.609(18) 1 calc R U P A 1
H32B H 0.279462 0.299618 0.487765 0.072 Uiso 0.609(18) 1 calc R U P A 1
C32B C 0.312(2) 0.192(2) 0.4427(13) 0.091(6) Uani 0.391(18) 1 d . . P A 2
H32C H 0.341089 0.113075 0.453523 0.109 Uiso 0.391(18) 1 calc R U P A 2
H32D H 0.331823 0.250997 0.496124 0.109 Uiso 0.391(18) 1 calc R U P A 2
B1 B 0.6699(2) 0.25975(17) 0.73609(11) 0.0224(4) Uani 1 1 d . . . . .
B2 B 0.7474(2) 0.45389(19) 0.87895(12) 0.0257(4) Uani 1 1 d . . . . .
H2A H 0.8063(18) 0.3949(15) 0.9156(10) 0.024(4) Uiso 1 1 d . . . . .
H2B H 0.6903(18) 0.5107(15) 0.9211(10) 0.023(4) Uiso 1 1 d . . . . .
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 -1.00 0.0710
0.00 -1.00 0.00 0.0430
0.00 1.00 0.00 0.0310
0.00 0.00 -1.00 0.0810
0.00 0.00 1.00 0.0720
0.00 1.00 -1.00 0.0590
0.00 -1.00 1.00 0.0480
-1.00 -1.00 0.00 0.0520
1.00 -1.00 1.00 0.0880
-1.00 1.00 -1.00 0.0920
1.00 -1.00 0.00 0.0780
-1.00 1.00 0.00 0.0770
-1.00 -1.00 1.00 0.0670
1.00 1.00 -1.00 0.0670
1.00 -1.00 -1.00 0.0680
-1.00 2.00 2.00 0.0680
-1.00 0.00 2.00 0.0940
-1.00 -2.00 2.00 0.0590
-1.00 -2.00 -2.00 0.0670
1.00 2.00 1.00 0.0570
1.00 0.00 2.00 0.0830
-1.00 -2.00 0.00 0.0510
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 C1 100.21(7) . . ?
N1 P1 C7 114.34(8) . . ?
N1 P1 C10 113.73(8) . . ?
C1 P1 C7 111.40(8) . . ?
C1 P1 C10 110.45(8) . . ?
C7 P1 C10 106.71(8) . . ?
P1 N1 B1 112.84(10) . . ?
B2 N1 P1 117.34(12) . . ?
B2 N1 B1 128.42(14) . . ?
C25 N2 B2 117.31(13) . . ?
C29 N2 C25 116.51(14) . . ?
C29 N2 B2 126.11(14) . . ?
C27 N3 C30 120.54(15) . . ?
C27 N3 C31 121.41(16) . . ?
C31 N3 C30 117.69(15) . . ?
C2 C1 P1 108.46(12) . . ?
C6 C1 P1 128.85(13) . . ?
C6 C1 C2 122.68(15) . . ?
C1 C2 B1 116.60(14) . . ?
C3 C2 C1 116.15(15) . . ?
C3 C2 B1 127.25(15) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.59(17) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.76(16) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.56(16) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 H6 120.4 . . ?
C5 C6 C1 119.25(17) . . ?
C5 C6 H6 120.4 . . ?
P1 C7 H7 106.9 . . ?
C8 C7 P1 110.67(12) . . ?
C8 C7 H7 106.9 . . ?
C8 C7 C9 111.07(16) . . ?
C9 C7 P1 113.89(13) . . ?
C9 C7 H7 106.9 . . ?
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 . . ?
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 . . ?
P1 C10 H10 105.0 . . ?
C11 C10 P1 116.43(13) . . ?
C11 C10 H10 105.0 . . ?
C11 C10 C12 111.46(16) . . ?
C12 C10 P1 112.79(13) . . ?
C12 C10 H10 105.0 . . ?
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 . . ?
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 . . ?
C14 C13 H13 104.2 . . ?
C14 C13 B1 117.96(14) . . ?
C18 C13 H13 104.2 . . ?
C18 C13 C14 107.83(14) . . ?
C18 C13 B1 116.76(14) . . ?
B1 C13 H13 104.2 . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C15 C14 C13 111.97(16) . . ?
C15 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C14 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
C16 C15 C14 111.44(16) . . ?
C16 C15 H15A 109.3 . . ?
C16 C15 H15B 109.3 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C15 C16 C17 111.07(16) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C16 C17 H17A 109.3 . . ?
C16 C17 H17B 109.3 . . ?
C16 C17 C18 111.41(16) . . ?
H17A C17 H17B 108.0 . . ?
C18 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
C13 C18 C17 112.03(15) . . ?
C13 C18 H18A 109.2 . . ?
C13 C18 H18B 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C20 C19 H19 106.6 . . ?
C20 C19 C24 106.20(14) . . ?
C20 C19 B1 114.57(14) . . ?
C24 C19 H19 106.6 . . ?
C24 C19 B1 115.77(14) . . ?
B1 C19 H19 106.6 . . ?
C19 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 C19 113.78(15) . . ?
C21 C20 H20A 108.8 . . ?
C21 C20 H20B 108.8 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 C20 111.11(16) . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 C21 110.89(16) . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C22 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C22 C23 C24 111.92(16) . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
C19 C24 H24A 109.0 . . ?
C19 C24 H24B 109.0 . . ?
C23 C24 C19 112.90(16) . . ?
C23 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
N2 C25 H25 118.0 . . ?
N2 C25 C26 123.98(16) . . ?
C26 C25 H25 118.0 . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.15(16) . . ?
C27 C26 H26 119.9 . . ?
N3 C27 C26 121.70(16) . . ?
N3 C27 C28 122.92(16) . . ?
C28 C27 C26 115.38(15) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.45(16) . . ?
C29 C28 H28 119.8 . . ?
N2 C29 C28 123.51(16) . . ?
N2 C29 H29 118.2 . . ?
C28 C29 H29 118.2 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Cl1A C32A Cl2A 115.6(5) . . ?
Cl1A C32A H32A 108.4 . . ?
Cl1A C32A H32B 108.4 . . ?
Cl2A C32A H32A 108.4 . . ?
Cl2A C32A H32B 108.4 . . ?
H32A C32A H32B 107.4 . . ?
Cl1B C32B Cl2B 113.7(12) . . ?
Cl1B C32B H32C 108.8 . . ?
Cl1B C32B H32D 108.8 . . ?
Cl2B C32B H32C 108.8 . . ?
Cl2B C32B H32D 108.8 . . ?
H32C C32B H32D 107.7 . . ?
N1 B1 C13 115.22(13) . . ?
N1 B1 C19 110.35(13) . . ?
C2 B1 N1 101.40(13) . . ?
C2 B1 C13 108.49(13) . . ?
C2 B1 C19 110.40(13) . . ?
C13 B1 C19 110.57(14) . . ?
N1 B2 N2 113.79(14) . . ?
N1 B2 H2A 113.7(9) . . ?
N1 B2 H2B 112.1(9) . . ?
N2 B2 H2A 104.8(9) . . ?
N2 B2 H2B 102.9(9) . . ?
H2A B2 H2B 108.8(12) . . ?
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
Cl1A C32A 1.722(11) . ?
Cl1B C32B 1.65(2) . ?
Cl2A C32A 1.724(14) . ?
Cl2B C32B 1.70(2) . ?
P1 N1 1.6125(14) . ?
P1 C1 1.7910(16) . ?
P1 C7 1.8348(17) . ?
P1 C10 1.8431(18) . ?
N1 B1 1.643(2) . ?
N1 B2 1.527(2) . ?
N2 C25 1.349(2) . ?
N2 C29 1.340(2) . ?
N2 B2 1.633(2) . ?
N3 C27 1.354(2) . ?
N3 C30 1.454(2) . ?
N3 C31 1.453(2) . ?
C1 C2 1.403(2) . ?
C1 C6 1.400(2) . ?
C2 C3 1.401(2) . ?
C2 B1 1.633(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(2) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.516(3) . ?
C7 C9 1.529(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.530(3) . ?
C10 C12 1.532(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 1.0000 . ?
C13 C14 1.534(2) . ?
C13 C18 1.529(2) . ?
C13 B1 1.647(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.527(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.520(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.524(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.532(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19 1.0000 . ?
C19 C20 1.538(2) . ?
C19 C24 1.540(2) . ?
C19 B1 1.662(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.528(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.522(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.521(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.526(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25 0.9500 . ?
C25 C26 1.361(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.411(2) . ?
C27 C28 1.408(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.370(2) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32A H32A 0.9900 . ?
C32A H32B 0.9900 . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
B2 H2A 1.125(17) . ?
B2 H2B 1.130(17) . ?
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 B1 C2 -7.23(15) . . . . ?
P1 N1 B1 C13 -124.14(13) . . . . ?
P1 N1 B1 C19 109.77(13) . . . . ?
P1 N1 B2 N2 -114.05(14) . . . . ?
P1 C1 C2 C3 177.49(12) . . . . ?
P1 C1 C2 B1 -2.28(17) . . . . ?
P1 C1 C6 C5 -177.58(13) . . . . ?
N1 P1 C1 C2 -2.31(13) . . . . ?
N1 P1 C1 C6 176.28(15) . . . . ?
N1 P1 C7 C8 -48.96(15) . . . . ?
N1 P1 C7 C9 -174.93(13) . . . . ?
N1 P1 C10 C11 146.66(14) . . . . ?
N1 P1 C10 C12 -82.64(15) . . . . ?
N2 C25 C26 C27 -0.1(3) . . . . ?
N3 C27 C28 C29 179.23(17) . . . . ?
C1 P1 N1 B1 6.01(12) . . . . ?
C1 P1 N1 B2 -161.64(12) . . . . ?
C1 P1 C7 C8 63.77(15) . . . . ?
C1 P1 C7 C9 -62.20(16) . . . . ?
C1 P1 C10 C11 34.91(16) . . . . ?
C1 P1 C10 C12 165.61(13) . . . . ?
C1 C2 C3 C4 0.6(2) . . . . ?
C1 C2 B1 N1 5.79(18) . . . . ?
C1 C2 B1 C13 127.51(15) . . . . ?
C1 C2 B1 C19 -111.18(16) . . . . ?
C2 C1 C6 C5 0.8(3) . . . . ?
C2 C3 C4 C5 0.4(3) . . . . ?
C3 C2 B1 N1 -173.95(15) . . . . ?
C3 C2 B1 C13 -52.2(2) . . . . ?
C3 C2 B1 C19 69.1(2) . . . . ?
C3 C4 C5 C6 -0.8(3) . . . . ?
C4 C5 C6 C1 0.2(3) . . . . ?
C6 C1 C2 C3 -1.2(2) . . . . ?
C6 C1 C2 B1 179.02(15) . . . . ?
C7 P1 N1 B1 125.24(11) . . . . ?
C7 P1 N1 B2 -42.40(14) . . . . ?
C7 P1 C1 C2 -123.67(12) . . . . ?
C7 P1 C1 C6 54.92(18) . . . . ?
C7 P1 C10 C11 -86.32(15) . . . . ?
C7 P1 C10 C12 44.38(16) . . . . ?
C10 P1 N1 B1 -111.84(12) . . . . ?
C10 P1 N1 B2 80.52(14) . . . . ?
C10 P1 C1 C2 117.93(12) . . . . ?
C10 P1 C1 C6 -63.49(17) . . . . ?
C10 P1 C7 C8 -175.61(13) . . . . ?
C10 P1 C7 C9 58.42(16) . . . . ?
C13 C14 C15 C16 -57.2(2) . . . . ?
C14 C13 C18 C17 -57.63(19) . . . . ?
C14 C13 B1 N1 -74.98(19) . . . . ?
C14 C13 B1 C2 172.20(14) . . . . ?
C14 C13 B1 C19 51.00(19) . . . . ?
C14 C15 C16 C17 53.8(2) . . . . ?
C15 C16 C17 C18 -53.5(2) . . . . ?
C16 C17 C18 C13 56.8(2) . . . . ?
C18 C13 C14 C15 57.87(19) . . . . ?
C18 C13 B1 N1 56.02(19) . . . . ?
C18 C13 B1 C2 -56.80(18) . . . . ?
C18 C13 B1 C19 -178.01(14) . . . . ?
C19 C20 C21 C22 57.0(2) . . . . ?
C20 C19 C24 C23 56.59(19) . . . . ?
C20 C19 B1 N1 -65.23(17) . . . . ?
C20 C19 B1 C2 46.04(19) . . . . ?
C20 C19 B1 C13 166.11(13) . . . . ?
C20 C21 C22 C23 -52.8(2) . . . . ?
C21 C22 C23 C24 53.5(2) . . . . ?
C22 C23 C24 C19 -57.3(2) . . . . ?
C24 C19 C20 C21 -56.91(19) . . . . ?
C24 C19 B1 N1 170.61(14) . . . . ?
C24 C19 B1 C2 -78.12(18) . . . . ?
C24 C19 B1 C13 41.95(19) . . . . ?
C25 N2 C29 C28 1.9(3) . . . . ?
C25 N2 B2 N1 -169.31(15) . . . . ?
C25 C26 C27 N3 -178.63(16) . . . . ?
C25 C26 C27 C28 0.9(3) . . . . ?
C26 C27 C28 C29 -0.3(3) . . . . ?
C27 C28 C29 N2 -1.2(3) . . . . ?
C29 N2 C25 C26 -1.3(3) . . . . ?
C29 N2 B2 N1 13.5(2) . . . . ?
C30 N3 C27 C26 -9.1(3) . . . . ?
C30 N3 C27 C28 171.41(17) . . . . ?
C31 N3 C27 C26 177.93(17) . . . . ?
C31 N3 C27 C28 -1.6(3) . . . . ?
B1 N1 B2 N2 80.5(2) . . . . ?
B1 C2 C3 C4 -179.69(16) . . . . ?
B1 C13 C14 C15 -167.19(15) . . . . ?
B1 C13 C18 C17 166.82(14) . . . . ?
B1 C19 C20 C21 173.98(14) . . . . ?
B1 C19 C24 C23 -175.01(15) . . . . ?
B2 N1 B1 C2 158.73(14) . . . . ?
B2 N1 B1 C13 41.8(2) . . . . ?
B2 N1 B1 C19 -84.27(19) . . . . ?
B2 N2 C25 C26 -178.69(16) . . . . ?
B2 N2 C29 C28 179.08(17) . . . . ?
