#------------------------------------------------------------------------------
#$Date: 2021-10-06 16:57:59 +0300 (Wed, 06 Oct 2021) $
#$Revision: 269648 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/88/7128817.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_7128817
loop_
_publ_author_name
'Morris, Louis J.'
'Carpentier, Ambre'
'Maron, Laurent'
'Okuda, Jun'
_publ_section_title
;
 Reductive elimination of [AlH₂]⁺ from a cationic
 Ga-Al dihydride.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9454
_journal_page_last               9457
_journal_paper_doi               10.1039/d1cc03706d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C14 H26 Al N4, C32 H36 B'
_chemical_formula_sum            'C46 H62 Al B N4'
_chemical_formula_weight         708.78
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-09 deposited with the CCDC.	2021-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.03(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.068(3)
_cell_length_b                   12.667(3)
_cell_length_c                   22.560(5)
_cell_measurement_reflns_used    37994
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.22
_cell_measurement_theta_min      4.06
_cell_volume                     4340.8(18)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
 3531 frames, detector distance = 55 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            60757
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.999
_diffrn_reflns_theta_min         4.059
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.8750
_exptl_absorpt_correction_T_min  0.4759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0380
_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)+(0.0618P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6020
_reflns_number_total             8449
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc03706d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7128813--7128817.cif.'
_cod_original_cell_volume        4340.8(17)
_cod_database_code               7128817
_shelx_shelxl_version_number     2014/7
_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   0.962
_shelx_estimated_absorpt_t_min   0.880
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C20(H20), C24(H24), C26(H26), C28(H28), C32(H32),
 C34(H34), C36(H36), C40(H40), C42(H42), C44(H44)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,
 H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Al1 Al 0.17621(3) 0.45194(4) 0.56931(2) 0.03267(12) Uani 1 1 d . . . . .
H1 H 0.1365(12) 0.4415(14) 0.6204(9) 0.045(5) Uiso 1 1 d . . . . .
H2 H 0.1743(13) 0.5611(15) 0.5423(9) 0.051(5) Uiso 1 1 d . . . . .
N1 N 0.11589(8) 0.24491(10) 0.50273(6) 0.0301(3) Uani 1 1 d . . . . .
N2 N 0.07646(8) 0.37080(10) 0.43647(6) 0.0297(3) Uani 1 1 d . . . . .
N3 N 0.35850(8) 0.39654(11) 0.56999(6) 0.0338(3) Uani 1 1 d . . . . .
N4 N 0.34834(8) 0.36303(10) 0.66046(6) 0.0315(3) Uani 1 1 d . . . . .
C1 C 0.11851(9) 0.35073(12) 0.49809(7) 0.0291(3) Uani 1 1 d . . . . .
C2 C 0.15172(12) 0.18561(14) 0.56112(8) 0.0401(4) Uani 1 1 d . . . . .
H2A H 0.1052 0.1422 0.5679 0.060 Uiso 1 1 calc R U . . .
H2B H 0.1744 0.2349 0.5962 0.060 Uiso 1 1 calc R U . . .
H2C H 0.1996 0.1399 0.5584 0.060 Uiso 1 1 calc R U . . .
C3 C 0.07291(10) 0.19810(12) 0.44517(7) 0.0310(3) Uani 1 1 d . . . . .
C4 C 0.06362(11) 0.08196(13) 0.43688(8) 0.0391(4) Uani 1 1 d . . . . .
H4A H 0.0321 0.0538 0.4640 0.059 Uiso 1 1 calc R U . . .
H4B H 0.1221 0.0496 0.4481 0.059 Uiso 1 1 calc R U . . .
H4C H 0.0305 0.0658 0.3930 0.059 Uiso 1 1 calc R U . . .
C5 C 0.04729(9) 0.27851(12) 0.40324(7) 0.0311(3) Uani 1 1 d . . . . .
C6 C -0.00385(11) 0.27876(14) 0.33500(8) 0.0406(4) Uani 1 1 d . . . . .
H6A H -0.0572 0.3213 0.3277 0.061 Uiso 1 1 calc R U . . .
H6B H -0.0202 0.2062 0.3209 0.061 Uiso 1 1 calc R U . . .
H6C H 0.0322 0.3090 0.3116 0.061 Uiso 1 1 calc R U . . .
C7 C 0.06476(11) 0.47503(13) 0.40745(8) 0.0380(4) Uani 1 1 d . . . . .
H7A H 0.0924 0.5283 0.4393 0.057 Uiso 1 1 calc R U . . .
H7B H 0.0018 0.4903 0.3890 0.057 Uiso 1 1 calc R U . . .
H7C H 0.0923 0.4765 0.3745 0.057 Uiso 1 1 calc R U . . .
C8 C 0.30127(9) 0.39820(12) 0.60258(7) 0.0306(3) Uani 1 1 d . . . . .
C9 C 0.33726(11) 0.42773(16) 0.50438(8) 0.0443(4) Uani 1 1 d . . . . .
H9A H 0.3427 0.3664 0.4794 0.066 Uiso 1 1 calc R U . . .
H9B H 0.3780 0.4831 0.5009 0.066 Uiso 1 1 calc R U . . .
H9C H 0.2768 0.4546 0.4888 0.066 Uiso 1 1 calc R U . . .
C10 C 0.44084(10) 0.36171(13) 0.60739(8) 0.0369(4) Uani 1 1 d . . . . .
C11 C 0.51703(11) 0.35366(17) 0.58358(10) 0.0504(5) Uani 1 1 d . . . . .
H11A H 0.5342 0.4245 0.5745 0.076 Uiso 1 1 calc R U . . .
H11B H 0.5002 0.3111 0.5452 0.076 Uiso 1 1 calc R U . . .
H11C H 0.5667 0.3201 0.6154 0.076 Uiso 1 1 calc R U . . .
C12 C 0.43428(9) 0.34092(13) 0.66440(8) 0.0348(4) Uani 1 1 d . . . . .
C13 C 0.50099(11) 0.30288(15) 0.72346(9) 0.0475(4) Uani 1 1 d . . . . .
H13A H 0.5560 0.2865 0.7155 0.071 Uiso 1 1 calc R U . . .
H13B H 0.4790 0.2392 0.7381 0.071 Uiso 1 1 calc R U . . .
H13C H 0.5118 0.3580 0.7556 0.071 Uiso 1 1 calc R U . . .
C14 C 0.31350(11) 0.34252(14) 0.71183(8) 0.0381(4) Uani 1 1 d . . . . .
H14A H 0.2541 0.3721 0.7013 0.057 Uiso 1 1 calc R U . . .
H14B H 0.3519 0.3756 0.7503 0.057 Uiso 1 1 calc R U . . .
H14C H 0.3113 0.2662 0.7182 0.057 Uiso 1 1 calc R U . . .
C15 C 0.74393(9) 0.50179(12) 0.81372(7) 0.0291(3) Uani 1 1 d . . . . .
C16 C 0.80218(10) 0.44037(12) 0.86145(7) 0.0318(3) Uani 1 1 d . . . . .
H16 H 0.8548 0.4162 0.8554 0.038 Uiso 1 1 calc R U . . .
C17 C 0.78743(10) 0.41310(13) 0.91660(8) 0.0362(4) Uani 1 1 d . . . . .
C18 C 0.71199(11) 0.45186(14) 0.92698(8) 0.0398(4) Uani 1 1 d . . . . .
H18 H 0.7008 0.4345 0.9647 0.048 Uiso 1 1 calc R U . . .
C19 C 0.65321(11) 0.51544(13) 0.88271(8) 0.0379(4) Uani 1 1 d . . . . .
C20 C 0.67023(9) 0.53936(12) 0.82721(7) 0.0316(3) Uani 1 1 d . . . . .
H20 H 0.6298 0.5833 0.7972 0.038 Uiso 1 1 calc R U . . .
C21 C 0.85076(11) 0.34091(15) 0.96379(9) 0.0468(4) Uani 1 1 d . . . . .
H21A H 0.8258 0.2697 0.9602 0.070 Uiso 1 1 calc R U . . .
H21B H 0.8606 0.3679 1.0062 0.070 Uiso 1 1 calc R U . . .
H21C H 0.9069 0.3385 0.9555 0.070 Uiso 1 1 calc R U . . .
C22 C 0.57136(13) 0.55742(17) 0.89410(10) 0.0531(5) Uani 1 1 d . . . . .
H22A H 0.5834 0.6278 0.9130 0.080 Uiso 1 1 calc R U . . .
H22B H 0.5546 0.5097 0.9225 0.080 Uiso 1 1 calc R U . . .
H22C H 0.5232 0.5619 0.8541 0.080 Uiso 1 1 calc R U . . .
C23 C 0.86960(9) 0.54505(12) 0.76574(7) 0.0266(3) Uani 1 1 d . . . . .
C24 C 0.90018(9) 0.63696(12) 0.80100(7) 0.0275(3) Uani 1 1 d . . . . .
H24 H 0.8581 0.6827 0.8089 0.033 Uiso 1 1 calc R U . . .
C25 C 0.98877(9) 0.66478(12) 0.82502(7) 0.0282(3) Uani 1 1 d . . . . .
C26 C 1.05030(9) 0.59955(12) 0.81161(7) 0.0307(3) Uani 1 1 d . . . . .
H26 H 1.1110 0.6174 0.8273 0.037 Uiso 1 1 calc R U . . .
C27 C 1.02425(9) 0.50916(12) 0.77571(7) 0.0299(3) Uani 1 1 d . . . . .
C28 C 0.93452(9) 0.48287(12) 0.75389(7) 0.0281(3) Uani 1 1 d . . . . .
H28 H 0.9170 0.4201 0.7300 0.034 Uiso 1 1 calc R U . . .
C29 C 1.01885(10) 0.76072(13) 0.86590(8) 0.0348(3) Uani 1 1 d . . . . .
H29A H 0.9687 0.8080 0.8608 0.052 Uiso 1 1 calc R U . . .
H29B H 1.0643 0.7977 0.8537 0.052 Uiso 1 1 calc R U . . .
H29C H 1.0431 0.7388 0.9099 0.052 Uiso 1 1 calc R U . . .
C30 C 1.09176(10) 0.44081(14) 0.76056(8) 0.0385(4) Uani 1 1 d . . . . .
H30A H 1.0750 0.3664 0.7605 0.058 Uiso 1 1 calc R U . . .
H30B H 1.1496 0.4518 0.7922 0.058 Uiso 1 1 calc R U . . .
H30C H 1.0945 0.4599 0.7191 0.058 Uiso 1 1 calc R U . . .
C31 C 0.74696(9) 0.39679(12) 0.71139(8) 0.0314(3) Uani 1 1 d . . . . .
C32 C 0.74633(9) 0.38697(13) 0.64945(8) 0.0336(3) Uani 1 1 d . . . . .
H32 H 0.7565 0.4484 0.6287 0.040 Uiso 1 1 calc R U . . .
C33 C 0.73150(10) 0.29168(14) 0.61659(9) 0.0398(4) Uani 1 1 d . . . . .
C34 C 0.71714(10) 0.20126(14) 0.64698(10) 0.0444(4) Uani 1 1 d . . . . .
H34 H 0.7071 0.1357 0.6253 0.053 Uiso 1 1 calc R U . . .
C35 C 0.71731(10) 0.20553(13) 0.70824(9) 0.0427(4) Uani 1 1 d . . . . .
C36 C 0.73183(10) 0.30263(13) 0.73928(8) 0.0363(4) Uani 1 1 d . . . . .
H36 H 0.7315 0.3052 0.7813 0.044 Uiso 1 1 calc R U . . .
C37 C 0.72719(13) 0.28638(17) 0.54914(10) 0.0552(5) Uani 1 1 d . . . . .
H37A H 0.6664 0.2979 0.5220 0.083 Uiso 1 1 calc R U . . .
H37B H 0.7472 0.2168 0.5404 0.083 Uiso 1 1 calc R U . . .
H37C H 0.7652 0.3411 0.5410 0.083 Uiso 1 1 calc R U . . .
C38 C 0.70089(13) 0.10748(15) 0.74133(11) 0.0582(5) Uani 1 1 d . . . . .
H38A H 0.7534 0.0916 0.7771 0.087 Uiso 1 1 calc R U . . .
H38B H 0.6879 0.0478 0.7121 0.087 Uiso 1 1 calc R U . . .
H38C H 0.6507 0.1197 0.7561 0.087 Uiso 1 1 calc R U . . .
C39 C 0.70106(9) 0.59851(12) 0.69820(7) 0.0284(3) Uani 1 1 d . . . . .
C40 C 0.60877(9) 0.58951(13) 0.67954(7) 0.0323(3) Uani 1 1 d . . . . .
H40 H 0.5845 0.5318 0.6952 0.039 Uiso 1 1 calc R U . . .
C41 C 0.55116(10) 0.66033(13) 0.63942(8) 0.0360(4) Uani 1 1 d . . . . .
C42 C 0.58625(11) 0.74203(14) 0.61371(8) 0.0386(4) Uani 1 1 d . . . . .
H42 H 0.5478 0.7910 0.5861 0.046 Uiso 1 1 calc R U . . .
C43 C 0.67676(11) 0.75290(13) 0.62791(8) 0.0361(4) Uani 1 1 d . . . . .
C44 C 0.73223(10) 0.68190(12) 0.67009(7) 0.0311(3) Uani 1 1 d . . . . .
H44 H 0.7940 0.6905 0.6803 0.037 Uiso 1 1 calc R U . . .
C45 C 0.45234(10) 0.64927(16) 0.62391(9) 0.0470(4) Uani 1 1 d . . . . .
H45A H 0.4276 0.7166 0.6316 0.070 Uiso 1 1 calc R U . . .
H45B H 0.4398 0.5944 0.6504 0.070 Uiso 1 1 calc R U . . .
H45C H 0.4258 0.6296 0.5797 0.070 Uiso 1 1 calc R U . . .
C46 C 0.71393(13) 0.83878(16) 0.59704(9) 0.0500(5) Uani 1 1 d . . . . .
H46A H 0.7048 0.9077 0.6137 0.075 Uiso 1 1 calc R U . . .
H46B H 0.6839 0.8373 0.5516 0.075 Uiso 1 1 calc R U . . .
H46C H 0.7771 0.8269 0.6059 0.075 Uiso 1 1 calc R U . . .
B1 B 0.76478(10) 0.51243(14) 0.74678(8) 0.0281(4) Uani 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 0.0181 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'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 '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'
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
H1 Al1 H2 115.8(10) . . ?
C1 Al1 H1 110.8(7) . . ?
C1 Al1 H2 108.4(7) . . ?
C8 Al1 H1 107.9(7) . . ?
C8 Al1 H2 110.2(7) . . ?
C8 Al1 C1 102.92(7) . . ?
C1 N1 C2 124.66(13) . . ?
C1 N1 C3 111.77(13) . . ?
C3 N1 C2 123.55(14) . . ?
C1 N2 C5 111.34(13) . . ?
C1 N2 C7 125.29(13) . . ?
C5 N2 C7 123.35(13) . . ?
C8 N3 C9 124.83(13) . . ?
C8 N3 C10 110.90(14) . . ?
C10 N3 C9 124.27(13) . . ?
C8 N4 C12 111.15(13) . . ?
C8 N4 C14 125.75(13) . . ?
C12 N4 C14 122.96(14) . . ?
N1 C1 Al1 125.85(11) . . ?
N1 C1 N2 104.39(13) . . ?
N2 C1 Al1 129.75(12) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 C4 122.67(14) . . ?
C5 C3 N1 106.03(14) . . ?
C5 C3 C4 131.28(15) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 122.18(14) . . ?
C3 C5 N2 106.47(14) . . ?
C3 C5 C6 131.33(15) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 Al1 125.02(12) . . ?
N3 C8 N4 104.74(13) . . ?
N4 C8 Al1 130.13(11) . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 C11 122.26(16) . . ?
C12 C10 N3 106.61(14) . . ?
C12 C10 C11 131.12(16) . . ?
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 . . ?
N4 C12 C13 122.30(15) . . ?
C10 C12 N4 106.59(14) . . ?
C10 C12 C13 131.10(15) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 B1 117.43(13) . . ?
C20 C15 C16 114.86(14) . . ?
C20 C15 B1 127.46(14) . . ?
C15 C16 H16 118.0 . . ?
C17 C16 C15 124.00(14) . . ?
C17 C16 H16 118.0 . . ?
C16 C17 C18 118.38(15) . . ?
C16 C17 C21 120.61(15) . . ?
C18 C17 C21 120.99(15) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.53(15) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C20 118.97(15) . . ?
C18 C19 C22 120.42(16) . . ?
C20 C19 C22 120.60(15) . . ?
C15 C20 C19 123.19(15) . . ?
C15 C20 H20 118.4 . . ?
C19 C20 H20 118.4 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 B1 119.56(13) . . ?
C28 C23 C24 115.42(13) . . ?
C28 C23 B1 124.80(13) . . ?
C23 C24 H24 118.2 . . ?
C25 C24 C23 123.65(14) . . ?
C25 C24 H24 118.2 . . ?
C24 C25 C26 118.18(14) . . ?
C24 C25 C29 121.69(14) . . ?
C26 C25 C29 120.12(13) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 C25 121.04(13) . . ?
C27 C26 H26 119.5 . . ?
C26 C27 C28 118.75(14) . . ?
C26 C27 C30 120.20(13) . . ?
C28 C27 C30 121.05(14) . . ?
C23 C28 C27 122.93(14) . . ?
C23 C28 H28 118.5 . . ?
C27 C28 H28 118.5 . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C36 115.17(15) . . ?
C32 C31 B1 120.41(14) . . ?
C36 C31 B1 124.42(14) . . ?
C31 C32 H32 118.3 . . ?
C33 C32 C31 123.47(16) . . ?
C33 C32 H32 118.3 . . ?
C32 C33 C37 121.34(17) . . ?
C34 C33 C32 118.49(17) . . ?
C34 C33 C37 120.12(16) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 C33 120.91(16) . . ?
C35 C34 H34 119.5 . . ?
C34 C35 C36 118.76(17) . . ?
C34 C35 C38 121.09(17) . . ?
C36 C35 C38 120.14(18) . . ?
C31 C36 H36 118.4 . . ?
C35 C36 C31 123.20(17) . . ?
C35 C36 H36 118.4 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 B1 120.77(14) . . ?
C44 C39 C40 114.92(14) . . ?
C44 C39 B1 124.25(13) . . ?
C39 C40 H40 118.1 . . ?
C41 C40 C39 123.71(15) . . ?
C41 C40 H40 118.1 . . ?
C40 C41 C42 118.46(15) . . ?
C40 C41 C45 120.99(16) . . ?
C42 C41 C45 120.54(15) . . ?
C41 C42 H42 119.6 . . ?
C43 C42 C41 120.86(15) . . ?
C43 C42 H42 119.6 . . ?
C42 C43 C44 118.68(15) . . ?
C42 C43 C46 120.30(15) . . ?
C44 C43 C46 121.01(15) . . ?
C39 C44 H44 118.4 . . ?
C43 C44 C39 123.27(14) . . ?
C43 C44 H44 118.4 . . ?
C41 C45 H45A 109.5 . . ?
C41 C45 H45B 109.5 . . ?
C41 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C23 B1 C15 106.08(12) . . ?
C31 B1 C15 108.34(12) . . ?
C31 B1 C23 110.47(12) . . ?
C39 B1 C15 113.24(12) . . ?
C39 B1 C23 111.58(12) . . ?
C39 B1 C31 107.11(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
Al1 H1 1.495(18) . ?
Al1 H2 1.508(19) . ?
Al1 C1 2.0281(17) . ?
Al1 C8 2.0203(16) . ?
N1 C1 1.346(2) . ?
N1 C2 1.462(2) . ?
N1 C3 1.389(2) . ?
N2 C1 1.357(2) . ?
N2 C5 1.385(2) . ?
N2 C7 1.458(2) . ?
N3 C8 1.3517(19) . ?
N3 C9 1.461(2) . ?
N3 C10 1.389(2) . ?
N4 C8 1.353(2) . ?
N4 C12 1.3832(19) . ?
N4 C14 1.465(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.484(2) . ?
C3 C5 1.359(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.490(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.492(2) . ?
C10 C12 1.350(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.492(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.408(2) . ?
C15 C20 1.399(2) . ?
C15 B1 1.656(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(2) . ?
C17 C18 1.397(2) . ?
C17 C21 1.516(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(2) . ?
C19 C20 1.399(2) . ?
C19 C22 1.516(2) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.405(2) . ?
C23 C28 1.401(2) . ?
C23 B1 1.649(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.393(2) . ?
C25 C26 1.395(2) . ?
C25 C29 1.507(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.386(2) . ?
C27 C28 1.403(2) . ?
C27 C30 1.512(2) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.400(2) . ?
C31 C36 1.406(2) . ?
C31 B1 1.648(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.396(2) . ?
C33 C34 1.392(3) . ?
C33 C37 1.502(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.382(3) . ?
C35 C36 1.397(2) . ?
C35 C38 1.516(3) . ?
C36 H36 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.408(2) . ?
C39 C44 1.406(2) . ?
C39 B1 1.645(2) . ?
C40 H40 0.9500 . ?
C40 C41 1.391(2) . ?
C41 C42 1.392(2) . ?
C41 C45 1.517(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.390(2) . ?
C43 C44 1.398(2) . ?
C43 C46 1.515(2) . ?
C44 H44 0.9500 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
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
N1 C3 C5 N2 0.76(15) . . . . ?
N1 C3 C5 C6 -177.60(15) . . . . ?
N3 C10 C12 N4 0.23(18) . . . . ?
N3 C10 C12 C13 -179.09(17) . . . . ?
C1 N1 C3 C4 177.85(14) . . . . ?
C1 N1 C3 C5 -0.47(16) . . . . ?
C1 N2 C5 C3 -0.83(16) . . . . ?
C1 N2 C5 C6 177.71(14) . . . . ?
C2 N1 C1 Al1 2.5(2) . . . . ?
C2 N1 C1 N2 -178.66(13) . . . . ?
C2 N1 C3 C4 -3.5(2) . . . . ?
C2 N1 C3 C5 178.18(14) . . . . ?
C3 N1 C1 Al1 -178.84(10) . . . . ?
C3 N1 C1 N2 -0.03(15) . . . . ?
C4 C3 C5 N2 -177.36(15) . . . . ?
C4 C3 C5 C6 4.3(3) . . . . ?
C5 N2 C1 Al1 179.27(10) . . . . ?
C5 N2 C1 N1 0.53(15) . . . . ?
C7 N2 C1 Al1 0.9(2) . . . . ?
C7 N2 C1 N1 -177.84(13) . . . . ?
C7 N2 C5 C3 177.58(13) . . . . ?
C7 N2 C5 C6 -3.9(2) . . . . ?
C8 N3 C10 C11 -179.09(16) . . . . ?
C8 N3 C10 C12 0.25(19) . . . . ?
C8 N4 C12 C10 -0.65(18) . . . . ?
C8 N4 C12 C13 178.75(15) . . . . ?
C9 N3 C8 Al1 -3.7(2) . . . . ?
C9 N3 C8 N4 179.74(15) . . . . ?
C9 N3 C10 C11 0.5(3) . . . . ?
C9 N3 C10 C12 179.89(15) . . . . ?
C10 N3 C8 Al1 175.91(11) . . . . ?
C10 N3 C8 N4 -0.63(17) . . . . ?
C11 C10 C12 N4 179.49(18) . . . . ?
C11 C10 C12 C13 0.2(3) . . . . ?
C12 N4 C8 Al1 -175.51(12) . . . . ?
C12 N4 C8 N3 0.79(17) . . . . ?
C14 N4 C8 Al1 8.8(2) . . . . ?
C14 N4 C8 N3 -174.88(14) . . . . ?
C14 N4 C12 C10 175.15(14) . . . . ?
C14 N4 C12 C13 -5.4(2) . . . . ?
C15 C16 C17 C18 -2.6(3) . . . . ?
C15 C16 C17 C21 176.11(16) . . . . ?
C16 C15 C20 C19 -2.1(2) . . . . ?
C16 C15 B1 C23 -49.36(17) . . . . ?
C16 C15 B1 C31 69.26(16) . . . . ?
C16 C15 B1 C39 -172.07(13) . . . . ?
C16 C17 C18 C19 0.5(3) . . . . ?
C17 C18 C19 C20 0.6(3) . . . . ?
C17 C18 C19 C22 180.00(18) . . . . ?
C18 C19 C20 C15 0.3(3) . . . . ?
C20 C15 C16 C17 3.3(2) . . . . ?
C20 C15 B1 C23 136.71(15) . . . . ?
C20 C15 B1 C31 -104.67(17) . . . . ?
C20 C15 B1 C39 14.0(2) . . . . ?
C21 C17 C18 C19 -178.19(17) . . . . ?
C22 C19 C20 C15 -179.10(16) . . . . ?
C23 C24 C25 C26 2.2(2) . . . . ?
C23 C24 C25 C29 -176.18(14) . . . . ?
C24 C23 C28 C27 0.4(2) . . . . ?
C24 C23 B1 C15 -57.58(17) . . . . ?
C24 C23 B1 C31 -174.79(13) . . . . ?
C24 C23 B1 C39 66.18(17) . . . . ?
C24 C25 C26 C27 -0.4(2) . . . . ?
C25 C26 C27 C28 -1.2(2) . . . . ?
C25 C26 C27 C30 178.69(14) . . . . ?
C26 C27 C28 C23 1.3(2) . . . . ?
C28 C23 C24 C25 -2.1(2) . . . . ?
C28 C23 B1 C15 116.75(15) . . . . ?
C28 C23 B1 C31 -0.5(2) . . . . ?
C28 C23 B1 C39 -119.50(15) . . . . ?
C29 C25 C26 C27 178.00(14) . . . . ?
C30 C27 C28 C23 -178.67(14) . . . . ?
C31 C32 C33 C34 -0.5(2) . . . . ?
C31 C32 C33 C37 177.01(15) . . . . ?
C32 C31 C36 C35 0.1(2) . . . . ?
C32 C31 B1 C15 170.11(12) . . . . ?
C32 C31 B1 C23 -74.09(17) . . . . ?
C32 C31 B1 C39 47.63(17) . . . . ?
C32 C33 C34 C35 0.2(2) . . . . ?
C33 C34 C35 C36 0.3(2) . . . . ?
C33 C34 C35 C38 179.44(15) . . . . ?
C34 C35 C36 C31 -0.4(2) . . . . ?
C36 C31 C32 C33 0.3(2) . . . . ?
C36 C31 B1 C15 -10.07(18) . . . . ?
C36 C31 B1 C23 105.73(16) . . . . ?
C36 C31 B1 C39 -132.55(14) . . . . ?
C37 C33 C34 C35 -177.34(15) . . . . ?
C38 C35 C36 C31 -179.61(15) . . . . ?
C39 C40 C41 C42 3.2(2) . . . . ?
C39 C40 C41 C45 -176.73(15) . . . . ?
C40 C39 C44 C43 1.5(2) . . . . ?
C40 C39 B1 C15 -55.92(19) . . . . ?
C40 C39 B1 C23 -175.53(13) . . . . ?
C40 C39 B1 C31 63.45(17) . . . . ?
C40 C41 C42 C43 -0.2(2) . . . . ?
C41 C42 C43 C44 -1.9(2) . . . . ?
C41 C42 C43 C46 176.86(16) . . . . ?
C42 C43 C44 C39 1.2(2) . . . . ?
C44 C39 C40 C41 -3.8(2) . . . . ?
C44 C39 B1 C15 127.13(15) . . . . ?
C44 C39 B1 C23 7.5(2) . . . . ?
C44 C39 B1 C31 -113.50(15) . . . . ?
C45 C41 C42 C43 179.73(16) . . . . ?
C46 C43 C44 C39 -177.56(16) . . . . ?
B1 C15 C16 C17 -171.41(15) . . . . ?
B1 C15 C20 C19 171.95(15) . . . . ?
B1 C23 C24 C25 172.72(14) . . . . ?
B1 C23 C28 C27 -174.17(14) . . . . ?
B1 C31 C32 C33 -179.86(13) . . . . ?
B1 C31 C36 C35 -179.69(14) . . . . ?
B1 C39 C40 C41 178.99(14) . . . . ?
B1 C39 C44 C43 178.66(15) . . . . ?
