# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_mo_mbx01_0m_5
_database_code_depnum_ccdc_archive 'CCDC 2371034'
loop_
_audit_author_name
_audit_author_address
'Frederic Capet'
;CNRS, UCCS
France
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_audit_creation_date             2022-01-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        '[(PyA1)Y(BH4)3]2[Mg(THF)6]'
_chemical_formula_moiety         'C24 H48 Mg O6, 2(C19 H37 B3 N2 Y)'
_chemical_formula_sum            'C62 H122 B6 Mg N4 O6 Y2'
_chemical_formula_weight         1286.62
_chemical_melting_point          ?
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'
Mg Mg 0.0486 0.0363 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4849(7)
_cell_length_b                   10.9594(8)
_cell_length_c                   16.5868(12)
_cell_angle_alpha                85.776(4)
_cell_angle_beta                 85.716(4)
_cell_angle_gamma                70.181(4)
_cell_volume                     1785.7(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9681
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0753 before and 0.0445 after correction.
 
For component 2:
 wR2(int) was 0.1770 before and 0.0565 after correction.
 The Ratio of minimum to maximum transmission is 0.85.

Final HKLF 4 output contains 104062 reflections, Rint = 0.0550
 (63002 with I > 3sig(I), Rint = 0.0453)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8210
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.716
_diffrn_reflns_theta_min         1.233
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.979
_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_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.61
_diffrn_source_power             0.0305
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7396
_reflns_number_total             8210
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX2 Ver. 2014.7-1 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.302
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         8210
_refine_ls_number_restraints     456
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0444
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0531P)²+2.0797P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1124
_refine_special_details          
'The disorder on Tetrahydrofuran groups was modelled using the FragmentDB plugins in Olex2 (D. Kratzert, I. Krossing, J. Appl. Cryst. 2018, 51, 928-934),Twin,disorder'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.7515(19)
 0.2485(19)
2. 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
3. Shared sites
{O1A, O1B}
{O2A, O2B}
{O3A, O3B}
4. Restrained distances
 O3A-C31A = O3A-C28A
 1.44 with sigma of 0.02
 C30A-C29A
 1.54 with sigma of 0.02
 O1A-C20A = O1A-C23A
 1.44 with sigma of 0.02
 C31A-C30A = C29A-C28A
 1.53 with sigma of 0.02
 C20A-C21A = C22A-C23A
 1.53 with sigma of 0.02
 O2A-C27A = O2A-C24A
 1.44 with sigma of 0.02
 C26A-C25A
 1.54 with sigma of 0.02
 O3B-C28B = O3B-C31B
 1.44 with sigma of 0.02
 C21A-C22A
 1.54 with sigma of 0.02
 C29B-C30B
 1.54 with sigma of 0.02
 C28B-C29B = C30B-C31B
 1.53 with sigma of 0.02
 C27A-C26A = C25A-C24A
 1.53 with sigma of 0.02
 O1B-C20B = O1B-C23B
 1.44 with sigma of 0.02
 O2B-C24B = O2B-C27B
 1.44 with sigma of 0.02
 C25B-C26B
 1.54 with sigma of 0.02
 C20B-C21B = C22B-C23B
 1.53 with sigma of 0.02
 C21B-C22B
 1.54 with sigma of 0.02
 C24B-C25B = C26B-C27B
 1.53 with sigma of 0.02
 O3A-C30A = O3A-C29A = C31A-C29A = C30A-C28A
 2.38 with sigma of 0.04
 O1A-C21A = O1A-C22A = C20A-C22A = C21A-C23A
 2.38 with sigma of 0.04
 O2A-C26A = O2A-C25A = C27A-C25A = C26A-C24A
 2.38 with sigma of 0.04
 O3B-C29B = O3B-C30B = C28B-C30B = C29B-C31B
 2.38 with sigma of 0.04
 O1B-C21B = O1B-C22B = C20B-C22B = C21B-C23B
 2.38 with sigma of 0.04
 O2B-C25B = O2B-C26B = C24B-C26B = C25B-C27B
 2.38 with sigma of 0.04
 O2A-C26A \\sim O2A-C25A
 with sigma of 0.04
 O1A-C21A \\sim O1A-C22A
 with sigma of 0.04
 C26A-C24A \\sim C27A-C25A
 with sigma of 0.04
 O3A-C31A \\sim O3A-C28A
 with sigma of 0.02
 C20A-C21A \\sim C21A-C22A \\sim C22A-C23A
 with sigma of 0.02
 O3A-C30A \\sim O3A-C29A
 with sigma of 0.04
 C31A-C30A \\sim C30A-C29A \\sim C29A-C28A
 with sigma of 0.02
 O1A-C20A \\sim O1A-C23A
 with sigma of 0.02
 C30A-C28A \\sim C31A-C29A
 with sigma of 0.04
 O2A-C27A \\sim O2A-C24A
 with sigma of 0.02
 C28B-C29B \\sim C29B-C30B \\sim C30B-C31B
 with sigma of 0.02
 C29B-C31B \\sim C28B-C30B
 with sigma of 0.04
 C27A-C26A \\sim C26A-C25A \\sim C25A-C24A
 with sigma of 0.02
 O3B-C28B \\sim O3B-C31B
 with sigma of 0.02
 C21A-C23A \\sim C20A-C22A
 with sigma of 0.04
 O3B-C29B \\sim O3B-C30B
 with sigma of 0.04
 O2B-C25B \\sim O2B-C26B
 with sigma of 0.04
 O1B-C21B \\sim O1B-C22B
 with sigma of 0.04
 O1B-C20B \\sim O1B-C23B
 with sigma of 0.02
 O2B-C24B \\sim O2B-C27B
 with sigma of 0.02
 C21B-C23B \\sim C20B-C22B
 with sigma of 0.04
 C24B-C25B \\sim C25B-C26B \\sim C26B-C27B
 with sigma of 0.02
 C25B-C27B \\sim C24B-C26B
 with sigma of 0.04
 C20B-C21B \\sim C21B-C22B \\sim C22B-C23B
 with sigma of 0.02
 B3-H3B \\sim B3-H3C \\sim B3-H3D \\sim B3-H3A
 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
O3A \\sim C31A \\sim C30A \\sim C29A \\sim C28A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O2A \\sim C27A \\sim C26A \\sim C25A \\sim C24A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O3B \\sim C28B \\sim C29B \\sim C30B \\sim C31B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1A \\sim C20A \\sim C21A \\sim C22A \\sim C23A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O2B \\sim C24B \\sim C25B \\sim C26B \\sim C27B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1B \\sim C20B \\sim C21B \\sim C22B \\sim C23B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(O3A) = Uanis(O3B)
Uanis(C31A) = Uanis(C30A) = Uanis(C29A) = Uanis(C28A) = Uanis(C28B) =
Uanis(C29B) = Uanis(C30B) = Uanis(C31B)
Uanis(O1A) = Uanis(O1B)
Uanis(O2A) = Uanis(O2B)
Uanis(C20A) = Uanis(C21A) = Uanis(C22A) = Uanis(C23A) = Uanis(C20B) =
Uanis(C21B) = Uanis(C22B) = Uanis(C23B)
Uanis(C27A) = Uanis(C26A) = Uanis(C25A) = Uanis(C24A) = Uanis(C24B) =
Uanis(C25B) = Uanis(C26B) = Uanis(C27B)
6. Rigid body (RIGU) restrains
 O3A, C31A, C30A, C29A, C28A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2A, C27A, C26A, C25A, C24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3B, C28B, C29B, C30B, C31B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, C20A, C21A, C22A, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2B, C24B, C25B, C26B, C27B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1B, C20B, C21B, C22B, C23B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O1B)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=Sof(H21C)=Sof(H21D)=
 Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=Sof(H23D)=1-FVAR(1)
 Sof(O1A)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(H21A)=Sof(H21B)=
 Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C23A)=Sof(H23A)=Sof(H23B)=FVAR(1)
 Sof(O2B)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25C)=Sof(H25D)=
 Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(O3B)=Sof(C28B)=
 Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29C)=Sof(H29D)=Sof(C30B)=Sof(H30C)=
 Sof(H30D)=Sof(C31B)=Sof(H31C)=Sof(H31D)=1-FVAR(2)
 Sof(O2A)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=
 Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(O3A)=Sof(C31A)=
 Sof(H31A)=Sof(H31B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(C29A)=Sof(H29A)=
 Sof(H29B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=FVAR(2)
8.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C6(H6)
8.b Secondary CH2 refined with riding coordinates:
 C20A(H20A,H20B), C21A(H21A,H21B), C22A(H22A,H22B), C23A(H23A,H23B), C20B(H20C,
 H20D), C21B(H21C,H21D), C22B(H22C,H22D), C23B(H23C,H23D), C27A(H27A,H27B),
 C26A(H26A,H26B), C25A(H25A,H25B), C24A(H24A,H24B), C24B(H24C,H24D), C25B(H25C,
 H25D), C26B(H26C,H26D), C27B(H27C,H27D), C31A(H31A,H31B), C30A(H30A,H30B),
 C29A(H29A,H29B), C28A(H28A,H28B), C28B(H28C,H28D), C29B(H29C,H29D), C30B(H30C,
 H30D), C31B(H31C,H31D)
8.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C10(H10), C2(H2), C3(H3), C4(H4), C1(H1)
8.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C7(H7A,H7B,H7C), C19(H19A,H19B,
 H19C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Y1 Y 0.65710(2) 0.73359(2) 0.22822(2) 0.01639(8) Uani 1 1 d . . . . .
Mg1 Mg 1.000000 1.000000 0.500000 0.0144(2) Uani 1 2 d S . P . .
N2 N 0.5905(2) 0.60774(19) 0.15562(12) 0.0156(4) Uani 1 1 d . . . . .
C8 C 0.6179(2) 0.4712(2) 0.16934(14) 0.0149(5) Uani 1 1 d . . . . .
N1 N 0.4947(2) 0.8689(2) 0.13082(14) 0.0240(5) Uani 1 1 d . . . . .
C12 C 0.7663(3) 0.2474(3) 0.16002(16) 0.0217(5) Uani 1 1 d . . . . .
H12 H 0.851957 0.186353 0.144674 0.026 Uiso 1 1 calc R U . . .
C13 C 0.7449(2) 0.3796(2) 0.14535(15) 0.0179(5) Uani 1 1 d . . . . .
C11 C 0.6667(3) 0.2026(3) 0.19612(16) 0.0228(5) Uani 1 1 d . . . . .
H11 H 0.683201 0.112066 0.204855 0.027 Uiso 1 1 calc R U . . .
C10 C 0.5424(3) 0.2914(2) 0.21948(15) 0.0202(5) Uani 1 1 d . . . . .
H10 H 0.473670 0.260776 0.244458 0.024 Uiso 1 1 calc R U . . .
C14 C 0.3784(2) 0.5164(2) 0.23648(15) 0.0192(5) Uani 1 1 d . . . . .
H14 H 0.372995 0.606966 0.218133 0.023 Uiso 1 1 calc R U . . .
C17 C 0.8607(3) 0.4184(3) 0.10428(17) 0.0232(5) Uani 1 1 d . . . . .
H17 H 0.828229 0.515043 0.095242 0.028 Uiso 1 1 calc R U . . .
C9 C 0.5161(2) 0.4244(2) 0.20716(14) 0.0163(5) Uani 1 1 d . . . . .
C16 C 0.3623(3) 0.5096(3) 0.32903(17) 0.0269(6) Uani 1 1 d . . . . .
H16A H 0.370226 0.420829 0.348432 0.040 Uiso 1 1 calc R U . . .
H16B H 0.273023 0.569337 0.346445 0.040 Uiso 1 1 calc R U . . .
H16C H 0.433425 0.534302 0.351454 0.040 Uiso 1 1 calc R U . . .
C15 C 0.2614(3) 0.4878(3) 0.20114(18) 0.0273(6) Uani 1 1 d . . . . .
H15A H 0.271541 0.492884 0.141893 0.041 Uiso 1 1 calc R U . . .
H15B H 0.174937 0.551688 0.218972 0.041 Uiso 1 1 calc R U . . .
H15C H 0.262964 0.400424 0.219919 0.041 Uiso 1 1 calc R U . . .
C7 C 0.5809(3) 0.6169(3) 0.00521(17) 0.0310(6) Uani 1 1 d . . . . .
H7A H 0.517964 0.650251 -0.038371 0.046 Uiso 1 1 calc R U . . .
H7B H 0.617759 0.521938 0.005240 0.046 Uiso 1 1 calc R U . . .
H7C H 0.655345 0.652326 -0.003388 0.046 Uiso 1 1 calc R U . . .
C2 C 0.3431(3) 1.0710(3) 0.07485(19) 0.0316(6) Uani 1 1 d . . . . .
H2 H 0.310766 1.163262 0.072947 0.038 Uiso 1 1 calc R U . . .
C19 C 0.9842(3) 0.3791(3) 0.1572(2) 0.0343(7) Uani 1 1 d . . . . .
H19A H 0.956934 0.418977 0.209523 0.051 Uiso 1 1 calc R U . . .
H19B H 1.055347 0.408863 0.129914 0.051 Uiso 1 1 calc R U . . .
H19C H 1.019011 0.284355 0.165845 0.051 Uiso 1 1 calc R U . . .
C18 C 0.9064(3) 0.3584(3) 0.02180(19) 0.0331(7) Uani 1 1 d . . . . .
H18A H 0.945002 0.263734 0.029621 0.050 Uiso 1 1 calc R U . . .
H18B H 0.975226 0.392040 -0.004835 0.050 Uiso 1 1 calc R U . . .
H18C H 0.828166 0.381128 -0.012078 0.050 Uiso 1 1 calc R U . . .
C3 C 0.2892(3) 1.0038(3) 0.02734(19) 0.0342(7) Uani 1 1 d . . . . .
H3 H 0.219095 1.049070 -0.007918 0.041 Uiso 1 1 calc R U . . .
C6 C 0.5059(3) 0.6578(3) 0.08616(16) 0.0242(6) Uani 1 1 d . . . . .
H6 H 0.429837 0.621522 0.092562 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3397(3) 0.8687(3) 0.03223(18) 0.0310(6) Uani 1 1 d . . . . .
H4 H 0.303793 0.820663 0.000462 0.037 Uiso 1 1 calc R U . . .
C5 C 0.4432(3) 0.8043(3) 0.08388(16) 0.0224(5) Uani 1 1 d . . . . .
C1 C 0.4454(3) 1.0004(3) 0.12536(19) 0.0295(6) Uani 1 1 d . . . . .
H1 H 0.482738 1.046632 0.157684 0.035 Uiso 1 1 calc R U . . .
B2 B 0.4985(4) 0.9315(4) 0.3252(2) 0.0329(7) Uani 1 1 d . . . . .
B3 B 0.8565(3) 0.7878(4) 0.1566(2) 0.0316(7) Uani 1 1 d D . . . .
B1 B 0.7322(4) 0.5829(4) 0.3520(2) 0.0356(8) Uani 1 1 d . . . . .
H2A H 0.528(4) 0.908(4) 0.391(2) 0.041(10) Uiso 1 1 d . . . . .
H1A H 0.620(4) 0.613(4) 0.342(2) 0.045(10) Uiso 1 1 d . . . . .
H1B H 0.787(4) 0.540(4) 0.296(2) 0.044(10) Uiso 1 1 d . . . . .
H1C H 0.760(4) 0.674(4) 0.350(3) 0.064(13) Uiso 1 1 d . . . . .
H2B H 0.472(4) 0.855(4) 0.302(2) 0.049(11) Uiso 1 1 d . . . . .
H2C H 0.596(4) 0.928(3) 0.287(2) 0.038(9) Uiso 1 1 d . . . . .
H2D H 0.409(4) 1.028(4) 0.307(2) 0.045(10) Uiso 1 1 d . . . . .
H1D H 0.760(4) 0.522(4) 0.407(2) 0.051(11) Uiso 1 1 d . . . . .
O1A O 1.03756(18) 0.95900(18) 0.37712(11) 0.0209(4) Uani 0.736(3) 1 d D U P A 1
C20A C 1.0801(4) 1.0442(4) 0.3150(2) 0.0269(4) Uani 0.736(3) 1 d D U P A 1
H20A H 1.163465 1.057895 0.330439 0.032 Uiso 0.736(3) 1 calc R U P A 1
H20B H 1.007585 1.129695 0.309221 0.032 Uiso 0.736(3) 1 calc R U P A 1
C21A C 1.1064(5) 0.9749(4) 0.2365(2) 0.0269(4) Uani 0.736(3) 1 d D U P A 1
H21A H 1.187301 0.984278 0.205528 0.032 Uiso 0.736(3) 1 calc R U P A 1
H21B H 1.027135 1.008593 0.202338 0.032 Uiso 0.736(3) 1 calc R U P A 1
C22A C 1.1303(4) 0.8339(4) 0.2652(2) 0.0269(4) Uani 0.736(3) 1 d D U P A 1
H22A H 1.110450 0.784511 0.223037 0.032 Uiso 0.736(3) 1 calc R U P A 1
H22B H 1.224469 0.790032 0.281674 0.032 Uiso 0.736(3) 1 calc R U P A 1
C23A C 1.0294(4) 0.8508(4) 0.3367(2) 0.0269(4) Uani 0.736(3) 1 d D U P A 1
H23A H 0.936588 0.868939 0.318542 0.032 Uiso 0.736(3) 1 calc R U P A 1
H23B H 1.053107 0.771538 0.373174 0.032 Uiso 0.736(3) 1 calc R U P A 1
O1B O 1.03756(18) 0.95900(18) 0.37712(11) 0.0209(4) Uani 0.264(3) 1 d D U P A 2
C20B C 0.9509(9) 0.9949(11) 0.3118(5) 0.0269(4) Uani 0.264(3) 1 d D U P A 2
H20C H 0.888627 1.085521 0.315430 0.032 Uiso 0.264(3) 1 calc R U P A 2
H20D H 0.896450 0.936806 0.311176 0.032 Uiso 0.264(3) 1 calc R U P A 2
C21B C 1.0459(11) 0.9811(10) 0.2363(6) 0.0269(4) Uani 0.264(3) 1 d D U P A 2
H21C H 1.002336 0.969061 0.187939 0.032 Uiso 0.264(3) 1 calc R U P A 2
H21D H 1.076220 1.057397 0.226007 0.032 Uiso 0.264(3) 1 calc R U P A 2
C22B C 1.1625(11) 0.8601(11) 0.2591(6) 0.0269(4) Uani 0.264(3) 1 d D U P A 2
H22C H 1.247684 0.859225 0.228675 0.032 Uiso 0.264(3) 1 calc R U P A 2
H22D H 1.142881 0.780808 0.248198 0.032 Uiso 0.264(3) 1 calc R U P A 2
C23B C 1.1729(9) 0.8690(10) 0.3495(5) 0.0269(4) Uani 0.264(3) 1 d D U P A 2
H23C H 1.192415 0.782576 0.377994 0.032 Uiso 0.264(3) 1 calc R U P A 2
H23D H 1.245569 0.904022 0.359355 0.032 Uiso 0.264(3) 1 calc R U P A 2
O2A O 0.93507(18) 0.83930(18) 0.52381(12) 0.0236(4) Uani 0.739(2) 1 d D U P A 3
C27A C 0.7930(4) 0.8443(4) 0.5129(3) 0.0359(5) Uani 0.739(2) 1 d D U P A 3
H27A H 0.776597 0.846553 0.454731 0.043 Uiso 0.739(2) 1 calc R U P A 3
H27B H 0.726626 0.922278 0.537004 0.043 Uiso 0.739(2) 1 calc R U P A 3
C26A C 0.7810(4) 0.7229(4) 0.5557(3) 0.0359(5) Uani 0.739(2) 1 d D U P A 3
H26A H 0.774411 0.662469 0.515933 0.043 Uiso 0.739(2) 1 calc R U P A 3
H26B H 0.698606 0.744119 0.592573 0.043 Uiso 0.739(2) 1 calc R U P A 3
C25A C 0.9070(4) 0.6611(4) 0.6034(3) 0.0359(5) Uani 0.739(2) 1 d D U P A 3
H25A H 0.934402 0.565160 0.606520 0.043 Uiso 0.739(2) 1 calc R U P A 3
H25B H 0.893984 0.692975 0.658732 0.043 Uiso 0.739(2) 1 calc R U P A 3
C24A C 1.0113(4) 0.7094(4) 0.5502(3) 0.0359(5) Uani 0.739(2) 1 d D U P A 3
H24A H 1.087642 0.708212 0.582360 0.043 Uiso 0.739(2) 1 calc R U P A 3
H24B H 1.047920 0.654435 0.503453 0.043 Uiso 0.739(2) 1 calc R U P A 3
O2B O 0.93507(18) 0.83930(18) 0.52381(12) 0.0236(4) Uani 0.261(2) 1 d D U P A 4
C24B C 0.9306(13) 0.7395(10) 0.4745(6) 0.0359(5) Uani 0.261(2) 1 d D U P A 4
H24C H 1.014243 0.709036 0.439098 0.043 Uiso 0.261(2) 1 calc R U P A 4
H24D H 0.851259 0.771497 0.440305 0.043 Uiso 0.261(2) 1 calc R U P A 4
C25B C 0.9184(12) 0.6280(10) 0.5356(7) 0.0359(5) Uani 0.261(2) 1 d D U P A 4
H25C H 0.877330 0.570840 0.511671 0.043 Uiso 0.261(2) 1 calc R U P A 4
H25D H 1.006902 0.575243 0.557291 0.043 Uiso 0.261(2) 1 calc R U P A 4
C26B C 0.8245(13) 0.7109(11) 0.5983(7) 0.0359(5) Uani 0.261(2) 1 d D U P A 4
H26C H 0.810122 0.660110 0.647836 0.043 Uiso 0.261(2) 1 calc R U P A 4
H26D H 0.736172 0.765053 0.576956 0.043 Uiso 0.261(2) 1 calc R U P A 4
C27B C 0.9188(12) 0.7910(11) 0.6106(6) 0.0359(5) Uani 0.261(2) 1 d D U P A 4
H27C H 0.874584 0.863446 0.646624 0.043 Uiso 0.261(2) 1 calc R U P A 4
H27D H 1.006607 0.735804 0.632014 0.043 Uiso 0.261(2) 1 calc R U P A 4
O3A O 0.80429(17) 1.11750(19) 0.47511(11) 0.0216(4) Uani 0.739(2) 1 d D U P A 5
C31A C 0.7366(4) 1.1303(4) 0.4015(2) 0.0270(4) Uani 0.739(2) 1 d D U P A 5
H31A H 0.758824 1.044871 0.377626 0.032 Uiso 0.739(2) 1 calc R U P A 5
H31B H 0.763261 1.190134 0.361507 0.032 Uiso 0.739(2) 1 calc R U P A 5
C30A C 0.5868(4) 1.1848(4) 0.4260(2) 0.0270(4) Uani 0.739(2) 1 d D U P A 5
H30A H 0.551681 1.115867 0.449267 0.032 Uiso 0.739(2) 1 calc R U P A 5
H30B H 0.532762 1.230808 0.379688 0.032 Uiso 0.739(2) 1 calc R U P A 5
C29A C 0.5863(5) 1.2792(5) 0.4902(3) 0.0270(4) Uani 0.739(2) 1 d D U P A 5
H29A H 0.591294 1.362197 0.464713 0.032 Uiso 0.739(2) 1 calc R U P A 5
H29B H 0.504080 1.297297 0.527073 0.032 Uiso 0.739(2) 1 calc R U P A 5
C28A C 0.7118(4) 1.2065(4) 0.5341(2) 0.0270(4) Uani 0.739(2) 1 d D U P A 5
H28A H 0.754310 1.267175 0.552035 0.032 Uiso 0.739(2) 1 calc R U P A 5
H28B H 0.689832 1.156638 0.582111 0.032 Uiso 0.739(2) 1 calc R U P A 5
O3B O 0.80429(17) 1.11750(19) 0.47511(11) 0.0216(4) Uani 0.261(2) 1 d D U P A 6
C28B C 0.7434(9) 1.2508(9) 0.4541(6) 0.0270(4) Uani 0.261(2) 1 d D U P A 6
H28C H 0.758007 1.268229 0.395345 0.032 Uiso 0.261(2) 1 calc R U P A 6
H28D H 0.782784 1.303249 0.484033 0.032 Uiso 0.261(2) 1 calc R U P A 6
C29B C 0.5931(12) 1.2844(13) 0.4769(9) 0.0270(4) Uani 0.261(2) 1 d D U P A 6
H29C H 0.574037 1.295540 0.535774 0.032 Uiso 0.261(2) 1 calc R U P A 6
H29D H 0.538631 1.364307 0.446901 0.032 Uiso 0.261(2) 1 calc R U P A 6
C30B C 0.5657(10) 1.1662(10) 0.4516(7) 0.0270(4) Uani 0.261(2) 1 d D U P A 6
H30C H 0.547982 1.173941 0.393295 0.032 Uiso 0.261(2) 1 calc R U P A 6
H30D H 0.487219 1.153372 0.483488 0.032 Uiso 0.261(2) 1 calc R U P A 6
C31B C 0.6958(9) 1.0559(9) 0.4693(7) 0.0270(4) Uani 0.261(2) 1 d D U P A 6
H31C H 0.721050 0.994384 0.425270 0.032 Uiso 0.261(2) 1 calc R U P A 6
H31D H 0.684327 1.008219 0.520800 0.032 Uiso 0.261(2) 1 calc R U P A 6
H3A H 0.898(3) 0.724(2) 0.2150(14) 0.013(6) Uiso 1 1 d D . . . .
H3B H 0.949(3) 0.816(4) 0.128(2) 0.058(12) Uiso 1 1 d D . . . .
H3C H 0.782(4) 0.881(3) 0.185(3) 0.073(14) Uiso 1 1 d D . . . .
H3D H 0.782(5) 0.769(6) 0.113(3) 0.12(2) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Y1 N2 2.205(2) . ?
Y1 N1 2.460(2) . ?
Y1 B2 2.780(3) . ?
Y1 B3 2.550(3) . ?
Y1 B1 2.534(4) . ?
Y1 H1A 2.30(4) . ?
Y1 H1B 2.36(4) . ?
Y1 H1C 2.30(4) . ?
Y1 H2B 2.28(4) . ?
Y1 H2C 2.28(4) . ?
Y1 H3A 2.48(3) . ?
Y1 H3C 2.44(5) . ?
Y1 H3D 2.32(6) . ?
Mg1 O1A 2.0990(17) 2_776 ?
Mg1 O1A 2.0990(17) . ?
Mg1 O1B 2.0990(17) . ?
Mg1 O2A 2.0956(18) . ?
Mg1 O2A 2.0956(18) 2_776 ?
Mg1 O2B 2.0956(18) . ?
Mg1 O3A 2.0726(17) . ?
Mg1 O3A 2.0726(17) 2_776 ?
Mg1 O3B 2.0726(17) . ?
N2 C8 1.429(3) . ?
N2 C6 1.464(3) . ?
C8 C13 1.418(3) . ?
C8 C9 1.422(3) . ?
N1 C5 1.343(4) . ?
N1 C1 1.355(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.395(4) . ?
C12 C11 1.378(4) . ?
C13 C17 1.518(3) . ?
C11 H11 0.9500 . ?
C11 C10 1.384(4) . ?
C10 H10 0.9500 . ?
C10 C9 1.391(3) . ?
C14 H14 1.0000 . ?
C14 C9 1.522(3) . ?
C14 C16 1.531(4) . ?
C14 C15 1.530(4) . ?
C17 H17 1.0000 . ?
C17 C19 1.539(4) . ?
C17 C18 1.534(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 C6 1.521(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(5) . ?
C2 C1 1.389(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C3 H3 0.9500 . ?
C3 C4 1.391(4) . ?
C6 H6 1.0000 . ?
C6 C5 1.513(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.393(4) . ?
C1 H1 0.9500 . ?
B2 H2A 1.14(4) . ?
B2 H2B 1.07(4) . ?
B2 H2C 1.15(4) . ?
B2 H2D 1.19(4) . ?
B3 H3A 1.17(2) . ?
B3 H3B 1.17(2) . ?
B3 H3C 1.17(2) . ?
B3 H3D 1.18(2) . ?
B1 H1A 1.13(4) . ?
B1 H1B 1.10(4) . ?
B1 H1C 1.13(5) . ?
B1 H1D 1.08(4) . ?
O1A C20A 1.484(4) . ?
O1A C23A 1.435(4) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
C20A C21A 1.517(5) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C21A C22A 1.524(5) . ?
C22A H22A 0.9900 . ?
C22A H22B 0.9900 . ?
C22A C23A 1.507(5) . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
O1B C20B 1.413(9) . ?
O1B C23B 1.489(9) . ?
C20B H20C 0.9900 . ?
C20B H20D 0.9900 . ?
C20B C21B 1.524(10) . ?
C21B H21C 0.9900 . ?
C21B H21D 0.9900 . ?
C21B C22B 1.514(10) . ?
C22B H22C 0.9900 . ?
C22B H22D 0.9900 . ?
C22B C23B 1.524(10) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
O2A C27A 1.496(4) . ?
O2A C24A 1.430(4) . ?
C27A H27A 0.9900 . ?
C27A H27B 0.9900 . ?
C27A C26A 1.500(5) . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
C26A C25A 1.516(6) . ?
C25A H25A 0.9900 . ?
C25A H25B 0.9900 . ?
C25A C24A 1.560(5) . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
O2B C24B 1.428(10) . ?
O2B C27B 1.515(10) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
C24B C25B 1.563(11) . ?
C25B H25C 0.9900 . ?
C25B H25D 0.9900 . ?
C25B C26B 1.502(11) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
C26B C27B 1.560(11) . ?
C27B H27C 0.9900 . ?
C27B H27D 0.9900 . ?
O3A C31A 1.432(4) . ?
O3A C28A 1.485(4) . ?
C31A H31A 0.9900 . ?
C31A H31B 0.9900 . ?
C31A C30A 1.515(5) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
C30A C29A 1.536(6) . ?
C29A H29A 0.9900 . ?
C29A H29B 0.9900 . ?
C29A C28A 1.498(6) . ?
C28A H28A 0.9900 . ?
C28A H28B 0.9900 . ?
O3B C28B 1.411(9) . ?
O3B C31B 1.519(9) . ?
C28B H28C 0.9900 . ?
C28B H28D 0.9900 . ?
C28B C29B 1.517(11) . ?
C29B H29C 0.9900 . ?
C29B H29D 0.9900 . ?
C29B C30B 1.513(12) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C30B C31B 1.515(10) . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?

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
N2 Y1 N1 70.59(8) . . ?
N2 Y1 B2 128.22(10) . . ?
N2 Y1 B3 111.11(10) . . ?
N2 Y1 B1 99.90(10) . . ?
N2 Y1 H1A 87.9(9) . . ?
N2 Y1 H1B 85.8(9) . . ?
N2 Y1 H1C 126.0(12) . . ?
N2 Y1 H2B 107.4(10) . . ?
N2 Y1 H2C 145.7(9) . . ?
N2 Y1 H3A 119.5(6) . . ?
N2 Y1 H3C 129.5(9) . . ?
N2 Y1 H3D 86.8(9) . . ?
N1 Y1 B2 79.27(10) . . ?
N1 Y1 B3 93.21(10) . . ?
N1 Y1 B1 155.91(12) . . ?
N1 Y1 H1A 129.5(10) . . ?
N1 Y1 H1B 156.3(9) . . ?
N1 Y1 H1C 157.3(11) . . ?
N1 Y1 H2B 73.4(10) . . ?
N1 Y1 H2C 80.4(9) . . ?
N1 Y1 H3A 120.0(5) . . ?
N1 Y1 H3C 83.1(10) . . ?
N1 Y1 H3D 72.6(11) . . ?
B2 Y1 H1A 79.9(9) . . ?
B2 Y1 H1B 116.4(9) . . ?
B2 Y1 H1C 78.0(11) . . ?
B2 Y1 H2B 21.6(10) . . ?
B2 Y1 H2C 23.7(9) . . ?
B2 Y1 H3A 111.9(6) . . ?
B2 Y1 H3C 85.3(6) . . ?
B2 Y1 H3D 123.1(15) . . ?
B3 Y1 B2 111.68(11) . . ?
B3 Y1 H1A 137.3(10) . . ?
B3 Y1 H1B 96.7(9) . . ?
B3 Y1 H1C 94.0(11) . . ?
B3 Y1 H2B 131.9(10) . . ?
B3 Y1 H2C 88.0(9) . . ?
B3 Y1 H3A 26.9(5) . . ?
B3 Y1 H3C 26.9(6) . . ?
B3 Y1 H3D 27.6(6) . . ?
B1 Y1 B2 90.86(12) . . ?
B1 Y1 B3 110.87(13) . . ?
B1 Y1 H1A 26.4(9) . . ?
B1 Y1 H1B 25.7(9) . . ?
B1 Y1 H1C 26.5(11) . . ?
B1 Y1 H2B 89.3(10) . . ?
B1 Y1 H2C 99.3(9) . . ?
B1 Y1 H3A 84.0(5) . . ?
B1 Y1 H3C 118.2(11) . . ?
B1 Y1 H3D 130.2(13) . . ?
H1A Y1 H1B 45.2(13) . . ?
H1A Y1 H1C 46.6(14) . . ?
H1A Y1 H2B 70.4(14) . . ?
H1A Y1 H2C 97.0(13) . . ?
H1A Y1 H3A 110.4(11) . . ?
H1A Y1 H3C 139.7(15) . . ?
H1A Y1 H3D 153.4(18) . . ?
H1B Y1 H1C 43.0(14) . . ?
H1B Y1 H2B 114.1(13) . . ?
H1B Y1 H2C 121.3(13) . . ?
H1B Y1 H3A 72.5(10) . . ?
H1B Y1 H3C 114.4(13) . . ?
H1B Y1 H3D 108.4(17) . . ?
H1C Y1 H2B 85.8(15) . . ?
H1C Y1 H2C 78.3(14) . . ?
H1C Y1 H3A 68.4(12) . . ?
H1C Y1 H3C 93.8(16) . . ?
H1C Y1 H3D 119.8(14) . . ?
H2B Y1 H2C 44.8(13) . . ?
H2B Y1 H3A 133.1(12) . . ?
H2B Y1 H3C 105.0(11) . . ?
H2B Y1 H3D 135.8(18) . . ?
H2C Y1 H3A 90.6(11) . . ?
H2C Y1 H3C 61.8(11) . . ?
H2C Y1 H3D 102.0(16) . . ?
H3A Y1 H3C 42.9(11) . . ?
H3A Y1 H3D 51.5(11) . . ?
H3C Y1 H3D 43.7(14) . . ?
O1A Mg1 O1A 180.00(2) 2_776 . ?
O2A Mg1 O2A 180.0 2_776 . ?
O3A Mg1 O3A 180.00(11) 2_776 . ?
C8 N2 Y1 126.63(15) . . ?
C8 N2 C6 110.65(19) . . ?
C6 N2 Y1 122.69(15) . . ?
C13 C8 N2 121.6(2) . . ?
C13 C8 C9 118.5(2) . . ?
C9 C8 N2 119.9(2) . . ?
C5 N1 Y1 115.58(17) . . ?
C5 N1 C1 118.1(2) . . ?
C1 N1 Y1 126.1(2) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C11 C12 C13 121.9(2) . . ?
C8 C13 C17 123.0(2) . . ?
C12 C13 C8 119.3(2) . . ?
C12 C13 C17 117.7(2) . . ?
C12 C11 H11 120.4 . . ?
C12 C11 C10 119.2(2) . . ?
C10 C11 H11 120.4 . . ?
C11 C10 H10 119.3 . . ?
C11 C10 C9 121.4(2) . . ?
C9 C10 H10 119.3 . . ?
C9 C14 H14 108.1 . . ?
C9 C14 C16 110.9(2) . . ?
C9 C14 C15 111.8(2) . . ?
C16 C14 H14 108.1 . . ?
C15 C14 H14 108.1 . . ?
C15 C14 C16 109.6(2) . . ?
C13 C17 H17 108.1 . . ?
C13 C17 C19 111.7(2) . . ?
C13 C17 C18 112.0(2) . . ?
C19 C17 H17 108.1 . . ?
C18 C17 H17 108.1 . . ?
C18 C17 C19 108.7(2) . . ?
C8 C9 C14 121.7(2) . . ?
C10 C9 C8 119.8(2) . . ?
C10 C9 C14 118.5(2) . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
C3 C2 H2 120.8 . . ?
C3 C2 C1 118.4(3) . . ?
C1 C2 H2 120.8 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.7(3) . . ?
C4 C3 H3 120.6 . . ?
N2 C6 C7 113.5(2) . . ?
N2 C6 H6 107.4 . . ?
N2 C6 C5 111.8(2) . . ?
C7 C6 H6 107.4 . . ?
C5 C6 C7 109.0(2) . . ?
C5 C6 H6 107.4 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C6 117.6(2) . . ?
N1 C5 C4 121.8(3) . . ?
C4 C5 C6 120.6(2) . . ?
N1 C1 C2 123.2(3) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
Y1 B2 H2A 110.4(18) . . ?
Y1 B2 H2B 52(2) . . ?
Y1 B2 H2C 53.0(18) . . ?
Y1 B2 H2D 129.2(18) . . ?
H2A B2 H2B 111(3) . . ?
H2A B2 H2C 107(3) . . ?
H2A B2 H2D 120(3) . . ?
H2B B2 H2C 103(3) . . ?
H2B B2 H2D 105(3) . . ?
H2C B2 H2D 110(3) . . ?
Y1 B3 H3A 73.4(13) . . ?
Y1 B3 H3B 176(2) . . ?
Y1 B3 H3C 71(2) . . ?
Y1 B3 H3D 65(3) . . ?
H3A B3 H3B 104(2) . . ?
H3A B3 H3C 101(3) . . ?
H3A B3 H3D 125(3) . . ?
H3B B3 H3C 106(3) . . ?
H3B B3 H3D 119(4) . . ?
H3C B3 H3D 98(4) . . ?
Y1 B1 H1A 65.2(19) . . ?
Y1 B1 H1B 68.2(19) . . ?
Y1 B1 H1C 65(2) . . ?
Y1 B1 H1D 177(2) . . ?
H1A B1 H1B 107(3) . . ?
H1A B1 H1C 107(3) . . ?
H1A B1 H1D 113(3) . . ?
H1B B1 H1C 100(3) . . ?
H1B B1 H1D 115(3) . . ?
H1C B1 H1D 114(3) . . ?
C20A O1A Mg1 123.24(18) . . ?
C23A O1A Mg1 129.45(19) . . ?
C23A O1A C20A 107.3(2) . . ?
O1A C20A H20A 110.5 . . ?
O1A C20A H20B 110.5 . . ?
O1A C20A C21A 106.3(3) . . ?
H20A C20A H20B 108.7 . . ?
C21A C20A H20A 110.5 . . ?
C21A C20A H20B 110.5 . . ?
C20A C21A H21A 111.2 . . ?
C20A C21A H21B 111.2 . . ?
C20A C21A C22A 103.0(3) . . ?
H21A C21A H21B 109.1 . . ?
C22A C21A H21A 111.2 . . ?
C22A C21A H21B 111.2 . . ?
C21A C22A H22A 111.6 . . ?
C21A C22A H22B 111.6 . . ?
H22A C22A H22B 109.4 . . ?
C23A C22A C21A 101.1(3) . . ?
C23A C22A H22A 111.6 . . ?
C23A C22A H22B 111.6 . . ?
O1A C23A C22A 105.3(3) . . ?
O1A C23A H23A 110.7 . . ?
O1A C23A H23B 110.7 . . ?
C22A C23A H23A 110.7 . . ?
C22A C23A H23B 110.7 . . ?
H23A C23A H23B 108.8 . . ?
C20B O1B Mg1 131.1(4) . . ?
C20B O1B C23B 109.6(5) . . ?
C23B O1B Mg1 119.1(4) . . ?
O1B C20B H20C 110.8 . . ?
O1B C20B H20D 110.8 . . ?
O1B C20B C21B 104.9(7) . . ?
H20C C20B H20D 108.8 . . ?
C21B C20B H20C 110.8 . . ?
C21B C20B H20D 110.8 . . ?
C20B C21B H21C 111.4 . . ?
C20B C21B H21D 111.4 . . ?
H21C C21B H21D 109.3 . . ?
C22B C21B C20B 101.6(7) . . ?
C22B C21B H21C 111.4 . . ?
C22B C21B H21D 111.4 . . ?
C21B C22B H22C 110.9 . . ?
C21B C22B H22D 110.9 . . ?
C21B C22B C23B 104.0(7) . . ?
H22C C22B H22D 109.0 . . ?
C23B C22B H22C 110.9 . . ?
C23B C22B H22D 110.9 . . ?
O1B C23B C22B 104.7(6) . . ?
O1B C23B H23C 110.8 . . ?
O1B C23B H23D 110.8 . . ?
C22B C23B H23C 110.8 . . ?
C22B C23B H23D 110.8 . . ?
H23C C23B H23D 108.9 . . ?
C27A O2A Mg1 123.1(2) . . ?
C24A O2A Mg1 129.1(2) . . ?
C24A O2A C27A 107.8(3) . . ?
O2A C27A H27A 110.6 . . ?
O2A C27A H27B 110.6 . . ?
O2A C27A C26A 105.5(3) . . ?
H27A C27A H27B 108.8 . . ?
C26A C27A H27A 110.6 . . ?
C26A C27A H27B 110.6 . . ?
C27A C26A H26A 110.2 . . ?
C27A C26A H26B 110.2 . . ?
C27A C26A C25A 107.3(3) . . ?
H26A C26A H26B 108.5 . . ?
C25A C26A H26A 110.2 . . ?
C25A C26A H26B 110.2 . . ?
C26A C25A H25A 111.7 . . ?
C26A C25A H25B 111.7 . . ?
C26A C25A C24A 100.4(3) . . ?
H25A C25A H25B 109.5 . . ?
C24A C25A H25A 111.7 . . ?
C24A C25A H25B 111.7 . . ?
O2A C24A C25A 104.5(3) . . ?
O2A C24A H24A 110.9 . . ?
O2A C24A H24B 110.9 . . ?
C25A C24A H24A 110.9 . . ?
C25A C24A H24B 110.9 . . ?
H24A C24A H24B 108.9 . . ?
C24B O2B Mg1 132.7(4) . . ?
C24B O2B C27B 106.0(6) . . ?
C27B O2B Mg1 119.4(4) . . ?
O2B C24B H24C 110.7 . . ?
O2B C24B H24D 110.7 . . ?
O2B C24B C25B 105.0(7) . . ?
H24C C24B H24D 108.8 . . ?
C25B C24B H24C 110.7 . . ?
C25B C24B H24D 110.7 . . ?
C24B C25B H25C 112.2 . . ?
C24B C25B H25D 112.2 . . ?
H25C C25B H25D 109.8 . . ?
C26B C25B C24B 98.0(8) . . ?
C26B C25B H25C 112.2 . . ?
C26B C25B H25D 112.2 . . ?
C25B C26B H26C 112.8 . . ?
C25B C26B H26D 112.8 . . ?
C25B C26B C27B 94.7(8) . . ?
H26C C26B H26D 110.2 . . ?
C27B C26B H26C 112.8 . . ?
C27B C26B H26D 112.8 . . ?
O2B C27B C26B 99.2(7) . . ?
O2B C27B H27C 111.9 . . ?
O2B C27B H27D 111.9 . . ?
C26B C27B H27C 111.9 . . ?
C26B C27B H27D 111.9 . . ?
H27C C27B H27D 109.6 . . ?
C31A O3A Mg1 127.86(18) . . ?
C31A O3A C28A 109.0(2) . . ?
C28A O3A Mg1 123.15(17) . . ?
O3A C31A H31A 110.8 . . ?
O3A C31A H31B 110.8 . . ?
O3A C31A C30A 104.8(3) . . ?
H31A C31A H31B 108.9 . . ?
C30A C31A H31A 110.8 . . ?
C30A C31A H31B 110.8 . . ?
C31A C30A H30A 111.5 . . ?
C31A C30A H30B 111.5 . . ?
C31A C30A C29A 101.4(3) . . ?
H30A C30A H30B 109.3 . . ?
C29A C30A H30A 111.5 . . ?
C29A C30A H30B 111.5 . . ?
C30A C29A H29A 111.2 . . ?
C30A C29A H29B 111.2 . . ?
H29A C29A H29B 109.2 . . ?
C28A C29A C30A 102.6(4) . . ?
C28A C29A H29A 111.2 . . ?
C28A C29A H29B 111.2 . . ?
O3A C28A C29A 105.8(3) . . ?
O3A C28A H28A 110.6 . . ?
O3A C28A H28B 110.6 . . ?
C29A C28A H28A 110.6 . . ?
C29A C28A H28B 110.6 . . ?
H28A C28A H28B 108.7 . . ?
C28B O3B Mg1 134.1(4) . . ?
C28B O3B C31B 106.3(6) . . ?
C31B O3B Mg1 119.3(4) . . ?
O3B C28B H28C 110.4 . . ?
O3B C28B H28D 110.4 . . ?
O3B C28B C29B 106.4(8) . . ?
H28C C28B H28D 108.6 . . ?
C29B C28B H28C 110.4 . . ?
C29B C28B H28D 110.4 . . ?
C28B C29B H29C 111.4 . . ?
C28B C29B H29D 111.4 . . ?
H29C C29B H29D 109.3 . . ?
C30B C29B C28B 101.7(8) . . ?
C30B C29B H29C 111.4 . . ?
C30B C29B H29D 111.4 . . ?
C29B C30B H30C 111.1 . . ?
C29B C30B H30D 111.1 . . ?
C29B C30B C31B 103.4(8) . . ?
H30C C30B H30D 109.1 . . ?
C31B C30B H30C 111.1 . . ?
C31B C30B H30D 111.1 . . ?
O3B C31B H31C 110.4 . . ?
O3B C31B H31D 110.4 . . ?
C30B C31B O3B 106.4(7) . . ?
C30B C31B H31C 110.4 . . ?
C30B C31B H31D 110.4 . . ?
H31C C31B H31D 108.6 . . ?

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
Y1 N2 C8 C13 -79.2(3) . . . . ?
Y1 N2 C8 C9 101.4(2) . . . . ?
Y1 N2 C6 C7 109.7(2) . . . . ?
Y1 N2 C6 C5 -14.1(3) . . . . ?
Y1 N1 C5 C6 -9.5(3) . . . . ?
Y1 N1 C5 C4 173.1(2) . . . . ?
Y1 N1 C1 C2 -172.9(2) . . . . ?
Mg1 O1A C20A C21A 175.8(2) . . . . ?
Mg1 O1A C23A C22A -151.5(2) . . . . ?
Mg1 O1B C20B C21B 159.1(5) . . . . ?
Mg1 O1B C23B C22B 178.8(6) . . . . ?
Mg1 O2A C27A C26A -166.0(3) . . . . ?
Mg1 O2A C24A C25A 147.8(2) . . . . ?
Mg1 O2B C24B C25B 161.3(5) . . . . ?
Mg1 O2B C27B C26B 160.9(6) . . . . ?
Mg1 O3A C31A C30A 159.0(2) . . . . ?
Mg1 O3A C28A C29A 175.9(3) . . . . ?
Mg1 O3B C28B C29B -157.8(6) . . . . ?
Mg1 O3B C31B C30B 179.5(6) . . . . ?
N2 C8 C13 C12 -179.8(2) . . . . ?
N2 C8 C13 C17 0.4(4) . . . . ?
N2 C8 C9 C10 179.1(2) . . . . ?
N2 C8 C9 C14 -2.1(3) . . . . ?
N2 C6 C5 N1 14.9(3) . . . . ?
N2 C6 C5 C4 -167.7(2) . . . . ?
C8 N2 C6 C7 -71.9(3) . . . . ?
C8 N2 C6 C5 164.2(2) . . . . ?
C8 C13 C17 C19 115.4(3) . . . . ?
C8 C13 C17 C18 -122.4(3) . . . . ?
C12 C13 C17 C19 -64.4(3) . . . . ?
C12 C13 C17 C18 57.8(3) . . . . ?
C12 C11 C10 C9 0.1(4) . . . . ?
C13 C8 C9 C10 -0.2(3) . . . . ?
C13 C8 C9 C14 178.5(2) . . . . ?
C13 C12 C11 C10 -0.8(4) . . . . ?
C11 C12 C13 C8 1.0(4) . . . . ?
C11 C12 C13 C17 -179.2(2) . . . . ?
C11 C10 C9 C8 0.4(4) . . . . ?
C11 C10 C9 C14 -178.4(2) . . . . ?
C9 C8 C13 C12 -0.5(3) . . . . ?
C9 C8 C13 C17 179.8(2) . . . . ?
C16 C14 C9 C8 -111.6(3) . . . . ?
C16 C14 C9 C10 67.1(3) . . . . ?
C15 C14 C9 C8 125.7(3) . . . . ?
C15 C14 C9 C10 -55.6(3) . . . . ?
C7 C6 C5 N1 -111.5(3) . . . . ?
C7 C6 C5 C4 66.0(3) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C3 C2 C1 N1 -0.4(4) . . . . ?
C3 C4 C5 N1 1.3(4) . . . . ?
C3 C4 C5 C6 -176.0(3) . . . . ?
C6 N2 C8 C13 102.5(3) . . . . ?
C6 N2 C8 C9 -76.8(3) . . . . ?
C5 N1 C1 C2 1.2(4) . . . . ?
C1 N1 C5 C6 175.8(2) . . . . ?
C1 N1 C5 C4 -1.6(4) . . . . ?
C1 C2 C3 C4 0.0(4) . . . . ?
O1A C20A C21A C22A -21.3(4) . . . . ?
C20A O1A C23A C22A 28.3(4) . . . . ?
C20A C21A C22A C23A 37.1(4) . . . . ?
C21A C22A C23A O1A -40.9(4) . . . . ?
C23A O1A C20A C21A -4.0(4) . . . . ?
O1B C20B C21B C22B 38.3(11) . . . . ?
C20B O1B C23B C22B 3.3(10) . . . . ?
C20B C21B C22B C23B -35.6(12) . . . . ?
C21B C22B C23B O1B 20.9(11) . . . . ?
C23B O1B C20B C21B -26.1(10) . . . . ?
O2A C27A C26A C25A 9.9(5) . . . . ?
C27A O2A C24A C25A -33.6(4) . . . . ?
C27A C26A C25A C24A -28.6(5) . . . . ?
C26A C25A C24A O2A 37.9(4) . . . . ?
C24A O2A C27A C26A 15.2(4) . . . . ?
O2B C24B C25B C26B 38.5(11) . . . . ?
C24B O2B C27B C26B -32.5(10) . . . . ?
C24B C25B C26B C27B -55.9(10) . . . . ?
C25B C26B C27B O2B 55.3(10) . . . . ?
C27B O2B C24B C25B -2.8(10) . . . . ?
O3A C31A C30A C29A 37.7(4) . . . . ?
C31A O3A C28A C29A -2.9(4) . . . . ?
C31A C30A C29A C28A -38.8(4) . . . . ?
C30A C29A C28A O3A 26.2(4) . . . . ?
C28A O3A C31A C30A -22.2(4) . . . . ?
O3B C28B C29B C30B -40.1(12) . . . . ?
C28B O3B C31B C30B -5.5(9) . . . . ?
C28B C29B C30B C31B 34.8(13) . . . . ?
C29B C30B C31B O3B -19.1(11) . . . . ?
C31B O3B C28B C29B 28.2(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7515(19)
2 0.2485(19)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF + pentane layer at -- 20°C'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_mbx14_0m
_database_code_depnum_ccdc_archive 'CCDC 2371041'
loop_
_audit_author_name
_audit_author_address
'Frederic Capet'
;CNRS, UCCS
France
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_audit_creation_date             2022-02-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        (PyA2)Mg(BH4)(THF)
_chemical_formula_moiety         'C24 H39 B Mg N2 O'
_chemical_formula_sum            'C24 H39 B Mg N2 O'
_chemical_formula_weight         406.69
_chemical_melting_point          ?
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'
Mg Mg 0.0486 0.0363 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   11.6575(4)
_cell_length_b                   18.0090(6)
_cell_length_c                   12.3915(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.6880(10)
_cell_angle_gamma                90
_cell_volume                     2564.37(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    100.06
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.977
_shelx_estimated_absorpt_T_min   0.971
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1024 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.9401.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            95391
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.485
_diffrn_reflns_theta_min         1.772
_diffrn_ambient_temperature      100.06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6101
_reflns_number_total             7802
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2019.11-0 (Bruker-AXS, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         7802
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      1.110
_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)+(0.0561P)²+0.2145P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1053
_refine_special_details          
;
H atoms were positioned geometrically and allowed to ride on their parent atoms 
except for H atoms bonded B atom ; those H atoms were located from a 
difference Fourier map and refined freely.
;
_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:
 C7(H7), C18(H18), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C23(H23A,H23B), C21(H21A,H21B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C11(H11), C5(H5), C12(H12), C4(H4), C3(H3)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C16(H16A,H16B,
 H16C), C1(H1A,H1B,H1C), C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Mg1 Mg 0.16104(3) 0.65543(2) 0.33261(2) 0.01733(8) Uani 1 1 d . . . . .
O1 O 0.19425(6) 0.76108(3) 0.38271(5) 0.02290(14) Uani 1 1 d . . . . .
N2 N 0.29941(6) 0.59165(4) 0.36094(6) 0.01610(14) Uani 1 1 d . . . . .
N1 N 0.12539(6) 0.60566(4) 0.47900(6) 0.01808(15) Uani 1 1 d . . . . .
C9 C 0.37583(7) 0.56853(5) 0.29010(7) 0.01614(16) Uani 1 1 d . . . . .
C6 C 0.20728(8) 0.55512(5) 0.51726(7) 0.01747(17) Uani 1 1 d . . . . .
C14 C 0.35561(8) 0.50158(5) 0.22886(7) 0.01749(17) Uani 1 1 d . . . . .
C7 C 0.31379(8) 0.54936(5) 0.46242(7) 0.01662(16) Uani 1 1 d . . . . .
H7 H 0.324080 0.495976 0.444007 0.020 Uiso 1 1 calc R U . . .
C10 C 0.47304(8) 0.61288(5) 0.27563(7) 0.01805(17) Uani 1 1 d . . . . .
C2 C 0.03016(8) 0.61322(5) 0.52811(8) 0.02306(19) Uani 1 1 d . . . . .
C13 C 0.43226(8) 0.48029(5) 0.15912(7) 0.02117(18) Uani 1 1 d . . . . .
H13 H 0.418679 0.435203 0.119213 0.025 Uiso 1 1 calc R U . . .
C11 C 0.54657(8) 0.58962(5) 0.20410(7) 0.02223(18) Uani 1 1 d . . . . .
H11 H 0.610930 0.619791 0.194490 0.027 Uiso 1 1 calc R U . . .
C18 C 0.24858(8) 0.45426(5) 0.23381(7) 0.01987(17) Uani 1 1 d . . . . .
H18 H 0.205367 0.477627 0.288236 0.024 Uiso 1 1 calc R U . . .
C8 C 0.42113(8) 0.57333(5) 0.54604(7) 0.02095(18) Uani 1 1 d . . . . .
H8A H 0.490648 0.571734 0.511300 0.031 Uiso 1 1 calc R U . . .
H8B H 0.431161 0.539458 0.608820 0.031 Uiso 1 1 calc R U . . .
H8C H 0.409618 0.624002 0.571014 0.031 Uiso 1 1 calc R U . . .
C15 C 0.49485(8) 0.68690(5) 0.33424(7) 0.02066(18) Uani 1 1 d . . . . .
H15 H 0.446647 0.687862 0.393788 0.025 Uiso 1 1 calc R U . . .
C5 C 0.19634(9) 0.50942(5) 0.60620(7) 0.02296(19) Uani 1 1 d . . . . .
H5 H 0.255552 0.474663 0.633183 0.028 Uiso 1 1 calc R U . . .
C12 C 0.52752(8) 0.52337(5) 0.14685(7) 0.02326(19) Uani 1 1 d . . . . .
H12 H 0.579272 0.507741 0.099737 0.028 Uiso 1 1 calc R U . . .
C4 C 0.09807(9) 0.51563(6) 0.65422(8) 0.0275(2) Uani 1 1 d . . . . .
H4 H 0.087825 0.484168 0.713390 0.033 Uiso 1 1 calc R U . . .
C24 C 0.26537(9) 0.77719(5) 0.48873(7) 0.02334(19) Uani 1 1 d . . . . .
H24A H 0.338185 0.747824 0.498898 0.028 Uiso 1 1 calc R U . . .
H24B H 0.222345 0.765437 0.548996 0.028 Uiso 1 1 calc R U . . .
C3 C 0.01475(9) 0.56815(6) 0.61523(8) 0.0273(2) Uani 1 1 d . . . . .
H3 H -0.052821 0.573311 0.648059 0.033 Uiso 1 1 calc R U . . .
C20 C 0.27993(9) 0.37488(5) 0.27264(9) 0.0284(2) Uani 1 1 d . . . . .
H20A H 0.320332 0.349919 0.219582 0.043 Uiso 1 1 calc R U . . .
H20B H 0.208692 0.347548 0.279037 0.043 Uiso 1 1 calc R U . . .
H20C H 0.330809 0.376424 0.344126 0.043 Uiso 1 1 calc R U . . .
C17 C 0.45342(9) 0.75096(5) 0.25582(8) 0.0272(2) Uani 1 1 d . . . . .
H17A H 0.497851 0.750915 0.195346 0.041 Uiso 1 1 calc R U . . .
H17B H 0.465440 0.798212 0.295337 0.041 Uiso 1 1 calc R U . . .
H17C H 0.370488 0.744712 0.226640 0.041 Uiso 1 1 calc R U . . .
C16 C 0.62174(9) 0.69778(6) 0.38804(8) 0.0292(2) Uani 1 1 d . . . . .
H16A H 0.646624 0.655751 0.436599 0.044 Uiso 1 1 calc R U . . .
H16B H 0.629026 0.743875 0.430685 0.044 Uiso 1 1 calc R U . . .
H16C H 0.670868 0.700692 0.331315 0.044 Uiso 1 1 calc R U . . .
C23 C 0.29156(10) 0.85919(6) 0.48642(9) 0.0309(2) Uani 1 1 d . . . . .
H23A H 0.361938 0.868825 0.453668 0.037 Uiso 1 1 calc R U . . .
H23B H 0.302287 0.880927 0.560824 0.037 Uiso 1 1 calc R U . . .
C21 C 0.15554(10) 0.83045(5) 0.32754(8) 0.0301(2) Uani 1 1 d . . . . .
H21A H 0.071013 0.828900 0.298867 0.036 Uiso 1 1 calc R U . . .
H21B H 0.197834 0.840011 0.266036 0.036 Uiso 1 1 calc R U . . .
C1 C -0.05634(9) 0.67157(6) 0.48336(9) 0.0317(2) Uani 1 1 d . . . . .
H1A H -0.018352 0.720288 0.489197 0.048 Uiso 1 1 calc R U . . .
H1B H -0.120534 0.671778 0.525265 0.048 Uiso 1 1 calc R U . . .
H1C H -0.086773 0.660844 0.406326 0.048 Uiso 1 1 calc R U . . .
C19 C 0.16680(10) 0.45297(7) 0.12322(9) 0.0337(2) Uani 1 1 d . . . . .
H19A H 0.143357 0.503821 0.101595 0.051 Uiso 1 1 calc R U . . .
H19B H 0.097623 0.423453 0.129534 0.051 Uiso 1 1 calc R U . . .
H19C H 0.207125 0.430822 0.067797 0.051 Uiso 1 1 calc R U . . .
C22 C 0.18306(11) 0.88958(6) 0.41485(9) 0.0351(3) Uani 1 1 d . . . . .
H22A H 0.118545 0.895370 0.456913 0.042 Uiso 1 1 calc R U . . .
H22B H 0.198672 0.938039 0.382499 0.042 Uiso 1 1 calc R U . . .
B1 B 0.02563(11) 0.66002(7) 0.17813(10) 0.0305(2) Uani 1 1 d . . . . .
H1D H 0.1198(12) 0.6803(8) 0.1720(11) 0.043(4) Uiso 1 1 d . . . . .
H1E H -0.0298(13) 0.6583(8) 0.1003(12) 0.048(4) Uiso 1 1 d . . . . .
H1F H 0.0359(13) 0.6047(9) 0.2209(12) 0.055(4) Uiso 1 1 d . . . . .
H1G H -0.0052(16) 0.6993(11) 0.2405(15) 0.082(6) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Mg1 O1 2.0186(7) . ?
Mg1 N2 1.9631(8) . ?
Mg1 N1 2.1261(8) . ?
Mg1 B1 2.2685(12) . ?
Mg1 H1D 2.018(13) . ?
Mg1 H1F 2.049(15) . ?
Mg1 H1G 2.222(18) . ?
O1 C24 1.4598(11) . ?
O1 C21 1.4587(11) . ?
N2 C9 1.4145(11) . ?
N2 C7 1.4555(10) . ?
N1 C6 1.3461(12) . ?
N1 C2 1.3596(11) . ?
C9 C14 1.4230(12) . ?
C9 C10 1.4223(12) . ?
C6 C7 1.5160(12) . ?
C6 C5 1.3984(12) . ?
C14 C13 1.3973(12) . ?
C14 C18 1.5206(12) . ?
C7 H7 1.0000 . ?
C7 C8 1.5458(12) . ?
C10 C11 1.3970(13) . ?
C10 C15 1.5188(12) . ?
C2 C3 1.3863(14) . ?
C2 C1 1.4968(15) . ?
C13 H13 0.9500 . ?
C13 C12 1.3839(14) . ?
C11 H11 0.9500 . ?
C11 C12 1.3867(13) . ?
C18 H18 1.0000 . ?
C18 C20 1.5328(13) . ?
C18 C19 1.5322(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C17 1.5332(13) . ?
C15 C16 1.5294(13) . ?
C5 H5 0.9500 . ?
C5 C4 1.3813(14) . ?
C12 H12 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.3832(16) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.5092(14) . ?
C3 H3 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.5193(16) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.5134(14) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
B1 H1D 1.172(14) . ?
B1 H1E 1.067(15) . ?
B1 H1F 1.125(15) . ?
B1 H1G 1.149(19) . ?

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
O1 Mg1 N1 100.94(3) . . ?
O1 Mg1 B1 107.18(4) . . ?
O1 Mg1 H1D 95.5(4) . . ?
O1 Mg1 H1F 134.9(4) . . ?
O1 Mg1 H1G 85.9(5) . . ?
N2 Mg1 O1 112.78(3) . . ?
N2 Mg1 N1 82.73(3) . . ?
N2 Mg1 B1 127.33(4) . . ?
N2 Mg1 H1D 111.0(4) . . ?
N2 Mg1 H1F 109.3(4) . . ?
N2 Mg1 H1G 156.8(5) . . ?
N1 Mg1 B1 121.82(4) . . ?
N1 Mg1 H1D 152.5(4) . . ?
N1 Mg1 H1F 99.8(4) . . ?
N1 Mg1 H1G 108.0(5) . . ?
B1 Mg1 H1D 31.0(4) . . ?
B1 Mg1 H1F 29.6(4) . . ?
B1 Mg1 H1G 29.6(5) . . ?
H1D Mg1 H1F 53.7(6) . . ?
H1D Mg1 H1G 51.1(6) . . ?
H1F Mg1 H1G 49.5(6) . . ?
C24 O1 Mg1 120.97(5) . . ?
C21 O1 Mg1 129.41(6) . . ?
C21 O1 C24 109.61(7) . . ?
C9 N2 Mg1 130.21(6) . . ?
C9 N2 C7 112.90(7) . . ?
C7 N2 Mg1 115.62(5) . . ?
C6 N1 Mg1 110.90(6) . . ?
C6 N1 C2 119.61(8) . . ?
C2 N1 Mg1 129.14(6) . . ?
N2 C9 C14 121.02(8) . . ?
N2 C9 C10 120.75(8) . . ?
C10 C9 C14 118.20(8) . . ?
N1 C6 C7 118.30(7) . . ?
N1 C6 C5 121.48(8) . . ?
C5 C6 C7 120.21(8) . . ?
C9 C14 C18 121.11(8) . . ?
C13 C14 C9 119.77(8) . . ?
C13 C14 C18 119.05(8) . . ?
N2 C7 C6 111.56(7) . . ?
N2 C7 H7 107.9 . . ?
N2 C7 C8 113.30(7) . . ?
C6 C7 H7 107.9 . . ?
C6 C7 C8 108.19(7) . . ?
C8 C7 H7 107.9 . . ?
C9 C10 C15 120.36(8) . . ?
C11 C10 C9 119.90(8) . . ?
C11 C10 C15 119.70(8) . . ?
N1 C2 C3 120.83(9) . . ?
N1 C2 C1 117.03(9) . . ?
C3 C2 C1 122.14(9) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 C14 121.51(9) . . ?
C12 C13 H13 119.2 . . ?
C10 C11 H11 119.3 . . ?
C12 C11 C10 121.34(9) . . ?
C12 C11 H11 119.3 . . ?
C14 C18 H18 107.5 . . ?
C14 C18 C20 112.42(8) . . ?
C14 C18 C19 111.32(8) . . ?
C20 C18 H18 107.5 . . ?
C19 C18 H18 107.5 . . ?
C19 C18 C20 110.25(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 . . ?
C10 C15 H15 107.4 . . ?
C10 C15 C17 110.35(7) . . ?
C10 C15 C16 113.12(8) . . ?
C17 C15 H15 107.4 . . ?
C16 C15 H15 107.4 . . ?
C16 C15 C17 110.99(8) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 C6 118.95(9) . . ?
C4 C5 H5 120.5 . . ?
C13 C12 C11 119.24(8) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C5 C4 H4 120.3 . . ?
C5 C4 C3 119.30(9) . . ?
C3 C4 H4 120.3 . . ?
O1 C24 H24A 110.7 . . ?
O1 C24 H24B 110.7 . . ?
O1 C24 C23 105.27(7) . . ?
H24A C24 H24B 108.8 . . ?
C23 C24 H24A 110.7 . . ?
C23 C24 H24B 110.7 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.80(9) . . ?
C4 C3 H3 120.1 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C24 C23 H23A 111.3 . . ?
C24 C23 H23B 111.3 . . ?
C24 C23 C22 102.26(8) . . ?
H23A C23 H23B 109.2 . . ?
C22 C23 H23A 111.3 . . ?
C22 C23 H23B 111.3 . . ?
O1 C21 H21A 110.8 . . ?
O1 C21 H21B 110.8 . . ?
O1 C21 C22 104.83(8) . . ?
H21A C21 H21B 108.9 . . ?
C22 C21 H21A 110.8 . . ?
C22 C21 H21B 110.8 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C23 C22 H22A 111.2 . . ?
C23 C22 H22B 111.2 . . ?
C21 C22 C23 102.67(8) . . ?
C21 C22 H22A 111.2 . . ?
C21 C22 H22B 111.2 . . ?
H22A C22 H22B 109.1 . . ?
Mg1 B1 H1D 62.6(7) . . ?
Mg1 B1 H1E 172.3(8) . . ?
Mg1 B1 H1F 64.3(8) . . ?
Mg1 B1 H1G 73.0(9) . . ?
H1D B1 H1E 112.5(10) . . ?
H1D B1 H1F 106.3(10) . . ?
H1D B1 H1G 104.7(11) . . ?
H1E B1 H1F 113.6(11) . . ?
H1E B1 H1G 114.6(12) . . ?
H1F B1 H1G 104.4(12) . . ?

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
Mg1 O1 C24 C23 168.27(7) . . . . ?
Mg1 O1 C21 C22 166.82(7) . . . . ?
Mg1 N2 C9 C14 -90.90(9) . . . . ?
Mg1 N2 C9 C10 87.11(10) . . . . ?
Mg1 N2 C7 C6 8.63(9) . . . . ?
Mg1 N2 C7 C8 -113.75(7) . . . . ?
Mg1 N1 C6 C7 7.69(9) . . . . ?
Mg1 N1 C6 C5 -173.19(7) . . . . ?
Mg1 N1 C2 C3 170.72(7) . . . . ?
Mg1 N1 C2 C1 -8.89(12) . . . . ?
O1 C24 C23 C22 31.86(11) . . . . ?
O1 C21 C22 C23 32.02(12) . . . . ?
N2 C9 C14 C13 179.70(8) . . . . ?
N2 C9 C14 C18 2.56(12) . . . . ?
N2 C9 C10 C11 -179.08(8) . . . . ?
N2 C9 C10 C15 -1.40(12) . . . . ?
N1 C6 C7 N2 -10.90(11) . . . . ?
N1 C6 C7 C8 114.38(8) . . . . ?
N1 C6 C5 C4 1.21(13) . . . . ?
N1 C2 C3 C4 1.14(14) . . . . ?
C9 N2 C7 C6 -159.83(7) . . . . ?
C9 N2 C7 C8 77.78(9) . . . . ?
C9 C14 C13 C12 -0.77(13) . . . . ?
C9 C14 C18 C20 -121.74(9) . . . . ?
C9 C14 C18 C19 113.99(9) . . . . ?
C9 C10 C11 C12 -0.51(14) . . . . ?
C9 C10 C15 C17 -100.98(9) . . . . ?
C9 C10 C15 C16 134.00(9) . . . . ?
C6 N1 C2 C3 -1.76(12) . . . . ?
C6 N1 C2 C1 178.63(8) . . . . ?
C6 C5 C4 C3 -1.79(13) . . . . ?
C14 C9 C10 C11 -1.01(12) . . . . ?
C14 C9 C10 C15 176.66(8) . . . . ?
C14 C13 C12 C11 -0.76(14) . . . . ?
C7 N2 C9 C14 75.44(10) . . . . ?
C7 N2 C9 C10 -106.55(9) . . . . ?
C7 C6 C5 C4 -179.68(8) . . . . ?
C10 C9 C14 C13 1.64(12) . . . . ?
C10 C9 C14 C18 -175.50(8) . . . . ?
C10 C11 C12 C13 1.41(14) . . . . ?
C2 N1 C6 C7 -178.55(7) . . . . ?
C2 N1 C6 C5 0.57(12) . . . . ?
C13 C14 C18 C20 61.10(11) . . . . ?
C13 C14 C18 C19 -63.17(11) . . . . ?
C11 C10 C15 C17 76.70(10) . . . . ?
C11 C10 C15 C16 -48.32(11) . . . . ?
C18 C14 C13 C12 176.42(8) . . . . ?
C15 C10 C11 C12 -178.20(8) . . . . ?
C5 C6 C7 N2 169.97(8) . . . . ?
C5 C6 C7 C8 -64.75(10) . . . . ?
C5 C4 C3 C2 0.66(14) . . . . ?
C24 O1 C21 C22 -12.50(12) . . . . ?
C24 C23 C22 C21 -39.02(11) . . . . ?
C21 O1 C24 C23 -12.35(11) . . . . ?
C1 C2 C3 C4 -179.26(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mbxo5test
_database_code_depnum_ccdc_archive 'CCDC 2371036'
loop_
_audit_author_name
_audit_author_address
'Frederic Capet'
;CNRS, UCCS
France
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_audit_creation_date             2020-03-25
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        (PyA1)2Nd(BH4)
_chemical_formula_moiety         'C38 H54 B N4 Nd'
_chemical_formula_sum            'C38 H54 B N4 Nd'
_chemical_formula_weight         721.90
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.1304(11)
_cell_length_b                   10.7594(7)
_cell_length_c                   22.1049(15)
_cell_angle_alpha                90
_cell_angle_beta                 107.052(3)
_cell_angle_gamma                90
_cell_volume                     3667.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100.03
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.35
_shelx_estimated_absorpt_T_max   0.731
_shelx_estimated_absorpt_T_min   0.636
_exptl_absorpt_coefficient_mu    1.446
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0594 before and 0.0344 after correction.
The Ratio of minimum to maximum transmission is 0.9073.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 -1.00 0.00 0.0830
-1.00 1.00 0.00 0.1370
0.00 -1.00 1.00 0.1250
0.00 1.00 -1.00 0.1400
-1.00 0.00 1.00 0.1650
1.00 0.00 -1.00 0.1580
1.00 -1.00 1.00 0.0910
0.00 0.00 1.00 0.0850
0.00 0.00 -1.00 0.1150
1.00 0.00 0.00 0.1310
-1.00 0.00 0.00 0.1550
0.00 1.00 1.00 0.1260
0.00 -1.00 -1.00 0.1250
-1.00 1.00 1.00 0.1200
1.00 -1.00 -1.00 0.1240
-1.00 -1.00 0.00 0.1330
1.00 1.00 0.00 0.1150
0.00 1.00 0.00 0.1180
0.00 -1.00 0.00 0.1200
-1.00 -1.00 -1.00 0.1050

_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.231
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            55659
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.558
_diffrn_reflns_theta_min         1.927
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5518
_reflns_number_total             5593
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         5593
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0168
_refine_ls_restrained_S_all      1.143
_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)+(0.0143P)²+4.5954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0420
_refine_special_details          disorder
_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. Others
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=FVAR(1)
 Fixed Sof: H1B(0.5) H1C(0.5) H1D(0.5)
3.a Ternary CH refined with riding coordinates:
 C17(H17), C14(H14), C6B(H6B), C6A(H6A)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C12(H12), C10(H10), C2(H2), C11(H11), C3(H3), C4(H4)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Nd1 Nd 0.500000 0.62065(2) 0.250000 0.01383(3) Uani 1 2 d S T P A .
N1 N 0.62999(7) 0.67772(11) 0.21225(5) 0.0213(2) Uani 1 1 d . . . . .
N2 N 0.60838(6) 0.71958(9) 0.32443(4) 0.01537(17) Uani 1 1 d . . . . .
C1 C 0.63160(9) 0.66297(13) 0.15191(6) 0.0232(2) Uani 1 1 d . . . . .
H1 H 0.584718 0.620655 0.123085 0.028 Uiso 1 1 calc R U . . .
C13 C 0.54674(8) 0.85106(12) 0.39197(6) 0.0193(2) Uani 1 1 d . . . . .
C8 C 0.58943(7) 0.74033(11) 0.38261(5) 0.0159(2) Uani 1 1 d . . . . .
C9 C 0.60579(8) 0.64688(12) 0.43029(5) 0.0190(2) Uani 1 1 d . . . . .
C17 C 0.52887(9) 0.95725(12) 0.34454(6) 0.0227(2) Uani 1 1 d . . . . .
H17 H 0.542814 0.927871 0.305720 0.027 Uiso 1 1 calc R U . . .
C14 C 0.65260(9) 0.52663(12) 0.42499(6) 0.0244(3) Uani 1 1 d . . . . .
H14 H 0.659771 0.522425 0.381612 0.029 Uiso 1 1 calc R U . . .
C12 C 0.52132(10) 0.86500(14) 0.44682(7) 0.0271(3) Uani 1 1 d . . . . .
H12 H 0.492356 0.938888 0.452664 0.033 Uiso 1 1 calc R U . . .
C10 C 0.57927(9) 0.66598(14) 0.48442(6) 0.0255(3) Uani 1 1 d . . . . .
H10 H 0.590331 0.603425 0.516115 0.031 Uiso 1 1 calc R U . . .
C2 C 0.69812(10) 0.70647(15) 0.13018(7) 0.0302(3) Uani 1 1 d . . . . .
H2 H 0.697024 0.695069 0.087331 0.036 Uiso 1 1 calc R U . . .
C19 C 0.43439(11) 1.00054(16) 0.32494(9) 0.0374(4) Uani 1 1 d . . . . .
H19A H 0.396322 0.930105 0.307588 0.056 Uiso 1 1 calc R U . . .
H19B H 0.426266 1.065644 0.292722 0.056 Uiso 1 1 calc R U . . .
H19C H 0.420068 1.033594 0.361960 0.056 Uiso 1 1 calc R U . . .
C11 C 0.53742(10) 0.77351(15) 0.49284(6) 0.0292(3) Uani 1 1 d . . . . .
H11 H 0.519811 0.784693 0.529894 0.035 Uiso 1 1 calc R U . . .
C5 C 0.69615(9) 0.73719(17) 0.25328(6) 0.0326(3) Uani 1 1 d . . . . .
C3 C 0.76627(10) 0.76696(18) 0.17243(8) 0.0367(4) Uani 1 1 d . . . . .
H3 H 0.813144 0.798025 0.159034 0.044 Uiso 1 1 calc R U . . .
C4 C 0.76579(11) 0.7820(2) 0.23422(8) 0.0445(5) Uani 1 1 d . . . . .
H4 H 0.812741 0.822670 0.263789 0.053 Uiso 1 1 calc R U . . .
C18 C 0.58770(12) 1.06812(15) 0.37142(9) 0.0412(4) Uani 1 1 d . . . . .
H18A H 0.575800 1.097720 0.409974 0.062 Uiso 1 1 calc R U . . .
H18B H 0.576438 1.135157 0.340045 0.062 Uiso 1 1 calc R U . . .
H18C H 0.648522 1.042428 0.381454 0.062 Uiso 1 1 calc R U . . .
C15 C 0.60162(16) 0.41231(15) 0.43438(8) 0.0456(5) Uani 1 1 d . . . . .
H15A H 0.594038 0.414530 0.476766 0.068 Uiso 1 1 calc R U . . .
H15B H 0.633438 0.336973 0.429872 0.068 Uiso 1 1 calc R U . . .
H15C H 0.544656 0.412054 0.402535 0.068 Uiso 1 1 calc R U . . .
C6B C 0.7002(2) 0.7289(5) 0.32241(17) 0.0188(7) Uani 0.441(5) 1 d . . P A 1
H6B H 0.733801 0.653646 0.342146 0.023 Uiso 0.441(5) 1 calc R U P A 1
C16 C 0.74279(15) 0.5237(2) 0.47314(11) 0.0654(8) Uani 1 1 d . . . . .
H16A H 0.775200 0.598039 0.467990 0.098 Uiso 1 1 calc R U . . .
H16B H 0.773861 0.449345 0.466199 0.098 Uiso 1 1 calc R U . . .
H16C H 0.737057 0.521952 0.516057 0.098 Uiso 1 1 calc R U . . .
C7A C 0.76827(16) 0.7406(3) 0.36857(12) 0.0327(8) Uani 0.559(5) 1 d . . P A 2
H7AA H 0.762662 0.757664 0.410744 0.049 Uiso 0.559(5) 1 calc R U P A 2
H7AB H 0.816764 0.788629 0.362407 0.049 Uiso 0.559(5) 1 calc R U P A 2
H7AC H 0.779100 0.651697 0.364769 0.049 Uiso 0.559(5) 1 calc R U P A 2
C7B C 0.7461(2) 0.8471(4) 0.35392(17) 0.0367(11) Uani 0.441(5) 1 d . . P A 1
H7BA H 0.739515 0.854844 0.396441 0.055 Uiso 0.441(5) 1 calc R U P A 1
H7BB H 0.720242 0.919612 0.328546 0.055 Uiso 0.441(5) 1 calc R U P A 1
H7BC H 0.807842 0.842358 0.356912 0.055 Uiso 0.441(5) 1 calc R U P A 1
C6A C 0.68441(19) 0.7776(4) 0.31830(13) 0.0179(5) Uani 0.559(5) 1 d . . P A 2
H6A H 0.677278 0.869851 0.318783 0.021 Uiso 0.559(5) 1 calc R U P A 2
B1 B 0.500000 0.3745(2) 0.250000 0.0418(7) Uani 1 2 d S T P . .
H1A H 0.500000 0.271(3) 0.250000 0.053(9) Uiso 1 2 d S . P . .
H1B H 0.557(3) 0.414(4) 0.290(2) 0.033(10) Uiso 0.5 1 d . . P . .
H1C H 0.437(3) 0.413(5) 0.248(3) 0.058(14) Uiso 0.5 1 d . . P . .
H1D H 0.487(3) 0.421(4) 0.296(2) 0.042(11) Uiso 0.5 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Nd1 N1 2.5488(10) . ?
Nd1 N1 2.5488(10) 2_655 ?
Nd1 N2 2.2825(10) 2_655 ?
Nd1 N2 2.2824(10) . ?
Nd1 H1B 2.46(4) . ?
Nd1 H1B 2.46(4) 2_655 ?
Nd1 H1C 2.45(5) . ?
Nd1 H1D 2.42(4) . ?
N1 C1 1.3510(16) . ?
N1 C5 1.3429(17) . ?
N2 C8 1.4238(14) . ?
N2 C6B 1.499(4) . ?
N2 C6A 1.417(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.3797(19) . ?
C13 C8 1.4214(17) . ?
C13 C17 1.5201(18) . ?
C13 C12 1.3971(18) . ?
C8 C9 1.4242(17) . ?
C9 C14 1.5197(19) . ?
C9 C10 1.3990(18) . ?
C17 H17 1.0000 . ?
C17 C19 1.530(2) . ?
C17 C18 1.532(2) . ?
C14 H14 1.0000 . ?
C14 C15 1.527(2) . ?
C14 C16 1.530(2) . ?
C12 H12 0.9500 . ?
C12 C11 1.384(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.379(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.379(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C11 H11 0.9500 . ?
C5 C4 1.3960(19) . ?
C5 C6B 1.513(4) . ?
C5 C6A 1.565(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(2) . ?
C4 H4 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C6B H6B 1.0000 . ?
C6B C7B 1.532(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C7A C6A 1.530(4) . ?
C7B H7BA 0.9800 . ?
C7B H7BB 0.9800 . ?
C7B H7BC 0.9800 . ?
C6A H6A 1.0000 . ?
B1 B1 0.000(5) 2_655 ?
B1 H1A 1.12(3) . ?
B1 H1B 1.15(4) . ?
B1 H1B 1.15(4) 2_655 ?
B1 H1C 1.08(5) . ?
B1 H1D 1.21(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 Nd1 N1 152.12(5) 2_655 . ?
N1 Nd1 H1B 111.1(11) . 2_655 ?
N1 Nd1 H1B 94.3(11) . . ?
N1 Nd1 H1B 94.3(11) 2_655 2_655 ?
N1 Nd1 H1B 111.1(11) 2_655 . ?
N1 Nd1 H1C 126.1(12) . . ?
N1 Nd1 H1C 81.4(12) 2_655 . ?
N1 Nd1 H1D 83.8(11) 2_655 . ?
N1 Nd1 H1D 122.4(11) . . ?
N2 Nd1 N1 66.04(3) 2_655 2_655 ?
N2 Nd1 N1 100.45(4) . 2_655 ?
N2 Nd1 N1 66.04(3) . . ?
N2 Nd1 N1 100.45(4) 2_655 . ?
N2 Nd1 N2 124.40(5) . 2_655 ?
N2 Nd1 H1B 143.5(9) . 2_655 ?
N2 Nd1 H1B 143.5(9) 2_655 . ?
N2 Nd1 H1B 92.1(9) . . ?
N2 Nd1 H1B 92.1(9) 2_655 2_655 ?
N2 Nd1 H1C 100.9(13) 2_655 . ?
N2 Nd1 H1C 131.5(14) . . ?
N2 Nd1 H1D 104.8(11) . . ?
N2 Nd1 H1D 125.1(12) 2_655 . ?
H1B Nd1 H1B 51.5(19) . 2_655 ?
H1B Nd1 H1C 45.0(13) . . ?
H1B Nd1 H1D 28.3(12) . . ?
H1C Nd1 H1B 20.2(13) . 2_655 ?
H1C Nd1 H1D 26.7(14) . . ?
H1D Nd1 H1B 43.7(13) . 2_655 ?
C1 N1 Nd1 123.42(8) . . ?
C5 N1 Nd1 117.44(8) . . ?
C5 N1 C1 118.77(11) . . ?
C8 N2 Nd1 113.72(7) . . ?
C8 N2 C6B 119.50(16) . . ?
C6B N2 Nd1 124.37(16) . . ?
C6A N2 Nd1 129.62(13) . . ?
C6A N2 C8 115.99(14) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.09(13) . . ?
C2 C1 H1 118.5 . . ?
C8 C13 C17 122.11(11) . . ?
C12 C13 C8 119.63(12) . . ?
C12 C13 C17 118.26(12) . . ?
N2 C8 C9 121.03(11) . . ?
C13 C8 N2 120.30(10) . . ?
C13 C8 C9 118.46(11) . . ?
C8 C9 C14 122.17(11) . . ?
C10 C9 C8 119.50(12) . . ?
C10 C9 C14 118.32(12) . . ?
C13 C17 H17 108.0 . . ?
C13 C17 C19 113.32(12) . . ?
C13 C17 C18 110.31(11) . . ?
C19 C17 H17 108.0 . . ?
C19 C17 C18 108.98(13) . . ?
C18 C17 H17 108.0 . . ?
C9 C14 H14 108.2 . . ?
C9 C14 C15 112.07(13) . . ?
C9 C14 C16 110.87(12) . . ?
C15 C14 H14 108.2 . . ?
C15 C14 C16 109.21(16) . . ?
C16 C14 H14 108.2 . . ?
C13 C12 H12 119.3 . . ?
C11 C12 C13 121.46(13) . . ?
C11 C12 H12 119.3 . . ?
C9 C10 H10 119.2 . . ?
C11 C10 C9 121.55(13) . . ?
C11 C10 H10 119.2 . . ?
C1 C2 H2 120.9 . . ?
C3 C2 C1 118.11(13) . . ?
C3 C2 H2 120.9 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C11 H11 120.3 . . ?
C10 C11 C12 119.41(12) . . ?
C10 C11 H11 120.3 . . ?
N1 C5 C4 120.72(13) . . ?
N1 C5 C6B 116.41(18) . . ?
N1 C5 C6A 117.79(14) . . ?
C4 C5 C6B 121.65(18) . . ?
C4 C5 C6A 120.41(16) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.45(13) . . ?
C4 C3 H3 120.3 . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.85(14) . . ?
C3 C4 H4 120.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C6B C5 106.5(2) . . ?
N2 C6B H6B 110.3 . . ?
N2 C6B C7B 113.0(3) . . ?
C5 C6B H6B 110.3 . . ?
C5 C6B C7B 106.4(3) . . ?
C7B C6B H6B 110.3 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
C6A C7A H7AA 109.5 . . ?
C6A C7A H7AB 109.5 . . ?
C6A C7A H7AC 109.5 . . ?
C6B C7B H7BA 109.5 . . ?
C6B C7B H7BB 109.5 . . ?
C6B C7B H7BC 109.5 . . ?
H7BA C7B H7BB 109.5 . . ?
H7BA C7B H7BC 109.5 . . ?
H7BB C7B H7BC 109.5 . . ?
N2 C6A C5 107.86(19) . . ?
N2 C6A C7A 114.9(3) . . ?
N2 C6A H6A 109.3 . . ?
C5 C6A H6A 109.3 . . ?
C7A C6A C5 106.0(2) . . ?
C7A C6A H6A 109.3 . . ?
B1 B1 H1A 0(10) 2_655 . ?
B1 B1 H1B 0(10) 2_655 . ?
B1 B1 H1B 0(10) 2_655 2_655 ?
B1 B1 H1C 0(10) 2_655 . ?
B1 B1 H1D 0(10) 2_655 . ?
H1A B1 H1B 112(2) . 2_655 ?
H1A B1 H1B 112(2) . . ?
H1A B1 H1C 112(3) . . ?
H1A B1 H1D 114(2) . . ?
H1B B1 H1B 136(4) . 2_655 ?
H1B B1 H1C 115(3) . . ?
H1B B1 H1D 61(2) . . ?
H1C B1 H1B 45(3) . 2_655 ?
H1C B1 H1D 59(3) . . ?
H1D B1 H1B 101(3) . 2_655 ?

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
Nd1 N1 C1 C2 172.64(11) . . . . ?
Nd1 N1 C5 C4 -173.85(15) . . . . ?
Nd1 N1 C5 C6B 18.6(3) . . . . ?
Nd1 N1 C5 C6A -5.7(2) . . . . ?
Nd1 N2 C8 C13 -89.39(11) . . . . ?
Nd1 N2 C8 C9 85.13(11) . . . . ?
Nd1 N2 C6B C5 33.8(4) . . . . ?
Nd1 N2 C6B C7B 150.2(2) . . . . ?
Nd1 N2 C6A C5 -13.3(4) . . . . ?
Nd1 N2 C6A C7A -131.2(2) . . . . ?
N1 C1 C2 C3 0.5(2) . . . . ?
N1 C5 C4 C3 1.1(3) . . . . ?
N1 C5 C6B N2 -31.2(4) . . . . ?
N1 C5 C6B C7B -152.1(3) . . . . ?
N1 C5 C6A N2 11.0(3) . . . . ?
N1 C5 C6A C7A 134.5(2) . . . . ?
N2 C8 C9 C14 6.61(17) . . . . ?
N2 C8 C9 C10 -174.28(11) . . . . ?
C1 N1 C5 C4 -0.6(3) . . . . ?
C1 N1 C5 C6B -168.2(2) . . . . ?
C1 N1 C5 C6A 167.6(2) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C13 C8 C9 C14 -178.78(11) . . . . ?
C13 C8 C9 C10 0.34(17) . . . . ?
C13 C12 C11 C10 -0.2(2) . . . . ?
C8 N2 C6B C5 -164.98(19) . . . . ?
C8 N2 C6B C7B -48.5(4) . . . . ?
C8 N2 C6A C5 176.81(16) . . . . ?
C8 N2 C6A C7A 58.9(3) . . . . ?
C8 C13 C17 C19 128.91(13) . . . . ?
C8 C13 C17 C18 -108.59(15) . . . . ?
C8 C13 C12 C11 0.5(2) . . . . ?
C8 C9 C14 C15 -127.62(14) . . . . ?
C8 C9 C14 C16 110.07(17) . . . . ?
C8 C9 C10 C11 0.0(2) . . . . ?
C9 C10 C11 C12 -0.1(2) . . . . ?
C17 C13 C8 N2 -7.09(17) . . . . ?
C17 C13 C8 C9 178.25(11) . . . . ?
C17 C13 C12 C11 -178.37(13) . . . . ?
C14 C9 C10 C11 179.18(13) . . . . ?
C12 C13 C8 N2 174.03(11) . . . . ?
C12 C13 C8 C9 -0.62(17) . . . . ?
C12 C13 C17 C19 -52.20(17) . . . . ?
C12 C13 C17 C18 70.30(17) . . . . ?
C10 C9 C14 C15 53.25(16) . . . . ?
C10 C9 C14 C16 -69.06(19) . . . . ?
C2 C3 C4 C5 -0.7(3) . . . . ?
C5 N1 C1 C2 -0.2(2) . . . . ?
C4 C5 C6B N2 161.3(2) . . . . ?
C4 C5 C6B C7B 40.5(4) . . . . ?
C4 C5 C6A N2 179.2(2) . . . . ?
C4 C5 C6A C7A -57.2(3) . . . . ?
C6B N2 C8 C13 107.5(2) . . . . ?
C6B N2 C8 C9 -78.0(3) . . . . ?
C6B C5 C4 C3 168.0(3) . . . . ?
C6A N2 C8 C13 82.1(2) . . . . ?
C6A N2 C8 C9 -103.4(2) . . . . ?
C6A C5 C4 C3 -166.8(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene/pentane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mbx18
_database_code_depnum_ccdc_archive 'CCDC 2371042'
loop_
_audit_author_name
_audit_author_address
'Frederic Capet'
;CNRS, UCCS
France
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_audit_creation_date             2023-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        (PyA1)2Y(BH4)
_chemical_formula_moiety         'C38 H54 B N4 Y'
_chemical_formula_sum            'C38 H54 B N4 Y'
_chemical_formula_weight         666.57
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   15.8805(4)
_cell_length_b                   10.7056(3)
_cell_length_c                   22.3241(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.1020(10)
_cell_angle_gamma                90
_cell_volume                     3627.51(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9373
_cell_measurement_temperature    99.93
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.803
_shelx_estimated_absorpt_T_min   0.704
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0875 before and 0.0497 after correction.
The Ratio of minimum to maximum transmission is 0.9360.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            59875
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.254
_diffrn_reflns_theta_min         1.909
_diffrn_ambient_temperature      99.93
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Bruker PHOTON III C14'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker DUO PHOTON III'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4223
_reflns_number_total             4490
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2019.11-0 (Bruker-AXS, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0230
_refine_ls_restrained_S_all      1.045
_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)+(0.0255P)²+3.5629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0582
_refine_special_details          disorder
_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. Uiso/Uaniso restraints and constraints
Uanis(C6A) = Uanis(C6B)
Uanis(C7A) = Uanis(C7B)
3. Others
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=1-FVAR(1)
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=FVAR(1)
 Fixed Sof: H1B(0.5) H1C(0.5) H1D(0.5)
4.a Ternary CH refined with riding coordinates:
 C17(H17), C14(H14), C6A(H6A), C6B(H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C12(H12), C10(H10), C11(H11), C3(H3), C4(H4)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C16(H16A,H16B,
 H16C), C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Y1 Y 0.500000 0.38201(2) 0.750000 0.01341(5) Uani 1 2 d S T P A .
N2 N 0.39722(6) 0.28536(9) 0.67548(5) 0.0155(2) Uani 1 1 d . . . . .
N1 N 0.37486(7) 0.32825(11) 0.78712(5) 0.0203(2) Uani 1 1 d . . . . .
C8 C 0.41362(8) 0.26202(11) 0.61694(5) 0.0160(2) Uani 1 1 d . . . . .
C1 C 0.37203(9) 0.34545(13) 0.84653(6) 0.0226(3) Uani 1 1 d . . . . .
H1 H 0.419247 0.388667 0.875139 0.027 Uiso 1 1 calc R U . . .
C9 C 0.39430(8) 0.35415(12) 0.56898(6) 0.0189(2) Uani 1 1 d . . . . .
C17 C 0.47588(9) 0.04470(12) 0.65529(6) 0.0225(3) Uani 1 1 d . . . . .
H17 H 0.463617 0.075602 0.694168 0.027 Uiso 1 1 calc R U . . .
C2 C 0.30359(9) 0.30297(15) 0.86738(7) 0.0282(3) Uani 1 1 d . . . . .
H2 H 0.303896 0.316002 0.909537 0.034 Uiso 1 1 calc R U . . .
C14 C 0.34702(9) 0.47524(12) 0.57443(6) 0.0229(3) Uani 1 1 d . . . . .
H14 H 0.339631 0.479141 0.617357 0.027 Uiso 1 1 calc R U . . .
C12 C 0.47974(9) 0.13453(13) 0.55253(6) 0.0245(3) Uani 1 1 d . . . . .
H12 H 0.508907 0.060086 0.546668 0.029 Uiso 1 1 calc R U . . .
C13 C 0.45604(8) 0.15004(12) 0.60754(6) 0.0190(2) Uani 1 1 d . . . . .
C18 C 0.57177(10) 0.00053(15) 0.67305(8) 0.0361(3) Uani 1 1 d . . . . .
H18A H 0.583729 -0.037202 0.636389 0.054 Uiso 1 1 calc R U . . .
H18B H 0.581846 -0.061463 0.706719 0.054 Uiso 1 1 calc R U . . .
H18C H 0.611103 0.071994 0.687397 0.054 Uiso 1 1 calc R U . . .
C10 C 0.41931(9) 0.33342(13) 0.51476(6) 0.0244(3) Uani 1 1 d . . . . .
H10 H 0.406811 0.395386 0.482892 0.029 Uiso 1 1 calc R U . . .
C11 C 0.46165(10) 0.22527(14) 0.50639(6) 0.0272(3) Uani 1 1 d . . . . .
H11 H 0.478263 0.213187 0.469251 0.033 Uiso 1 1 calc R U . . .
C5 C 0.30792(9) 0.26773(16) 0.74650(6) 0.0308(3) Uani 1 1 d . . . . .
C3 C 0.23466(10) 0.24111(16) 0.82565(7) 0.0321(3) Uani 1 1 d . . . . .
H3 H 0.186727 0.210475 0.838718 0.039 Uiso 1 1 calc R U . . .
C15 C 0.39915(13) 0.59005(14) 0.56552(8) 0.0373(4) Uani 1 1 d . . . . .
H15A H 0.456662 0.590443 0.597506 0.056 Uiso 1 1 calc R U . . .
H15B H 0.366599 0.665804 0.569544 0.056 Uiso 1 1 calc R U . . .
H15C H 0.407648 0.587560 0.523798 0.056 Uiso 1 1 calc R U . . .
C4 C 0.23626(10) 0.22435(18) 0.76478(7) 0.0385(4) Uani 1 1 d . . . . .
H4 H 0.188728 0.183397 0.735322 0.046 Uiso 1 1 calc R U . . .
C19 C 0.41544(11) -0.06678(14) 0.63053(8) 0.0368(4) Uani 1 1 d . . . . .
H19A H 0.353849 -0.040738 0.621819 0.055 Uiso 1 1 calc R U . . .
H19B H 0.428207 -0.133420 0.662024 0.055 Uiso 1 1 calc R U . . .
H19C H 0.425542 -0.097631 0.591888 0.055 Uiso 1 1 calc R U . . .
C16 C 0.25541(13) 0.47910(18) 0.52659(10) 0.0567(6) Uani 1 1 d . . . . .
H16A H 0.261336 0.481045 0.484126 0.085 Uiso 1 1 calc R U . . .
H16B H 0.224134 0.554078 0.533549 0.085 Uiso 1 1 calc R U . . .
H16C H 0.222118 0.404660 0.531474 0.085 Uiso 1 1 calc R U . . .
C6A C 0.31953(18) 0.2242(3) 0.68230(12) 0.0189(5) Uani 0.587(2) 1 d . . P A 1
H6A H 0.329024 0.131741 0.683571 0.023 Uiso 0.587(2) 1 calc R U P A 1
B1 B 0.500000 0.6184(2) 0.750000 0.0352(6) Uani 1 2 d S T P . .
C7A C 0.23435(16) 0.2545(3) 0.63147(11) 0.0327(5) Uani 0.587(2) 1 d . . P A 1
H7AA H 0.220485 0.343293 0.633635 0.049 Uiso 0.587(2) 1 calc R U P A 1
H7AB H 0.186269 0.203889 0.637816 0.049 Uiso 0.587(2) 1 calc R U P A 1
H7AC H 0.241494 0.235885 0.590261 0.049 Uiso 0.587(2) 1 calc R U P A 1
C6B C 0.3050(3) 0.2778(4) 0.67855(19) 0.0189(5) Uani 0.413(2) 1 d . . P A 2
H6B H 0.271311 0.353960 0.659292 0.023 Uiso 0.413(2) 1 calc R U P A 2
C7B C 0.2572(2) 0.1595(4) 0.64706(17) 0.0327(5) Uani 0.413(2) 1 d . . P A 2
H7BA H 0.264020 0.151177 0.605022 0.049 Uiso 0.413(2) 1 calc R U P A 2
H7BB H 0.194419 0.165564 0.643865 0.049 Uiso 0.413(2) 1 calc R U P A 2
H7BC H 0.282553 0.086157 0.672207 0.049 Uiso 0.413(2) 1 calc R U P A 2
H1A H 0.500000 0.724(3) 0.750000 0.061(9) Uiso 1 2 d S . P . .
H1B H 0.440(3) 0.578(4) 0.714(2) 0.039(10) Uiso 0.5 1 d . . P . .
H1C H 0.488(3) 0.568(3) 0.7952(18) 0.034(9) Uiso 0.5 1 d . . P . .
H1D H 0.439(3) 0.578(4) 0.754(3) 0.052(12) Uiso 0.5 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Y1 N2 2.2147(10) . ?
Y1 N2 2.2148(10) 2_656 ?
Y1 N1 2.4363(10) . ?
Y1 N1 2.4363(10) 2_656 ?
Y1 H1B 2.34(4) . ?
Y1 H1C 2.26(4) . ?
Y1 H1D 2.33(4) . ?
N2 C8 1.4278(15) . ?
N2 C6A 1.444(3) . ?
N2 C6B 1.488(4) . ?
N1 C1 1.3527(16) . ?
N1 C5 1.3437(18) . ?
C8 C9 1.4211(17) . ?
C8 C13 1.4206(17) . ?
C1 H1 0.9500 . ?
C1 C2 1.3792(19) . ?
C9 C14 1.5208(18) . ?
C9 C10 1.3982(18) . ?
C17 H17 1.0000 . ?
C17 C13 1.5199(18) . ?
C17 C18 1.531(2) . ?
C17 C19 1.529(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.380(2) . ?
C14 H14 1.0000 . ?
C14 C15 1.5272(19) . ?
C14 C16 1.531(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.3960(17) . ?
C12 C11 1.383(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.379(2) . ?
C11 H11 0.9500 . ?
C5 C4 1.3965(19) . ?
C5 C6A 1.569(3) . ?
C5 C6B 1.508(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C4 H4 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C6A H6A 1.0000 . ?
C6A C7A 1.523(4) . ?
B1 H1A 1.13(3) . ?
B1 H1B 1.14(4) . ?
B1 H1C 1.21(4) . ?
B1 H1D 1.09(4) . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C6B H6B 1.0000 . ?
C6B C7B 1.537(6) . ?
C7B H7BA 0.9800 . ?
C7B H7BB 0.9800 . ?
C7B H7BC 0.9800 . ?

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
N2 Y1 N2 124.30(5) . 2_656 ?
N2 Y1 N1 69.54(4) . . ?
N2 Y1 N1 97.40(4) 2_656 . ?
N2 Y1 N1 97.40(4) . 2_656 ?
N2 Y1 N1 69.54(4) 2_656 2_656 ?
N2 Y1 H1B 144.3(10) 2_656 . ?
N2 Y1 H1B 91.2(10) . . ?
N2 Y1 H1C 102.5(10) 2_656 . ?
N2 Y1 H1C 127.1(10) . . ?
N2 Y1 H1D 128.0(13) 2_656 . ?
N2 Y1 H1D 103.1(13) . . ?
N1 Y1 N1 152.67(6) 2_656 . ?
N1 Y1 H1B 92.3(11) . . ?
N1 Y1 H1B 112.4(11) 2_656 . ?
N1 Y1 H1C 82.5(10) . . ?
N1 Y1 H1C 123.1(10) 2_656 . ?
N1 Y1 H1D 128.2(11) 2_656 . ?
N1 Y1 H1D 78.9(11) . . ?
H1B Y1 H1C 44.9(12) . . ?
H1B Y1 H1D 22.5(12) . . ?
H1C Y1 H1D 25.6(12) . . ?
C8 N2 Y1 118.48(7) . . ?
C8 N2 C6A 114.12(13) . . ?
C8 N2 C6B 118.65(18) . . ?
C6A N2 Y1 126.62(12) . . ?
C6B N2 Y1 120.56(17) . . ?
C1 N1 Y1 124.54(9) . . ?
C5 N1 Y1 116.54(8) . . ?
C5 N1 C1 118.66(11) . . ?
C9 C8 N2 120.72(11) . . ?
C13 C8 N2 120.33(11) . . ?
C13 C8 C9 118.76(11) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.87(13) . . ?
C2 C1 H1 118.6 . . ?
C8 C9 C14 122.26(11) . . ?
C10 C9 C8 119.25(12) . . ?
C10 C9 C14 118.49(12) . . ?
C13 C17 H17 108.1 . . ?
C13 C17 C18 113.32(12) . . ?
C13 C17 C19 110.30(11) . . ?
C18 C17 H17 108.1 . . ?
C19 C17 H17 108.1 . . ?
C19 C17 C18 108.86(12) . . ?
C1 C2 H2 120.7 . . ?
C1 C2 C3 118.54(13) . . ?
C3 C2 H2 120.7 . . ?
C9 C14 H14 108.2 . . ?
C9 C14 C15 112.10(12) . . ?
C9 C14 C16 110.94(12) . . ?
C15 C14 H14 108.2 . . ?
C15 C14 C16 109.13(14) . . ?
C16 C14 H14 108.2 . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C11 C12 C13 121.39(13) . . ?
C8 C13 C17 122.14(11) . . ?
C12 C13 C8 119.50(12) . . ?
C12 C13 C17 118.35(12) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C9 C10 H10 119.2 . . ?
C11 C10 C9 121.63(13) . . ?
C11 C10 H10 119.2 . . ?
C12 C11 H11 120.3 . . ?
C10 C11 C12 119.45(12) . . ?
C10 C11 H11 120.3 . . ?
N1 C5 C4 120.94(13) . . ?
N1 C5 C6A 118.54(14) . . ?
N1 C5 C6B 115.38(19) . . ?
C4 C5 C6A 119.53(15) . . ?
C4 C5 C6B 122.08(19) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.13(13) . . ?
C4 C3 H3 120.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.85(14) . . ?
C3 C4 H4 120.1 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C6A C5 107.16(17) . . ?
N2 C6A H6A 109.0 . . ?
N2 C6A C7A 115.1(2) . . ?
C5 C6A H6A 109.0 . . ?
C7A C6A C5 107.5(2) . . ?
C7A C6A H6A 109.0 . . ?
H1A B1 H1B 113(2) . . ?
H1A B1 H1C 116.6(17) . . ?
H1A B1 H1D 113(2) . . ?
H1B B1 H1C 97(2) . . ?
H1B B1 H1D 48(2) . . ?
H1C B1 H1D 52(3) . . ?
C6A C7A H7AA 109.5 . . ?
C6A C7A H7AB 109.5 . . ?
C6A C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
N2 C6B C5 108.1(3) . . ?
N2 C6B H6B 110.2 . . ?
N2 C6B C7B 112.6(3) . . ?
C5 C6B H6B 110.2 . . ?
C5 C6B C7B 105.4(3) . . ?
C7B C6B H6B 110.2 . . ?
C6B C7B H7BA 109.5 . . ?
C6B C7B H7BB 109.5 . . ?
C6B C7B H7BC 109.5 . . ?
H7BA C7B H7BB 109.5 . . ?
H7BA C7B H7BC 109.5 . . ?
H7BB C7B H7BC 109.5 . . ?

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
Y1 N2 C8 C9 -85.91(12) . . . . ?
Y1 N2 C8 C13 89.07(12) . . . . ?
Y1 N2 C6A C5 14.5(3) . . . . ?
Y1 N2 C6A C7A 133.89(18) . . . . ?
Y1 N2 C6B C5 -34.1(3) . . . . ?
Y1 N2 C6B C7B -150.1(2) . . . . ?
Y1 N1 C1 C2 -173.57(10) . . . . ?
Y1 N1 C5 C4 175.05(14) . . . . ?
Y1 N1 C5 C6A 6.5(2) . . . . ?
Y1 N1 C5 C6B -19.1(2) . . . . ?
N2 C8 C9 C14 -6.50(17) . . . . ?
N2 C8 C9 C10 173.57(11) . . . . ?
N2 C8 C13 C17 7.33(17) . . . . ?
N2 C8 C13 C12 -173.39(11) . . . . ?
N1 C1 C2 C3 -0.5(2) . . . . ?
N1 C5 C4 C3 -1.4(3) . . . . ?
N1 C5 C6A N2 -12.5(3) . . . . ?
N1 C5 C6A C7A -136.7(2) . . . . ?
N1 C5 C6B N2 32.8(3) . . . . ?
N1 C5 C6B C7B 153.4(2) . . . . ?
C8 N2 C6A C5 -175.88(14) . . . . ?
C8 N2 C6A C7A -56.5(3) . . . . ?
C8 N2 C6B C5 163.42(17) . . . . ?
C8 N2 C6B C7B 47.4(4) . . . . ?
C8 C9 C14 C15 125.11(13) . . . . ?
C8 C9 C14 C16 -112.61(16) . . . . ?
C8 C9 C10 C11 0.54(19) . . . . ?
C1 N1 C5 C4 0.6(2) . . . . ?
C1 N1 C5 C6A -167.90(16) . . . . ?
C1 N1 C5 C6B 166.5(2) . . . . ?
C1 C2 C3 C4 -0.3(2) . . . . ?
C9 C8 C13 C17 -177.60(11) . . . . ?
C9 C8 C13 C12 1.69(17) . . . . ?
C9 C10 C11 C12 0.2(2) . . . . ?
C2 C3 C4 C5 1.2(3) . . . . ?
C14 C9 C10 C11 -179.39(12) . . . . ?
C13 C8 C9 C14 178.44(11) . . . . ?
C13 C8 C9 C10 -1.48(17) . . . . ?
C13 C12 C11 C10 0.0(2) . . . . ?
C18 C17 C13 C8 -129.10(13) . . . . ?
C18 C17 C13 C12 51.61(16) . . . . ?
C10 C9 C14 C15 -54.97(16) . . . . ?
C10 C9 C14 C16 67.31(18) . . . . ?
C11 C12 C13 C8 -0.96(19) . . . . ?
C11 C12 C13 C17 178.35(12) . . . . ?
C5 N1 C1 C2 0.4(2) . . . . ?
C4 C5 C6A N2 178.81(17) . . . . ?
C4 C5 C6A C7A 54.6(3) . . . . ?
C4 C5 C6B N2 -161.5(2) . . . . ?
C4 C5 C6B C7B -40.9(4) . . . . ?
C19 C17 C13 C8 108.57(14) . . . . ?
C19 C17 C13 C12 -70.72(16) . . . . ?
C6A N2 C8 C9 103.54(17) . . . . ?
C6A N2 C8 C13 -81.48(18) . . . . ?
C6A C5 C4 C3 166.99(19) . . . . ?
C6B N2 C8 C9 77.0(2) . . . . ?
C6B N2 C8 C13 -108.1(2) . . . . ?
C6B C5 C4 C3 -166.4(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mbx11
_database_code_depnum_ccdc_archive 'CCDC 2371039'
loop_
_audit_author_name
_audit_author_address
'Frederic Capet'
;CNRS, UCCS
France
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_audit_creation_date             2021-06-15
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        PyAH2
_chemical_formula_moiety         'C20 H28 N2'
_chemical_formula_sum            'C20 H28 N2'
_chemical_formula_weight         296.44
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   14.5286(6)
_cell_length_b                   11.2578(4)
_cell_length_c                   22.0519(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3606.8(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.47
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.987
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1077 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.9036.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            70664
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         1.809
_diffrn_ambient_temperature      99.98
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.61
_diffrn_source_power             0.0305
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                7172
_reflns_number_total             8927
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2019.11-0 (Bruker-AXS, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 
;
 Flack x determined using 2895 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.5(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8927
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0491
_refine_ls_restrained_S_all      1.046
_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)+(0.0656P)²+0.6869P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1279
_refine_special_details          ?
_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 Riding coordinates:
 N1(H1), N3(H3A)
2.b Ternary CH refined with riding coordinates:
 C27(H27), C33(H33), C7(H7), C10(H10), C13(H13), C30(H30)
2.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C4(H4), C5(H5), C25(H25), C23(H23), C3(H3), C24(H24), C18(H18),
 C38(H38), C17(H17), C16(H16), C37(H37)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C34(H34A,H34B,H34C), C28(H28A,H28B,H28C), C31(H31A,H31B,
 H31C), C29(H29A,H29B,H29C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C9(H9A,
 H9B,H9C), C8(H8A,H8B,H8C), C32(H32A,H32B,H32C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
N1 N 0.44661(15) 0.5711(2) 0.67244(10) 0.0151(5) Uani 1 1 d . . . . .
H1 H 0.455176 0.625535 0.700529 0.018 Uiso 1 1 d R U . . .
N4 N 0.40779(16) 0.7112(2) 0.33420(11) 0.0189(5) Uani 1 1 d . . . . .
N2 N 0.34351(16) 0.7902(2) 0.66450(11) 0.0190(5) Uani 1 1 d . . . . .
N3 N 0.30568(15) 0.9301(2) 0.32839(11) 0.0163(5) Uani 1 1 d . . . . .
H3A H 0.295451 0.874981 0.300914 0.020 Uiso 1 1 d R U . . .
C1 C 0.52196(18) 0.5650(2) 0.63061(12) 0.0145(5) Uani 1 1 d . . . . .
C27 C 0.1787(2) 0.7230(3) 0.35447(13) 0.0174(6) Uani 1 1 d . . . . .
H27 H 0.229879 0.725789 0.324184 0.021 Uiso 1 1 calc R U . . .
C35 C 0.42056(18) 0.7959(3) 0.37663(12) 0.0174(6) Uani 1 1 d . . . . .
C2 C 0.58088(18) 0.6623(2) 0.62000(12) 0.0151(5) Uani 1 1 d . . . . .
C36 C 0.45134(19) 0.7702(3) 0.43459(14) 0.0204(6) Uani 1 1 d . . . . .
H36 H 0.458676 0.831672 0.463707 0.024 Uiso 1 1 calc R U . . .
C4 C 0.66342(19) 0.5445(3) 0.54548(13) 0.0192(6) Uani 1 1 d . . . . .
H4 H 0.709835 0.538861 0.515280 0.023 Uiso 1 1 calc R U . . .
C26 C 0.21942(18) 1.0502(2) 0.39964(13) 0.0166(6) Uani 1 1 d . . . . .
C39 C 0.42594(18) 0.5974(3) 0.34870(14) 0.0204(6) Uani 1 1 d . . . . .
C5 C 0.6073(2) 0.4477(3) 0.55808(13) 0.0197(6) Uani 1 1 d . . . . .
H5 H 0.616532 0.375157 0.536941 0.024 Uiso 1 1 calc R U . . .
C21 C 0.23271(18) 0.9386(2) 0.37205(13) 0.0153(5) Uani 1 1 d . . . . .
C25 C 0.15255(19) 1.0604(3) 0.44526(13) 0.0193(6) Uani 1 1 d . . . . .
H25 H 0.145151 1.134022 0.465730 0.023 Uiso 1 1 calc R U . . .
C23 C 0.10690(19) 0.8589(2) 0.43063(13) 0.0188(6) Uani 1 1 d . . . . .
H23 H 0.066876 0.794959 0.440341 0.023 Uiso 1 1 calc R U . . .
C33 C 0.39896(18) 0.9216(2) 0.35525(13) 0.0178(6) Uani 1 1 d . . . . .
H33 H 0.401771 0.975868 0.391109 0.021 Uiso 1 1 calc R U . . .
C22 C 0.17411(18) 0.8427(2) 0.38591(12) 0.0158(5) Uani 1 1 d . . . . .
C19 C 0.32849(19) 0.9032(3) 0.64826(14) 0.0215(6) Uani 1 1 d . . . . .
C7 C 0.5747(2) 0.7781(3) 0.65527(13) 0.0183(6) Uani 1 1 d . . . . .
H7 H 0.516551 0.775902 0.679554 0.022 Uiso 1 1 calc R U . . .
C3 C 0.65124(19) 0.6488(3) 0.57715(13) 0.0189(6) Uani 1 1 d . . . . .
H3 H 0.691721 0.713455 0.569700 0.023 Uiso 1 1 calc R U . . .
C40 C 0.4059(3) 0.5070(3) 0.30059(16) 0.0258(8) Uani 1 1 d . . . . .
H40A H 0.343299 0.518811 0.285192 0.039 Uiso 1 1 calc R U . . .
H40B H 0.411299 0.427058 0.317832 0.039 Uiso 1 1 calc R U . . .
H40C H 0.450022 0.515983 0.267286 0.039 Uiso 1 1 calc R U . . .
C6 C 0.53731(18) 0.4556(3) 0.60145(13) 0.0179(6) Uani 1 1 d . . . . .
C15 C 0.33416(18) 0.7044(3) 0.62216(13) 0.0168(5) Uani 1 1 d . . . . .
C10 C 0.48428(19) 0.3440(2) 0.61881(13) 0.0199(6) Uani 1 1 d . . . . .
H10 H 0.437475 0.366458 0.650029 0.024 Uiso 1 1 calc R U . . .
C13 C 0.35439(18) 0.5793(2) 0.64450(13) 0.0166(5) Uani 1 1 d . . . . .
H13 H 0.352138 0.524054 0.609033 0.020 Uiso 1 1 calc R U . . .
C24 C 0.0973(2) 0.9655(3) 0.46099(13) 0.0214(6) Uani 1 1 d . . . . .
H24 H 0.053029 0.973436 0.492436 0.026 Uiso 1 1 calc R U . . .
C34 C 0.4703(2) 0.9625(3) 0.30932(14) 0.0235(6) Uani 1 1 d . . . . .
H34A H 0.467778 0.911199 0.273468 0.035 Uiso 1 1 calc R U . . .
H34B H 0.531753 0.958079 0.327479 0.035 Uiso 1 1 calc R U . . .
H34C H 0.457301 1.044713 0.297406 0.035 Uiso 1 1 calc R U . . .
C18 C 0.3022(2) 0.9344(3) 0.58982(15) 0.0260(7) Uani 1 1 d . . . . .
H18 H 0.291426 1.015209 0.579644 0.031 Uiso 1 1 calc R U . . .
C30 C 0.27100(19) 1.1606(3) 0.37925(14) 0.0216(6) Uani 1 1 d . . . . .
H30 H 0.317573 1.135431 0.348432 0.026 Uiso 1 1 calc R U . . .
C38 C 0.4586(2) 0.5660(3) 0.40599(14) 0.0224(6) Uani 1 1 d . . . . .
H38 H 0.472037 0.485364 0.415098 0.027 Uiso 1 1 calc R U . . .
C17 C 0.2920(2) 0.8464(3) 0.54673(15) 0.0266(7) Uani 1 1 d . . . . .
H17 H 0.273585 0.865670 0.506578 0.032 Uiso 1 1 calc R U . . .
C28 C 0.1990(2) 0.6217(3) 0.39917(14) 0.0243(6) Uani 1 1 d . . . . .
H28A H 0.255806 0.639162 0.421373 0.036 Uiso 1 1 calc R U . . .
H28B H 0.206221 0.547091 0.376764 0.036 Uiso 1 1 calc R U . . .
H28C H 0.147821 0.614181 0.427882 0.036 Uiso 1 1 calc R U . . .
C16 C 0.30914(19) 0.7295(3) 0.56302(13) 0.0213(6) Uani 1 1 d . . . . .
H16 H 0.303744 0.667515 0.533990 0.026 Uiso 1 1 calc R U . . .
C31 C 0.2042(2) 1.2473(3) 0.34810(18) 0.0339(8) Uani 1 1 d . . . . .
H31A H 0.173947 1.207242 0.314028 0.051 Uiso 1 1 calc R U . . .
H31B H 0.238381 1.316306 0.333116 0.051 Uiso 1 1 calc R U . . .
H31C H 0.157574 1.273487 0.377324 0.051 Uiso 1 1 calc R U . . .
C29 C 0.0891(2) 0.6986(3) 0.32029(14) 0.0237(6) Uani 1 1 d . . . . .
H29A H 0.037073 0.703975 0.348442 0.036 Uiso 1 1 calc R U . . .
H29B H 0.091261 0.618813 0.302597 0.036 Uiso 1 1 calc R U . . .
H29C H 0.081536 0.757463 0.287921 0.036 Uiso 1 1 calc R U . . .
C14 C 0.28183(19) 0.5402(3) 0.69043(14) 0.0213(6) Uani 1 1 d . . . . .
H14A H 0.296817 0.460550 0.705356 0.032 Uiso 1 1 calc R U . . .
H14B H 0.221233 0.538936 0.670927 0.032 Uiso 1 1 calc R U . . .
H14C H 0.280876 0.596114 0.724503 0.032 Uiso 1 1 calc R U . . .
C37 C 0.4713(2) 0.6532(3) 0.44951(14) 0.0232(6) Uani 1 1 d . . . . .
H37 H 0.493273 0.633312 0.488794 0.028 Uiso 1 1 calc R U . . .
C20 C 0.3437(3) 0.9946(3) 0.69742(17) 0.0273(8) Uani 1 1 d . . . . .
H20A H 0.292791 0.991291 0.726497 0.041 Uiso 1 1 calc R U . . .
H20B H 0.346567 1.073924 0.679256 0.041 Uiso 1 1 calc R U . . .
H20C H 0.401747 0.977714 0.718403 0.041 Uiso 1 1 calc R U . . .
C9 C 0.6552(2) 0.7870(3) 0.69984(16) 0.0318(8) Uani 1 1 d . . . . .
H9A H 0.652975 0.720056 0.728205 0.048 Uiso 1 1 calc R U . . .
H9B H 0.650885 0.861735 0.722441 0.048 Uiso 1 1 calc R U . . .
H9C H 0.713421 0.784921 0.677371 0.048 Uiso 1 1 calc R U . . .
C8 C 0.5698(2) 0.8864(3) 0.61340(16) 0.0311(8) Uani 1 1 d . . . . .
H8A H 0.626481 0.891611 0.589469 0.047 Uiso 1 1 calc R U . . .
H8B H 0.562852 0.958570 0.637849 0.047 Uiso 1 1 calc R U . . .
H8C H 0.516924 0.878434 0.586107 0.047 Uiso 1 1 calc R U . . .
C32 C 0.3224(3) 1.2207(3) 0.43096(17) 0.0370(8) Uani 1 1 d . . . . .
H32A H 0.278103 1.249828 0.461002 0.055 Uiso 1 1 calc R U . . .
H32B H 0.358170 1.287559 0.415035 0.055 Uiso 1 1 calc R U . . .
H32C H 0.363977 1.163377 0.450147 0.055 Uiso 1 1 calc R U . . .
C11 C 0.4333(2) 0.2901(3) 0.56457(15) 0.0311(7) Uani 1 1 d . . . . .
H11A H 0.391618 0.349497 0.547219 0.047 Uiso 1 1 calc R U . . .
H11B H 0.397735 0.221019 0.578014 0.047 Uiso 1 1 calc R U . . .
H11C H 0.478027 0.265354 0.533786 0.047 Uiso 1 1 calc R U . . .
C12 C 0.5496(2) 0.2512(3) 0.64723(18) 0.0319(8) Uani 1 1 d . . . . .
H12A H 0.596342 0.228176 0.617462 0.048 Uiso 1 1 calc R U . . .
H12B H 0.514112 0.181049 0.659327 0.048 Uiso 1 1 calc R U . . .
H12C H 0.579631 0.285538 0.682944 0.048 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
N1 H1 0.8801 . ?
N1 C1 1.433(3) . ?
N1 C13 1.478(3) . ?
N4 C35 1.349(4) . ?
N4 C39 1.347(4) . ?
N2 C19 1.340(4) . ?
N2 C15 1.350(4) . ?
N3 H3A 0.8801 . ?
N3 C21 1.435(4) . ?
N3 C33 1.482(3) . ?
C1 C2 1.409(4) . ?
C1 C6 1.407(4) . ?
C27 H27 1.0000 . ?
C27 C22 1.518(4) . ?
C27 C28 1.536(4) . ?
C27 C29 1.529(4) . ?
C35 C36 1.385(4) . ?
C35 C33 1.524(4) . ?
C2 C7 1.520(4) . ?
C2 C3 1.400(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.388(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(4) . ?
C4 C3 1.377(4) . ?
C26 C21 1.410(4) . ?
C26 C25 1.403(4) . ?
C26 C30 1.519(4) . ?
C39 C40 1.499(4) . ?
C39 C38 1.395(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.399(4) . ?
C21 C22 1.408(4) . ?
C25 H25 0.9500 . ?
C25 C24 1.381(4) . ?
C23 H23 0.9500 . ?
C23 C22 1.400(4) . ?
C23 C24 1.381(4) . ?
C33 H33 1.0000 . ?
C33 C34 1.520(4) . ?
C19 C18 1.389(4) . ?
C19 C20 1.510(4) . ?
C7 H7 1.0000 . ?
C7 C9 1.532(4) . ?
C7 C8 1.531(4) . ?
C3 H3 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C6 C10 1.523(4) . ?
C15 C13 1.520(4) . ?
C15 C16 1.383(4) . ?
C10 H10 1.0000 . ?
C10 C11 1.532(4) . ?
C10 C12 1.544(4) . ?
C13 H13 1.0000 . ?
C13 C14 1.527(4) . ?
C24 H24 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C18 H18 0.9500 . ?
C18 C17 1.381(5) . ?
C30 H30 1.0000 . ?
C30 C31 1.539(4) . ?
C30 C32 1.522(5) . ?
C38 H38 0.9500 . ?
C38 C37 1.385(4) . ?
C17 H17 0.9500 . ?
C17 C16 1.387(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C16 H16 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C37 H37 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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
C1 N1 H1 112.2 . . ?
C1 N1 C13 115.3(2) . . ?
C13 N1 H1 112.2 . . ?
C39 N4 C35 118.8(3) . . ?
C19 N2 C15 118.6(3) . . ?
C21 N3 H3A 112.6 . . ?
C21 N3 C33 114.3(2) . . ?
C33 N3 H3A 112.6 . . ?
C2 C1 N1 122.3(2) . . ?
C6 C1 N1 117.2(2) . . ?
C6 C1 C2 120.5(3) . . ?
C22 C27 H27 108.0 . . ?
C22 C27 C28 112.0(2) . . ?
C22 C27 C29 110.3(2) . . ?
C28 C27 H27 108.0 . . ?
C29 C27 H27 108.0 . . ?
C29 C27 C28 110.3(2) . . ?
N4 C35 C36 122.5(3) . . ?
N4 C35 C33 114.4(2) . . ?
C36 C35 C33 123.1(3) . . ?
C1 C2 C7 123.0(2) . . ?
C3 C2 C1 118.1(2) . . ?
C3 C2 C7 118.8(2) . . ?
C35 C36 H36 120.5 . . ?
C35 C36 C37 119.0(3) . . ?
C37 C36 H36 120.5 . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.5(3) . . ?
C21 C26 C30 122.3(3) . . ?
C25 C26 C21 118.5(3) . . ?
C25 C26 C30 119.1(2) . . ?
N4 C39 C40 116.1(3) . . ?
N4 C39 C38 121.5(3) . . ?
C38 C39 C40 122.4(3) . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.9(3) . . ?
C6 C5 H5 119.6 . . ?
C26 C21 N3 116.7(2) . . ?
C22 C21 N3 122.8(2) . . ?
C22 C21 C26 120.4(3) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 C26 121.3(3) . . ?
C24 C25 H25 119.4 . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C24 C23 C22 121.7(3) . . ?
N3 C33 C35 111.8(2) . . ?
N3 C33 H33 108.3 . . ?
N3 C33 C34 109.7(2) . . ?
C35 C33 H33 108.3 . . ?
C34 C33 C35 110.3(2) . . ?
C34 C33 H33 108.3 . . ?
C21 C22 C27 123.7(2) . . ?
C23 C22 C27 117.9(2) . . ?
C23 C22 C21 118.4(2) . . ?
N2 C19 C18 122.2(3) . . ?
N2 C19 C20 115.5(3) . . ?
C18 C19 C20 122.3(3) . . ?
C2 C7 H7 107.7 . . ?
C2 C7 C9 109.8(2) . . ?
C2 C7 C8 112.2(2) . . ?
C9 C7 H7 107.7 . . ?
C8 C7 H7 107.7 . . ?
C8 C7 C9 111.7(3) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.9(3) . . ?
C4 C3 H3 119.1 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C1 C6 C10 121.8(3) . . ?
C5 C6 C1 118.9(3) . . ?
C5 C6 C10 119.1(2) . . ?
N2 C15 C13 114.8(2) . . ?
N2 C15 C16 122.2(3) . . ?
C16 C15 C13 123.0(3) . . ?
C6 C10 H10 108.0 . . ?
C6 C10 C11 112.0(2) . . ?
C6 C10 C12 110.5(2) . . ?
C11 C10 H10 108.0 . . ?
C11 C10 C12 110.2(3) . . ?
C12 C10 H10 108.0 . . ?
N1 C13 C15 111.6(2) . . ?
N1 C13 H13 108.5 . . ?
N1 C13 C14 109.3(2) . . ?
C15 C13 H13 108.5 . . ?
C15 C13 C14 110.4(2) . . ?
C14 C13 H13 108.5 . . ?
C25 C24 C23 119.5(3) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C19 C18 H18 120.4 . . ?
C17 C18 C19 119.1(3) . . ?
C17 C18 H18 120.4 . . ?
C26 C30 H30 107.7 . . ?
C26 C30 C31 109.9(2) . . ?
C26 C30 C32 112.6(3) . . ?
C31 C30 H30 107.7 . . ?
C32 C30 H30 107.7 . . ?
C32 C30 C31 111.2(3) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 C39 119.6(3) . . ?
C37 C38 H38 120.2 . . ?
C18 C17 H17 120.5 . . ?
C18 C17 C16 118.9(3) . . ?
C16 C17 H17 120.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C15 C16 C17 119.0(3) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C36 C37 H37 120.6 . . ?
C38 C37 C36 118.7(3) . . ?
C38 C37 H37 120.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 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 . . ?
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 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 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 . . ?
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_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 C1 C2 C7 5.0(4) . . . . ?
N1 C1 C2 C3 -178.4(2) . . . . ?
N1 C1 C6 C5 176.9(2) . . . . ?
N1 C1 C6 C10 -7.3(4) . . . . ?
N4 C35 C36 C37 1.1(4) . . . . ?
N4 C35 C33 N3 52.8(3) . . . . ?
N4 C35 C33 C34 -69.6(3) . . . . ?
N4 C39 C38 C37 1.1(4) . . . . ?
N2 C19 C18 C17 -0.6(5) . . . . ?
N2 C15 C13 N1 -54.6(3) . . . . ?
N2 C15 C13 C14 67.2(3) . . . . ?
N2 C15 C16 C17 -0.7(4) . . . . ?
N3 C21 C22 C27 -2.9(4) . . . . ?
N3 C21 C22 C23 177.9(2) . . . . ?
C1 N1 C13 C15 -78.0(3) . . . . ?
C1 N1 C13 C14 159.5(2) . . . . ?
C1 C2 C7 C9 106.5(3) . . . . ?
C1 C2 C7 C8 -128.7(3) . . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
C1 C6 C10 C11 123.0(3) . . . . ?
C1 C6 C10 C12 -113.7(3) . . . . ?
C35 N4 C39 C40 177.1(3) . . . . ?
C35 N4 C39 C38 -0.9(4) . . . . ?
C35 C36 C37 C38 -0.8(4) . . . . ?
C2 C1 C6 C5 -5.2(4) . . . . ?
C2 C1 C6 C10 170.7(2) . . . . ?
C36 C35 C33 N3 -127.6(3) . . . . ?
C36 C35 C33 C34 110.0(3) . . . . ?
C4 C5 C6 C1 2.6(4) . . . . ?
C4 C5 C6 C10 -173.4(3) . . . . ?
C26 C21 C22 C27 174.7(3) . . . . ?
C26 C21 C22 C23 -4.4(4) . . . . ?
C26 C25 C24 C23 -1.0(4) . . . . ?
C39 N4 C35 C36 -0.2(4) . . . . ?
C39 N4 C35 C33 179.4(2) . . . . ?
C39 C38 C37 C36 -0.2(4) . . . . ?
C5 C4 C3 C2 -3.0(4) . . . . ?
C5 C6 C10 C11 -61.1(3) . . . . ?
C5 C6 C10 C12 62.2(4) . . . . ?
C21 N3 C33 C35 80.0(3) . . . . ?
C21 N3 C33 C34 -157.3(2) . . . . ?
C21 C26 C25 C24 -3.3(4) . . . . ?
C21 C26 C30 C31 110.5(3) . . . . ?
C21 C26 C30 C32 -125.0(3) . . . . ?
C25 C26 C21 N3 -176.1(2) . . . . ?
C25 C26 C21 C22 6.0(4) . . . . ?
C25 C26 C30 C31 -66.0(4) . . . . ?
C25 C26 C30 C32 58.5(4) . . . . ?
C33 N3 C21 C26 77.6(3) . . . . ?
C33 N3 C21 C22 -104.6(3) . . . . ?
C33 C35 C36 C37 -178.5(3) . . . . ?
C22 C23 C24 C25 2.8(4) . . . . ?
C19 N2 C15 C13 178.9(2) . . . . ?
C19 N2 C15 C16 -0.4(4) . . . . ?
C19 C18 C17 C16 -0.6(4) . . . . ?
C7 C2 C3 C4 177.1(3) . . . . ?
C3 C2 C7 C9 -70.1(3) . . . . ?
C3 C2 C7 C8 54.8(3) . . . . ?
C3 C4 C5 C6 1.5(4) . . . . ?
C40 C39 C38 C37 -176.7(3) . . . . ?
C6 C1 C2 C7 -172.9(3) . . . . ?
C6 C1 C2 C3 3.7(4) . . . . ?
C15 N2 C19 C18 1.1(4) . . . . ?
C15 N2 C19 C20 -177.8(3) . . . . ?
C13 N1 C1 C2 105.5(3) . . . . ?
C13 N1 C1 C6 -76.5(3) . . . . ?
C13 C15 C16 C17 -180.0(3) . . . . ?
C24 C23 C22 C27 -179.3(3) . . . . ?
C24 C23 C22 C21 -0.1(4) . . . . ?
C18 C17 C16 C15 1.2(4) . . . . ?
C30 C26 C21 N3 7.4(4) . . . . ?
C30 C26 C21 C22 -170.4(3) . . . . ?
C30 C26 C25 C24 173.3(3) . . . . ?
C28 C27 C22 C21 119.9(3) . . . . ?
C28 C27 C22 C23 -61.0(3) . . . . ?
C16 C15 C13 N1 124.7(3) . . . . ?
C16 C15 C13 C14 -113.5(3) . . . . ?
C29 C27 C22 C21 -116.9(3) . . . . ?
C29 C27 C22 C23 62.3(3) . . . . ?
C20 C19 C18 C17 178.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_mbx10_0m
_database_code_depnum_ccdc_archive 'CCDC 2371038'
loop_
_audit_author_name
_audit_author_address
'Frederic Capet'
;CNRS, UCCS
France
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_audit_creation_date             2022-10-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        (PyA3)Mg(BH4)(THF)
_chemical_formula_moiety         'C38 H58 B Mg N3 O'
_chemical_formula_sum            'C38 H58 B Mg N3 O'
_chemical_formula_weight         607.99
_chemical_melting_point          ?
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'
Mg Mg 0.0486 0.0363 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   10.0564(8)
_cell_length_b                   16.3418(12)
_cell_length_c                   22.4870(17)
_cell_angle_alpha                90
_cell_angle_beta                 102.785(2)
_cell_angle_gamma                90
_cell_volume                     3603.9(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100.05
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.24
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.985
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0835 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.9305.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0313
_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       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75277
_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         25.666
_diffrn_reflns_theta_min         1.554
_diffrn_ambient_temperature      100.05
_diffrn_detector_area_resol_mean ?
_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_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5325
_reflns_number_total             6820
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2019.11-0 (Bruker-AXS, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6820
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0497
_refine_ls_restrained_S_all      1.047
_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)+(0.0488P)²+3.2041P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1266
_refine_special_details          
;
H atoms were positioned geometrically and allowed to ride on their parent atoms 
except for H atoms bonded to B atom ; those H atoms were located from a 
difference Fourier map and refined freely.
;
_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:
 C29(H29), C32(H32), C7(H7), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C38(H38A,H38B), C37(H37A,H37B), C36(H36A,H36B)
2.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C25(H25), C19(H19), C27(H27), C17(H17), C18(H18), C5(H5), C4(H4),
 C3(H3)
2.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C22(H22A,H22B,H22C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C30(H30A,H30B,H30C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C12(H12A,
 H12B,H12C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Mg1 Mg 0.69913(6) 0.49047(4) 0.26303(2) 0.01512(16) Uani 1 1 d . . . . .
O1 O 0.66984(14) 0.61419(9) 0.26378(7) 0.0273(3) Uani 1 1 d . . . . .
N2 N 0.48348(15) 0.46663(9) 0.24038(7) 0.0163(3) Uani 1 1 d . . . . .
N1 N 0.66434(15) 0.45277(10) 0.17356(7) 0.0166(3) Uani 1 1 d . . . . .
N3 N 0.61433(15) 0.47576(9) 0.35457(7) 0.0161(3) Uani 1 1 d . . . . .
C23 C 0.69769(18) 0.46916(12) 0.41553(8) 0.0169(4) Uani 1 1 d . . . . .
C20 C 0.40470(19) 0.47268(11) 0.28206(9) 0.0176(4) Uani 1 1 d . . . . .
C1 C 0.76311(19) 0.43063(12) 0.13950(8) 0.0181(4) Uani 1 1 d . . . . .
C26 C 0.8628(2) 0.45095(13) 0.53129(9) 0.0221(4) Uani 1 1 d . . . . .
H26 H 0.918626 0.444739 0.571052 0.026 Uiso 1 1 calc R U . . .
C13 C 0.52255(19) 0.44762(12) 0.13798(8) 0.0182(4) Uani 1 1 d . . . . .
C25 C 0.82203(19) 0.52769(13) 0.50912(9) 0.0203(4) Uani 1 1 d . . . . .
H25 H 0.851558 0.574188 0.533882 0.024 Uiso 1 1 calc R U . . .
C16 C 0.42642(19) 0.45671(11) 0.18141(8) 0.0174(4) Uani 1 1 d . . . . .
C28 C 0.74103(19) 0.39049(12) 0.43658(9) 0.0192(4) Uani 1 1 d . . . . .
C21 C 0.48387(19) 0.47648(11) 0.34654(9) 0.0176(4) Uani 1 1 d . . . . .
C24 C 0.73856(19) 0.53892(12) 0.45134(9) 0.0188(4) Uani 1 1 d . . . . .
C19 C 0.2645(2) 0.47078(12) 0.26509(9) 0.0224(4) Uani 1 1 d . . . . .
H19 H 0.210610 0.476420 0.294630 0.027 Uiso 1 1 calc R U . . .
C27 C 0.8220(2) 0.38312(13) 0.49520(9) 0.0227(4) Uani 1 1 d . . . . .
H27 H 0.849721 0.330265 0.510716 0.027 Uiso 1 1 calc R U . . .
C2 C 0.81170(19) 0.34852(13) 0.14023(9) 0.0214(4) Uani 1 1 d . . . . .
C29 C 0.6944(2) 0.62519(12) 0.43026(9) 0.0216(4) Uani 1 1 d . . . . .
H29 H 0.639237 0.622007 0.387479 0.026 Uiso 1 1 calc R U . . .
C32 C 0.6994(2) 0.31447(12) 0.39810(9) 0.0239(5) Uani 1 1 d . . . . .
H32 H 0.664493 0.332675 0.355017 0.029 Uiso 1 1 calc R U . . .
C7 C 0.7754(2) 0.28357(13) 0.18229(9) 0.0257(5) Uani 1 1 d . . . . .
H7 H 0.700548 0.305508 0.200522 0.031 Uiso 1 1 calc R U . . .
C17 C 0.2840(2) 0.45356(13) 0.16173(9) 0.0245(5) Uani 1 1 d . . . . .
H17 H 0.243406 0.446750 0.119677 0.029 Uiso 1 1 calc R U . . .
C10 C 0.8017(2) 0.58083(13) 0.11227(9) 0.0245(5) Uani 1 1 d . . . . .
H10 H 0.734825 0.589459 0.138641 0.029 Uiso 1 1 calc R U . . .
C31 C 0.6050(2) 0.66201(13) 0.47024(10) 0.0269(5) Uani 1 1 d . . . . .
H31A H 0.524591 0.627393 0.468288 0.040 Uiso 1 1 calc R U . . .
H31B H 0.575993 0.717048 0.455566 0.040 Uiso 1 1 calc R U . . .
H31C H 0.657151 0.665204 0.512511 0.040 Uiso 1 1 calc R U . . .
C18 C 0.2035(2) 0.46041(13) 0.20369(10) 0.0255(5) Uani 1 1 d . . . . .
H18 H 0.106985 0.458064 0.190803 0.031 Uiso 1 1 calc R U . . .
C5 C 0.9092(2) 0.46378(15) 0.06927(9) 0.0296(5) Uani 1 1 d . . . . .
H5 H 0.943332 0.503085 0.045316 0.035 Uiso 1 1 calc R U . . .
C6 C 0.8210(2) 0.48909(13) 0.10578(9) 0.0218(4) Uani 1 1 d . . . . .
C22 C 0.4049(2) 0.47789(13) 0.39587(9) 0.0240(5) Uani 1 1 d . . . . .
H22A H 0.468077 0.473165 0.435727 0.036 Uiso 1 1 calc R U . . .
H22B H 0.340741 0.431941 0.390212 0.036 Uiso 1 1 calc R U . . .
H22C H 0.354455 0.529471 0.393906 0.036 Uiso 1 1 calc R U . . .
C15 C 0.4853(2) 0.51513(13) 0.08883(9) 0.0242(5) Uani 1 1 d . . . . .
H15A H 0.500459 0.569034 0.108248 0.036 Uiso 1 1 calc R U . . .
H15B H 0.389127 0.509722 0.068086 0.036 Uiso 1 1 calc R U . . .
H15C H 0.542566 0.509373 0.059051 0.036 Uiso 1 1 calc R U . . .
C14 C 0.4878(2) 0.36515(13) 0.10478(9) 0.0230(4) Uani 1 1 d . . . . .
H14A H 0.547721 0.356658 0.076367 0.034 Uiso 1 1 calc R U . . .
H14B H 0.392626 0.365737 0.082136 0.034 Uiso 1 1 calc R U . . .
H14C H 0.501122 0.320675 0.134747 0.034 Uiso 1 1 calc R U . . .
C4 C 0.9478(2) 0.38287(15) 0.06726(10) 0.0325(5) Uani 1 1 d . . . . .
H4 H 1.004983 0.366218 0.041052 0.039 Uiso 1 1 calc R U . . .
C30 C 0.8171(2) 0.68088(13) 0.43079(10) 0.0286(5) Uani 1 1 d . . . . .
H30A H 0.867646 0.689054 0.472913 0.043 Uiso 1 1 calc R U . . .
H30B H 0.785229 0.733864 0.412676 0.043 Uiso 1 1 calc R U . . .
H30C H 0.876891 0.655384 0.407121 0.043 Uiso 1 1 calc R U . . .
C3 C 0.9021(2) 0.32683(14) 0.10374(10) 0.0283(5) Uani 1 1 d . . . . .
H3 H 0.932859 0.271820 0.104186 0.034 Uiso 1 1 calc R U . . .
C11 C 0.9385(2) 0.61945(14) 0.14437(10) 0.0320(5) Uani 1 1 d . . . . .
H11A H 0.972011 0.592610 0.183810 0.048 Uiso 1 1 calc R U . . .
H11B H 0.925354 0.677940 0.150814 0.048 Uiso 1 1 calc R U . . .
H11C H 1.005136 0.612388 0.118901 0.048 Uiso 1 1 calc R U . . .
C35 C 0.7800(2) 0.67074(14) 0.26248(11) 0.0315(5) Uani 1 1 d . . . . .
H35A H 0.848783 0.645342 0.242898 0.038 Uiso 1 1 calc R U . . .
H35B H 0.825069 0.687997 0.304276 0.038 Uiso 1 1 calc R U . . .
C8 C 0.7262(3) 0.20335(14) 0.14963(11) 0.0368(6) Uani 1 1 d . . . . .
H8A H 0.649932 0.214533 0.115144 0.055 Uiso 1 1 calc R U . . .
H8B H 0.696240 0.165997 0.178145 0.055 Uiso 1 1 calc R U . . .
H8C H 0.801070 0.178157 0.134701 0.055 Uiso 1 1 calc R U . . .
C12 C 0.7493(3) 0.62608(15) 0.05192(10) 0.0369(6) Uani 1 1 d . . . . .
H12A H 0.814472 0.619325 0.025715 0.055 Uiso 1 1 calc R U . . .
H12B H 0.739115 0.684398 0.060071 0.055 Uiso 1 1 calc R U . . .
H12C H 0.660745 0.603463 0.031407 0.055 Uiso 1 1 calc R U . . .
C34 C 0.5837(3) 0.26938(15) 0.41818(12) 0.0397(6) Uani 1 1 d . . . . .
H34A H 0.557796 0.221071 0.392383 0.060 Uiso 1 1 calc R U . . .
H34B H 0.504859 0.305878 0.414226 0.060 Uiso 1 1 calc R U . . .
H34C H 0.614045 0.252259 0.460793 0.060 Uiso 1 1 calc R U . . .
B1 B 0.9259(2) 0.47054(16) 0.31244(10) 0.0221(5) Uani 1 1 d . . . . .
C38 C 0.5416(2) 0.65829(14) 0.24945(11) 0.0334(5) Uani 1 1 d . . . . .
H38A H 0.490024 0.649756 0.281680 0.040 Uiso 1 1 calc R U . . .
H38B H 0.485024 0.639538 0.210040 0.040 Uiso 1 1 calc R U . . .
C33 C 0.8192(3) 0.25665(15) 0.39887(11) 0.0380(6) Uani 1 1 d . . . . .
H33A H 0.849023 0.232870 0.439659 0.057 Uiso 1 1 calc R U . . .
H33B H 0.894710 0.287165 0.388406 0.057 Uiso 1 1 calc R U . . .
H33C H 0.790576 0.212804 0.369049 0.057 Uiso 1 1 calc R U . . .
C9 C 0.8985(3) 0.26564(16) 0.23418(11) 0.0422(6) Uani 1 1 d . . . . .
H9A H 0.971294 0.241053 0.217482 0.063 Uiso 1 1 calc R U . . .
H9B H 0.871676 0.227629 0.263140 0.063 Uiso 1 1 calc R U . . .
H9C H 0.931292 0.316764 0.255154 0.063 Uiso 1 1 calc R U . . .
C37 C 0.5791(3) 0.74747(15) 0.24590(12) 0.0404(6) Uani 1 1 d . . . . .
H37A H 0.590808 0.774550 0.286107 0.048 Uiso 1 1 calc R U . . .
H37B H 0.509217 0.777287 0.215737 0.048 Uiso 1 1 calc R U . . .
C36 C 0.7129(3) 0.74259(15) 0.22569(13) 0.0439(6) Uani 1 1 d . . . . .
H36A H 0.698202 0.732101 0.181355 0.053 Uiso 1 1 calc R U . . .
H36B H 0.767164 0.793231 0.235949 0.053 Uiso 1 1 calc R U . . .
H1A H 0.928(2) 0.4842(14) 0.2633(11) 0.034(6) Uiso 1 1 d . . . . .
H1B H 1.023(3) 0.4456(15) 0.3383(11) 0.042(7) Uiso 1 1 d . . . . .
H1C H 0.845(2) 0.4169(14) 0.3101(10) 0.033(6) Uiso 1 1 d . . . . .
H1D H 0.889(3) 0.5211(16) 0.3331(12) 0.046(7) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Mg1 O1 2.0439(16) . ?
Mg1 N2 2.1507(16) . ?
Mg1 N1 2.0587(16) . ?
Mg1 N3 2.4081(16) . ?
Mg1 B1 2.328(2) . ?
Mg1 H1A 2.30(2) . ?
Mg1 H1C 2.00(2) . ?
Mg1 H1D 2.24(3) . ?
O1 C35 1.448(3) . ?
O1 C38 1.450(3) . ?
N2 C20 1.358(2) . ?
N2 C16 1.333(2) . ?
N1 C1 1.428(2) . ?
N1 C13 1.475(2) . ?
N3 C23 1.444(2) . ?
N3 C21 1.284(2) . ?
C23 C28 1.406(3) . ?
C23 C24 1.404(3) . ?
C20 C21 1.493(3) . ?
C20 C19 1.377(3) . ?
C1 C2 1.427(3) . ?
C1 C6 1.422(3) . ?
C26 H26 0.9500 . ?
C26 C25 1.378(3) . ?
C26 C27 1.381(3) . ?
C13 C16 1.526(3) . ?
C13 C15 1.548(3) . ?
C13 C14 1.543(3) . ?
C25 H25 0.9500 . ?
C25 C24 1.394(3) . ?
C16 C17 1.403(3) . ?
C28 C27 1.393(3) . ?
C28 C32 1.519(3) . ?
C21 C22 1.500(3) . ?
C24 C29 1.522(3) . ?
C19 H19 0.9500 . ?
C19 C18 1.392(3) . ?
C27 H27 0.9500 . ?
C2 C7 1.519(3) . ?
C2 C3 1.399(3) . ?
C29 H29 1.0000 . ?
C29 C31 1.529(3) . ?
C29 C30 1.531(3) . ?
C32 H32 1.0000 . ?
C32 C34 1.528(3) . ?
C32 C33 1.528(3) . ?
C7 H7 1.0000 . ?
C7 C8 1.530(3) . ?
C7 C9 1.530(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.378(3) . ?
C10 H10 1.0000 . ?
C10 C6 1.523(3) . ?
C10 C11 1.540(3) . ?
C10 C12 1.533(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C18 H18 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.398(3) . ?
C5 C4 1.382(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C4 H4 0.9500 . ?
C4 C3 1.374(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C3 H3 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.507(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
B1 H1A 1.13(2) . ?
B1 H1B 1.10(2) . ?
B1 H1C 1.19(2) . ?
B1 H1D 1.06(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C37 1.512(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C36 1.515(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?

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
O1 Mg1 N2 92.38(6) . . ?
O1 Mg1 N1 108.08(7) . . ?
O1 Mg1 N3 90.74(6) . . ?
O1 Mg1 B1 105.20(8) . . ?
O1 Mg1 H1A 100.9(6) . . ?
O1 Mg1 H1C 132.7(7) . . ?
O1 Mg1 H1D 82.8(7) . . ?
N2 Mg1 N3 69.83(6) . . ?
N2 Mg1 B1 156.58(8) . . ?
N2 Mg1 H1A 161.3(6) . . ?
N2 Mg1 H1C 126.6(7) . . ?
N2 Mg1 H1D 149.5(7) . . ?
N1 Mg1 N2 76.70(6) . . ?
N1 Mg1 N3 142.16(6) . . ?
N1 Mg1 B1 111.18(7) . . ?
N1 Mg1 H1A 86.7(6) . . ?
N1 Mg1 H1C 106.4(6) . . ?
N1 Mg1 H1D 133.4(7) . . ?
N3 Mg1 H1A 122.4(6) . . ?
N3 Mg1 H1C 81.0(6) . . ?
N3 Mg1 H1D 80.1(7) . . ?
B1 Mg1 N3 94.18(7) . . ?
B1 Mg1 H1A 28.3(6) . . ?
B1 Mg1 H1C 30.8(7) . . ?
B1 Mg1 H1D 26.7(7) . . ?
H1A Mg1 H1C 50.2(9) . . ?
H1A Mg1 H1D 46.8(9) . . ?
H1C Mg1 H1D 49.9(9) . . ?
C35 O1 Mg1 121.27(12) . . ?
C35 O1 C38 108.96(16) . . ?
C38 O1 Mg1 127.78(13) . . ?
C20 N2 Mg1 122.34(12) . . ?
C16 N2 Mg1 116.55(12) . . ?
C16 N2 C20 120.46(16) . . ?
C1 N1 Mg1 127.72(12) . . ?
C1 N1 C13 113.46(14) . . ?
C13 N1 Mg1 118.82(11) . . ?
C23 N3 Mg1 125.30(11) . . ?
C21 N3 Mg1 115.01(12) . . ?
C21 N3 C23 119.66(15) . . ?
C28 C23 N3 117.37(17) . . ?
C24 C23 N3 121.25(17) . . ?
C24 C23 C28 121.33(17) . . ?
N2 C20 C21 113.96(16) . . ?
N2 C20 C19 121.67(18) . . ?
C19 C20 C21 124.28(17) . . ?
C2 C1 N1 120.59(17) . . ?
C6 C1 N1 122.07(18) . . ?
C6 C1 C2 117.29(17) . . ?
C25 C26 H26 120.3 . . ?
C25 C26 C27 119.45(18) . . ?
C27 C26 H26 120.3 . . ?
N1 C13 C16 108.70(15) . . ?
N1 C13 C15 113.53(16) . . ?
N1 C13 C14 113.60(16) . . ?
C16 C13 C15 107.45(15) . . ?
C16 C13 C14 106.69(15) . . ?
C14 C13 C15 106.50(15) . . ?
C26 C25 H25 119.1 . . ?
C26 C25 C24 121.78(19) . . ?
C24 C25 H25 119.1 . . ?
N2 C16 C13 117.02(16) . . ?
N2 C16 C17 120.18(17) . . ?
C17 C16 C13 122.79(17) . . ?
C23 C28 C32 122.04(17) . . ?
C27 C28 C23 118.08(18) . . ?
C27 C28 C32 119.87(18) . . ?
N3 C21 C20 116.42(16) . . ?
N3 C21 C22 125.96(18) . . ?
C20 C21 C22 117.59(16) . . ?
C23 C24 C29 123.06(17) . . ?
C25 C24 C23 117.85(18) . . ?
C25 C24 C29 119.09(17) . . ?
C20 C19 H19 120.8 . . ?
C20 C19 C18 118.50(18) . . ?
C18 C19 H19 120.8 . . ?
C26 C27 C28 121.47(19) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C1 C2 C7 122.38(17) . . ?
C3 C2 C1 119.80(19) . . ?
C3 C2 C7 117.72(19) . . ?
C24 C29 H29 108.2 . . ?
C24 C29 C31 110.52(16) . . ?
C24 C29 C30 111.68(17) . . ?
C31 C29 H29 108.2 . . ?
C31 C29 C30 109.83(17) . . ?
C30 C29 H29 108.2 . . ?
C28 C32 H32 107.6 . . ?
C28 C32 C34 110.97(17) . . ?
C28 C32 C33 112.50(18) . . ?
C34 C32 H32 107.6 . . ?
C33 C32 H32 107.6 . . ?
C33 C32 C34 110.39(19) . . ?
C2 C7 H7 108.1 . . ?
C2 C7 C8 113.37(17) . . ?
C2 C7 C9 110.09(19) . . ?
C8 C7 H7 108.1 . . ?
C9 C7 H7 108.1 . . ?
C9 C7 C8 108.84(19) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.67(19) . . ?
C18 C17 H17 120.2 . . ?
C6 C10 H10 108.2 . . ?
C6 C10 C11 109.20(17) . . ?
C6 C10 C12 114.60(18) . . ?
C11 C10 H10 108.2 . . ?
C12 C10 H10 108.2 . . ?
C12 C10 C11 108.27(18) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C19 C18 H18 120.2 . . ?
C17 C18 C19 119.51(19) . . ?
C17 C18 H18 120.2 . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.4(2) . . ?
C1 C6 C10 122.31(17) . . ?
C5 C6 C1 120.1(2) . . ?
C5 C6 C10 117.28(18) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C5 C4 H4 120.5 . . ?
C3 C4 C5 119.00(19) . . ?
C3 C4 H4 120.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.9(2) . . ?
C4 C3 H3 119.1 . . ?
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 . . ?
O1 C35 H35A 110.8 . . ?
O1 C35 H35B 110.8 . . ?
O1 C35 C36 104.90(18) . . ?
H35A C35 H35B 108.8 . . ?
C36 C35 H35A 110.8 . . ?
C36 C35 H35B 110.8 . . ?
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 . . ?
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 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Mg1 B1 H1A 74.5(12) . . ?
Mg1 B1 H1B 165.1(13) . . ?
Mg1 B1 H1C 59.5(11) . . ?
Mg1 B1 H1D 72.3(14) . . ?
H1A B1 H1B 112.7(17) . . ?
H1A B1 H1C 105.1(16) . . ?
H1A B1 H1D 111.1(18) . . ?
H1B B1 H1C 105.7(17) . . ?
H1B B1 H1D 114.6(19) . . ?
H1C B1 H1D 106.8(18) . . ?
O1 C38 H38A 110.6 . . ?
O1 C38 H38B 110.6 . . ?
O1 C38 C37 105.73(18) . . ?
H38A C38 H38B 108.7 . . ?
C37 C38 H38A 110.6 . . ?
C37 C38 H38B 110.6 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 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 . . ?
C38 C37 H37A 111.3 . . ?
C38 C37 H37B 111.3 . . ?
C38 C37 C36 102.33(19) . . ?
H37A C37 H37B 109.2 . . ?
C36 C37 H37A 111.3 . . ?
C36 C37 H37B 111.3 . . ?
C35 C36 C37 101.3(2) . . ?
C35 C36 H36A 111.5 . . ?
C35 C36 H36B 111.5 . . ?
C37 C36 H36A 111.5 . . ?
C37 C36 H36B 111.5 . . ?
H36A C36 H36B 109.3 . . ?

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
Mg1 O1 C35 C36 145.50(15) . . . . ?
Mg1 O1 C38 C37 -169.93(14) . . . . ?
Mg1 N2 C20 C21 -14.4(2) . . . . ?
Mg1 N2 C20 C19 168.97(14) . . . . ?
Mg1 N2 C16 C13 10.9(2) . . . . ?
Mg1 N2 C16 C17 -170.15(14) . . . . ?
Mg1 N1 C1 C2 87.9(2) . . . . ?
Mg1 N1 C1 C6 -89.5(2) . . . . ?
Mg1 N1 C13 C16 -11.08(19) . . . . ?
Mg1 N1 C13 C15 108.43(16) . . . . ?
Mg1 N1 C13 C14 -129.68(14) . . . . ?
Mg1 N3 C23 C28 -87.75(19) . . . . ?
Mg1 N3 C23 C24 89.62(19) . . . . ?
Mg1 N3 C21 C20 9.5(2) . . . . ?
Mg1 N3 C21 C22 -172.73(15) . . . . ?
O1 C35 C36 C37 37.0(2) . . . . ?
O1 C38 C37 C36 28.9(2) . . . . ?
N2 C20 C21 N3 1.7(2) . . . . ?
N2 C20 C21 C22 -176.23(17) . . . . ?
N2 C20 C19 C18 1.5(3) . . . . ?
N2 C16 C17 C18 -0.3(3) . . . . ?
N1 C1 C2 C7 -7.5(3) . . . . ?
N1 C1 C2 C3 176.14(17) . . . . ?
N1 C1 C6 C10 11.0(3) . . . . ?
N1 C1 C6 C5 -174.98(17) . . . . ?
N1 C13 C16 N2 -0.4(2) . . . . ?
N1 C13 C16 C17 -179.24(17) . . . . ?
N3 C23 C28 C27 179.74(16) . . . . ?
N3 C23 C28 C32 -1.7(3) . . . . ?
N3 C23 C24 C25 -178.31(16) . . . . ?
N3 C23 C24 C29 2.5(3) . . . . ?
C23 N3 C21 C20 -172.45(16) . . . . ?
C23 N3 C21 C22 5.3(3) . . . . ?
C23 C28 C27 C26 -2.1(3) . . . . ?
C23 C28 C32 C34 -101.0(2) . . . . ?
C23 C28 C32 C33 134.8(2) . . . . ?
C23 C24 C29 C31 114.9(2) . . . . ?
C23 C24 C29 C30 -122.5(2) . . . . ?
C20 N2 C16 C13 -178.03(16) . . . . ?
C20 N2 C16 C17 0.9(3) . . . . ?
C20 C19 C18 C17 -0.9(3) . . . . ?
C1 N1 C13 C16 169.48(15) . . . . ?
C1 N1 C13 C15 -71.0(2) . . . . ?
C1 N1 C13 C14 50.9(2) . . . . ?
C1 C2 C7 C8 131.6(2) . . . . ?
C1 C2 C7 C9 -106.3(2) . . . . ?
C1 C2 C3 C4 0.8(3) . . . . ?
C26 C25 C24 C23 -0.7(3) . . . . ?
C26 C25 C24 C29 178.52(18) . . . . ?
C13 N1 C1 C2 -92.7(2) . . . . ?
C13 N1 C1 C6 89.9(2) . . . . ?
C13 C16 C17 C18 178.55(19) . . . . ?
C25 C26 C27 C28 0.5(3) . . . . ?
C25 C24 C29 C31 -64.3(2) . . . . ?
C25 C24 C29 C30 58.3(2) . . . . ?
C16 N2 C20 C21 175.11(16) . . . . ?
C16 N2 C20 C19 -1.5(3) . . . . ?
C16 C17 C18 C19 0.3(3) . . . . ?
C28 C23 C24 C25 -1.0(3) . . . . ?
C28 C23 C24 C29 179.82(17) . . . . ?
C21 N3 C23 C28 94.4(2) . . . . ?
C21 N3 C23 C24 -88.2(2) . . . . ?
C21 C20 C19 C18 -174.74(18) . . . . ?
C24 C23 C28 C27 2.4(3) . . . . ?
C24 C23 C28 C32 -179.12(17) . . . . ?
C19 C20 C21 N3 178.28(18) . . . . ?
C19 C20 C21 C22 0.3(3) . . . . ?
C27 C26 C25 C24 1.0(3) . . . . ?
C27 C28 C32 C34 77.5(2) . . . . ?
C27 C28 C32 C33 -46.7(3) . . . . ?
C2 C1 C6 C10 -166.45(17) . . . . ?
C2 C1 C6 C5 7.5(3) . . . . ?
C32 C28 C27 C26 179.37(18) . . . . ?
C7 C2 C3 C4 -175.70(19) . . . . ?
C5 C4 C3 C2 3.7(3) . . . . ?
C6 C1 C2 C7 170.03(18) . . . . ?
C6 C1 C2 C3 -6.3(3) . . . . ?
C6 C5 C4 C3 -2.4(3) . . . . ?
C15 C13 C16 N2 -123.60(18) . . . . ?
C15 C13 C16 C17 57.5(2) . . . . ?
C14 C13 C16 N2 122.51(18) . . . . ?
C14 C13 C16 C17 -56.4(2) . . . . ?
C4 C5 C6 C1 -3.3(3) . . . . ?
C4 C5 C6 C10 170.99(19) . . . . ?
C3 C2 C7 C8 -52.0(3) . . . . ?
C3 C2 C7 C9 70.2(2) . . . . ?
C11 C10 C6 C1 110.4(2) . . . . ?
C11 C10 C6 C5 -63.7(2) . . . . ?
C35 O1 C38 C37 -6.0(2) . . . . ?
C12 C10 C6 C1 -128.0(2) . . . . ?
C12 C10 C6 C5 57.9(3) . . . . ?
C38 O1 C35 C36 -19.6(2) . . . . ?
C38 C37 C36 C35 -39.9(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mbx4
_database_code_depnum_ccdc_archive 'CCDC 2371035'
loop_
_audit_author_name
_audit_author_address
'Frederic Capet'
;CNRS, UCCS
France
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(PyA1)K(N(Si(CH3)3))2]2'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H88 K2 N6 Si4'
_chemical_formula_sum            'C50 H88 K2 N6 Si4'
_chemical_formula_weight         963.82

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8057(7)
_cell_length_b                   11.7125(8)
_cell_length_c                   13.2613(9)
_cell_angle_alpha                88.7038(10)
_cell_angle_beta                 71.4150(10)
_cell_angle_gamma                64.5690(9)
_cell_volume                     1423.85(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    9909
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      30.54

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_F_000             524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.282
_exptl_absorpt_coefficient_mu    0.287
_shelx_estimated_absorpt_T_min   0.904
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7177
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
36247 Corrected reflections written to file mbx4s.hkl 
Estimated minimum and maximum transmission:  0.7177  0.7461 
The ratio (0.9619) of these values is more reliable than their absolute values! 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36247
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.943
_diffrn_reflns_theta_max         30.540
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8597
_reflns_number_gt                7613
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A colorless crystal of approximate dimensions 0.282 x 0.294 x 0.358 mm 
was mounted in a cryoloop and transferred to a Bruker SMART APEX II 
diffractometer system.  The APEX2 program package was used to determine 
the unit-cell parameters and for data collection (20 sec/frame scan time).  
The raw frame data was processed using SAINT and SADABS to yield the 
reflection data file.  Subsequent calculations were carried out using 
the SHELXTL program package.  There were no systematic absences nor any 
diffraction symmetry other than the Friedel condition.  The centrosymmetric 
triclinic space group P-1  was assigned and later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral 
atoms were used throughout the analysis.  Hydrogen atom H1 was located from 
a difference-Fourier map and refined (x,y,z and Uiso).  The rest of the 
hydrogen atoms were included using a riding model.  The molecule was located 
about an inversion center.

Least-squares analysis yielded wR2 = 0.0758 and Goof = 1.068 for 295 variables 
refined against 8597 data (0.70 Ã?), R1 = 0.0277 for those 7613 data 
with I > 2.0sigma(I).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0339P)²+0.3775P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8597
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form 
_vrf_PLAT414_mbx4                
; 
PROBLEM:  Short Intra D-H..H-X H1 ..H7 . 1.88 Ang. 
RESPONSE: ... The N-H hydrogen atom was located in a difference map 
and then refined. 
;
# end Validation Reply Form 

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
K1 K 0.49359(2) 0.14013(2) 0.41934(2) 0.01575(5) Uani 1 1 d . . . . .
Si1 Si 0.17124(3) 0.09745(2) 0.55740(2) 0.01326(5) Uani 1 1 d . . . . .
Si2 Si 0.28501(3) 0.18568(2) 0.71003(2) 0.01380(6) Uani 1 1 d . . . . .
N1 N 0.49179(8) 0.30918(7) 0.24718(6) 0.01381(14) Uani 1 1 d . . . . .
H1 H 0.4077(14) 0.3062(12) 0.2679(10) 0.017(3) Uiso 1 1 d . . . . .
N2 N 0.26641(8) 0.41157(7) 0.42764(6) 0.01610(14) Uani 1 1 d . . . . .
N3 N 0.29404(8) 0.11572(7) 0.59761(6) 0.01374(14) Uani 1 1 d . . . . .
C1 C 0.56469(10) 0.26804(8) 0.13398(7) 0.01467(16) Uani 1 1 d . . . . .
C2 C 0.48893(10) 0.25447(9) 0.06946(7) 0.01758(17) Uani 1 1 d . . . . .
C3 C 0.56675(11) 0.20421(10) -0.03871(8) 0.02125(19) Uani 1 1 d . . . . .
H3 H 0.5180 0.1906 -0.0820 0.026 Uiso 1 1 calc R U . . .
C4 C 0.71333(11) 0.17382(10) -0.08400(8) 0.02234(19) Uani 1 1 d . . . . .
H4 H 0.7641 0.1411 -0.1579 0.027 Uiso 1 1 calc R U . . .
C5 C 0.78552(11) 0.19156(9) -0.02056(8) 0.02010(18) Uani 1 1 d . . . . .
H5 H 0.8854 0.1732 -0.0523 0.024 Uiso 1 1 calc R U . . .
C6 C 0.71436(10) 0.23586(9) 0.08889(7) 0.01605(16) Uani 1 1 d . . . . .
C7 C 0.32613(11) 0.29113(11) 0.11177(8) 0.02241(19) Uani 1 1 d . . . . .
H7 H 0.2850 0.3368 0.1863 0.027 Uiso 1 1 calc R U . . .
C8 C 0.24687(12) 0.38276(12) 0.04382(10) 0.0304(2) Uani 1 1 d . . . . .
H8A H 0.2669 0.4571 0.0403 0.046 Uiso 1 1 calc R U . . .
H8B H 0.1416 0.4108 0.0766 0.046 Uiso 1 1 calc R U . . .
H8C H 0.2814 0.3389 -0.0289 0.046 Uiso 1 1 calc R U . . .
C9 C 0.29882(13) 0.17275(12) 0.11809(9) 0.0298(2) Uani 1 1 d . . . . .
H9A H 0.3402 0.1249 0.0462 0.045 Uiso 1 1 calc R U . . .
H9B H 0.1936 0.1991 0.1465 0.045 Uiso 1 1 calc R U . . .
H9C H 0.3452 0.1186 0.1656 0.045 Uiso 1 1 calc R U . . .
C10 C 0.80113(10) 0.24549(9) 0.15621(8) 0.01786(17) Uani 1 1 d . . . . .
H10 H 0.7388 0.2609 0.2335 0.021 Uiso 1 1 calc R U . . .
C11 C 0.83807(12) 0.35844(11) 0.13309(9) 0.0246(2) Uani 1 1 d . . . . .
H11A H 0.8989 0.3459 0.0576 0.037 Uiso 1 1 calc R U . . .
H11B H 0.8911 0.3639 0.1791 0.037 Uiso 1 1 calc R U . . .
H11C H 0.7477 0.4377 0.1479 0.037 Uiso 1 1 calc R U . . .
C12 C 0.94097(11) 0.12146(10) 0.13896(9) 0.0255(2) Uani 1 1 d . . . . .
H12A H 0.9165 0.0498 0.1518 0.038 Uiso 1 1 calc R U . . .
H12B H 0.9884 0.1280 0.1890 0.038 Uiso 1 1 calc R U . . .
H12C H 1.0074 0.1075 0.0651 0.038 Uiso 1 1 calc R U . . .
C13 C 0.40175(12) 0.54049(9) 0.21599(8) 0.02226(19) Uani 1 1 d . . . . .
H13A H 0.4750 0.5174 0.1438 0.033 Uiso 1 1 calc R U . . .
H13B H 0.3831 0.6239 0.2470 0.033 Uiso 1 1 calc R U . . .
H13C H 0.3111 0.5445 0.2117 0.033 Uiso 1 1 calc R U . . .
C14 C 0.45814(10) 0.43973(8) 0.28722(7) 0.01553(16) Uani 1 1 d . . . . .
H14 H 0.5492 0.4385 0.2919 0.019 Uiso 1 1 calc R U . . .
C15 C 0.34569(9) 0.47649(8) 0.39969(7) 0.01428(16) Uani 1 1 d . . . . .
C16 C 0.32304(11) 0.57779(9) 0.46794(8) 0.01914(18) Uani 1 1 d . . . . .
H16 H 0.3834 0.6200 0.4473 0.023 Uiso 1 1 calc R U . . .
C17 C 0.21108(12) 0.61591(9) 0.56641(8) 0.02129(19) Uani 1 1 d . . . . .
H17 H 0.1928 0.6854 0.6138 0.026 Uiso 1 1 calc R U . . .
C18 C 0.12631(11) 0.55114(9) 0.59454(8) 0.01967(18) Uani 1 1 d . . . . .
H18 H 0.0476 0.5763 0.6608 0.024 Uiso 1 1 calc R U . . .
C19 C 0.15908(10) 0.44902(9) 0.52380(8) 0.01834(17) Uani 1 1 d . . . . .
H19 H 0.1029 0.4029 0.5441 0.022 Uiso 1 1 calc R U . . .
C20 C -0.02661(10) 0.20654(10) 0.63212(8) 0.02114(18) Uani 1 1 d . . . . .
H20A H -0.0496 0.1966 0.7085 0.032 Uiso 1 1 calc R U . . .
H20B H -0.0878 0.1847 0.6033 0.032 Uiso 1 1 calc R U . . .
H20C H -0.0453 0.2951 0.6234 0.032 Uiso 1 1 calc R U . . .
C21 C 0.18400(11) -0.06878(9) 0.56612(8) 0.02142(19) Uani 1 1 d . . . . .
H21A H 0.2755 -0.1301 0.5129 0.032 Uiso 1 1 calc R U . . .
H21B H 0.1015 -0.0711 0.5518 0.032 Uiso 1 1 calc R U . . .
H21C H 0.1816 -0.0910 0.6382 0.032 Uiso 1 1 calc R U . . .
C22 C 0.20178(11) 0.11733(10) 0.41077(7) 0.01975(18) Uani 1 1 d . . . . .
H22A H 0.1964 0.2021 0.3993 0.030 Uiso 1 1 calc R U . . .
H22B H 0.1266 0.1084 0.3903 0.030 Uiso 1 1 calc R U . . .
H22C H 0.2982 0.0518 0.3668 0.030 Uiso 1 1 calc R U . . .
C23 C 0.10167(11) 0.31397(10) 0.79575(8) 0.02106(18) Uani 1 1 d . . . . .
H23A H 0.0600 0.3767 0.7510 0.032 Uiso 1 1 calc R U . . .
H23B H 0.1136 0.3563 0.8524 0.032 Uiso 1 1 calc R U . . .
H23C H 0.0362 0.2755 0.8283 0.032 Uiso 1 1 calc R U . . .
C24 C 0.34630(13) 0.06879(10) 0.80511(8) 0.0247(2) Uani 1 1 d . . . . .
H24A H 0.2910 0.0187 0.8199 0.037 Uiso 1 1 calc R U . . .
H24B H 0.3291 0.1156 0.8724 0.037 Uiso 1 1 calc R U . . .
H24C H 0.4505 0.0115 0.7723 0.037 Uiso 1 1 calc R U . . .
C25 C 0.41224(11) 0.26356(10) 0.67903(8) 0.02117(18) Uani 1 1 d . . . . .
H25A H 0.5128 0.1986 0.6439 0.032 Uiso 1 1 calc R U . . .
H25B H 0.4043 0.3046 0.7459 0.032 Uiso 1 1 calc R U . . .
H25C H 0.3854 0.3278 0.6312 0.032 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
K1 N3 2.7513(8) . ?
K1 N3 2.8446(8) 2_656 ?
K1 N1 2.9873(8) . ?
K1 N2 3.0474(8) . ?
K1 K1 3.8537(4) 2_656 ?
Si1 N3 1.6706(8) . ?
Si1 C20 1.8831(10) . ?
Si1 C22 1.8923(10) . ?
Si1 C21 1.8953(10) . ?
Si1 K1 3.6018(4) 2_656 ?
Si2 N3 1.6725(8) . ?
Si2 C23 1.8867(10) . ?
Si2 C24 1.8916(10) . ?
Si2 C25 1.8950(10) . ?
Si2 K1 3.6150(4) 2_656 ?
N1 C1 1.4349(11) . ?
N1 C14 1.4793(11) . ?
N2 C15 1.3394(12) . ?
N2 C19 1.3451(12) . ?
N3 K1 2.8446(8) 2_656 ?
C1 C6 1.4090(12) . ?
C1 C2 1.4114(13) . ?
C2 C3 1.3984(13) . ?
C2 C7 1.5254(13) . ?
C3 C4 1.3840(14) . ?
C4 C5 1.3873(14) . ?
C5 C6 1.3954(13) . ?
C6 C10 1.5224(13) . ?
C7 C9 1.5319(16) . ?
C7 C8 1.5350(15) . ?
C10 C12 1.5346(14) . ?
C10 C11 1.5365(14) . ?
C13 C14 1.5347(13) . ?
C14 C15 1.5201(12) . ?
C15 C16 1.3945(13) . ?
C16 C17 1.3869(14) . ?
C17 C18 1.3856(14) . ?
C18 C19 1.3825(13) . ?
C21 K1 3.2853(10) 2_656 ?
C24 K1 3.3543(11) 2_656 ?

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
N3 K1 N3 92.97(2) . 2_656 ?
N3 K1 N1 137.69(2) . . ?
N3 K1 N1 126.14(2) 2_656 . ?
N3 K1 N2 88.32(2) . . ?
N3 K1 N2 177.49(2) 2_656 . ?
N1 K1 N2 52.01(2) . . ?
N3 K1 K1 47.490(16) . 2_656 ?
N3 K1 K1 45.478(16) 2_656 2_656 ?
N1 K1 K1 164.427(17) . 2_656 ?
N2 K1 K1 135.766(17) . 2_656 ?
N3 Si1 C20 116.99(4) . . ?
N3 Si1 C22 111.51(4) . . ?
C20 Si1 C22 106.12(4) . . ?
N3 Si1 C21 112.65(4) . . ?
C20 Si1 C21 104.28(5) . . ?
C22 Si1 C21 104.23(5) . . ?
N3 Si1 K1 50.39(3) . 2_656 ?
C20 Si1 K1 145.22(3) . 2_656 ?
C22 Si1 K1 108.59(3) . 2_656 ?
C21 Si1 K1 64.99(3) . 2_656 ?
N3 Si2 C23 117.44(4) . . ?
N3 Si2 C24 113.00(4) . . ?
C23 Si2 C24 104.48(5) . . ?
N3 Si2 C25 110.99(4) . . ?
C23 Si2 C25 105.28(5) . . ?
C24 Si2 C25 104.56(5) . . ?
N3 Si2 K1 49.99(3) . 2_656 ?
C23 Si2 K1 148.90(3) . 2_656 ?
C24 Si2 K1 66.77(3) . 2_656 ?
C25 Si2 K1 105.82(3) . 2_656 ?
C1 N1 C14 117.44(7) . . ?
C1 N1 K1 126.10(5) . . ?
C14 N1 K1 112.71(5) . . ?
C15 N2 C19 118.03(8) . . ?
C15 N2 K1 103.27(5) . . ?
C19 N2 K1 109.83(6) . . ?
Si1 N3 Si2 133.68(5) . . ?
Si1 N3 K1 107.49(3) . . ?
Si2 N3 K1 111.54(4) . . ?
Si1 N3 K1 102.70(3) . 2_656 ?
Si2 N3 K1 103.24(3) . 2_656 ?
K1 N3 K1 87.03(2) . 2_656 ?
C6 C1 C2 120.39(8) . . ?
C6 C1 N1 119.20(8) . . ?
C2 C1 N1 120.35(8) . . ?
C3 C2 C1 118.56(9) . . ?
C3 C2 C7 118.08(8) . . ?
C1 C2 C7 123.36(8) . . ?
C4 C3 C2 121.41(9) . . ?
C3 C4 C5 119.45(9) . . ?
C4 C5 C6 121.30(9) . . ?
C5 C6 C1 118.79(8) . . ?
C5 C6 C10 119.13(8) . . ?
C1 C6 C10 122.07(8) . . ?
C2 C7 C9 111.26(9) . . ?
C2 C7 C8 111.29(9) . . ?
C9 C7 C8 111.06(9) . . ?
C6 C10 C12 111.83(8) . . ?
C6 C10 C11 111.30(8) . . ?
C12 C10 C11 110.16(8) . . ?
N1 C14 C15 108.28(7) . . ?
N1 C14 C13 114.13(8) . . ?
C15 C14 C13 109.58(7) . . ?
N2 C15 C16 122.19(8) . . ?
N2 C15 C14 117.24(8) . . ?
C16 C15 C14 120.50(8) . . ?
C17 C16 C15 119.01(9) . . ?
C18 C17 C16 118.99(9) . . ?
C19 C18 C17 118.37(9) . . ?
N2 C19 C18 123.35(9) . . ?
Si1 C21 K1 83.49(3) . 2_656 ?
Si2 C24 K1 82.02(3) . 2_656 ?

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
C20 Si1 N3 Si2 18.13(8) . . . . ?
C22 Si1 N3 Si2 140.51(6) . . . . ?
C21 Si1 N3 Si2 -102.70(7) . . . . ?
K1 Si1 N3 Si2 -122.68(7) 2_656 . . . ?
C20 Si1 N3 K1 -128.32(4) . . . . ?
C22 Si1 N3 K1 -5.93(5) . . . . ?
C21 Si1 N3 K1 110.86(4) . . . . ?
K1 Si1 N3 K1 90.88(3) 2_656 . . . ?
C20 Si1 N3 K1 140.80(4) . . . 2_656 ?
C22 Si1 N3 K1 -96.82(4) . . . 2_656 ?
C21 Si1 N3 K1 19.98(5) . . . 2_656 ?
C23 Si2 N3 Si1 -22.98(8) . . . . ?
C24 Si2 N3 Si1 98.79(7) . . . . ?
C25 Si2 N3 Si1 -144.12(6) . . . . ?
K1 Si2 N3 Si1 122.48(8) 2_656 . . . ?
C23 Si2 N3 K1 122.49(4) . . . . ?
C24 Si2 N3 K1 -115.74(5) . . . . ?
C25 Si2 N3 K1 1.35(5) . . . . ?
K1 Si2 N3 K1 -92.05(4) 2_656 . . . ?
C23 Si2 N3 K1 -145.46(4) . . . 2_656 ?
C24 Si2 N3 K1 -23.69(5) . . . 2_656 ?
C25 Si2 N3 K1 93.39(4) . . . 2_656 ?
C14 N1 C1 C6 74.73(10) . . . . ?
K1 N1 C1 C6 -81.78(9) . . . . ?
C14 N1 C1 C2 -108.11(10) . . . . ?
K1 N1 C1 C2 95.38(9) . . . . ?
C6 C1 C2 C3 2.31(13) . . . . ?
N1 C1 C2 C3 -174.82(8) . . . . ?
C6 C1 C2 C7 -178.07(9) . . . . ?
N1 C1 C2 C7 4.80(14) . . . . ?
C1 C2 C3 C4 -3.14(15) . . . . ?
C7 C2 C3 C4 177.22(9) . . . . ?
C2 C3 C4 C5 1.05(16) . . . . ?
C3 C4 C5 C6 1.96(15) . . . . ?
C4 C5 C6 C1 -2.73(14) . . . . ?
C4 C5 C6 C10 176.09(9) . . . . ?
C2 C1 C6 C5 0.55(13) . . . . ?
N1 C1 C6 C5 177.71(8) . . . . ?
C2 C1 C6 C10 -178.23(8) . . . . ?
N1 C1 C6 C10 -1.07(13) . . . . ?
C3 C2 C7 C9 70.48(11) . . . . ?
C1 C2 C7 C9 -109.14(10) . . . . ?
C3 C2 C7 C8 -53.94(13) . . . . ?
C1 C2 C7 C8 126.44(10) . . . . ?
C5 C6 C10 C12 -50.09(12) . . . . ?
C1 C6 C10 C12 128.69(9) . . . . ?
C5 C6 C10 C11 73.59(11) . . . . ?
C1 C6 C10 C11 -107.62(10) . . . . ?
C1 N1 C14 C15 163.92(7) . . . . ?
K1 N1 C14 C15 -36.52(8) . . . . ?
C1 N1 C14 C13 41.59(11) . . . . ?
K1 N1 C14 C13 -158.85(6) . . . . ?
C19 N2 C15 C16 1.94(13) . . . . ?
K1 N2 C15 C16 -119.42(8) . . . . ?
C19 N2 C15 C14 -175.14(8) . . . . ?
K1 N2 C15 C14 63.50(8) . . . . ?
N1 C14 C15 N2 -20.49(10) . . . . ?
C13 C14 C15 N2 104.58(9) . . . . ?
N1 C14 C15 C16 162.38(8) . . . . ?
C13 C14 C15 C16 -72.56(11) . . . . ?
N2 C15 C16 C17 -2.53(14) . . . . ?
C14 C15 C16 C17 174.46(8) . . . . ?
C15 C16 C17 C18 0.80(14) . . . . ?
C16 C17 C18 C19 1.33(14) . . . . ?
C15 N2 C19 C18 0.36(14) . . . . ?
K1 N2 C19 C18 118.29(9) . . . . ?
C17 C18 C19 N2 -2.00(15) . . . . ?
N3 Si1 C21 K1 -16.89(4) . . . 2_656 ?
C20 Si1 C21 K1 -144.74(3) . . . 2_656 ?
C22 Si1 C21 K1 104.16(4) . . . 2_656 ?
N3 Si2 C24 K1 19.57(4) . . . 2_656 ?
C23 Si2 C24 K1 148.38(3) . . . 2_656 ?
C25 Si2 C24 K1 -101.25(4) . . . 2_656 ?

_refine_diff_density_max         0.438
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.045



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Pyrophoric
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mbx06_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 2371037'
loop_
_audit_author_name
_audit_author_address
'Frederic Capet'
;CNRS, UCCS
France
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_audit_creation_date             2023-07-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        (PyA1)2Nd2(BH4)4(THF)2
_chemical_formula_moiety         'C46 H82 B4 N4 Nd2 O2 [+ solvent]'
_chemical_formula_sum            'C46 H82 B4 N4 Nd2 O2 [+ solvent]'
_chemical_formula_weight         1046.81
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.8551(9)
_cell_length_b                   15.2082(14)
_cell_length_c                   20.438(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.420(4)
_cell_angle_gamma                90
_cell_volume                     2991.5(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    100.05
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.44
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0477 after correction.
The Ratio of minimum to maximum transmission is 0.9017.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            74200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_min         1.683
_diffrn_ambient_temperature      100.05
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5081
_reflns_number_total             6095
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2019.11-0 (Bruker-AXS, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'

_refine_diff_density_max         1.619
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6095
_refine_ls_number_restraints     150
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0492
_refine_ls_restrained_S_all      1.167
_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)+(0.0409P)²+12.1450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1221
_refine_special_details          
;At the end of the refinement, five residual electron density
 peaks suggested the presence of a molecule of solvent
 (pentane or diethyl ether) highly disordered. We used the SQUEEZE
 procedure (Platon) to suppress its contribution because it was
 impossible to modelize il precisely.
 
 It was not possible to locate the 4 remaining H atomes on B2.,SQUEEZE,disorder
;
_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. Restrained distances
 O1A-C23A = O1A-C20A
 1.44 with sigma of 0.02
 C23A-C22A = C21A-C20A
 1.53 with sigma of 0.02
 C22A-C21A
 1.54 with sigma of 0.02
 O1B-C20B = O1B-C23B
 1.44 with sigma of 0.02
 C20B-C21B = C22B-C23B
 1.53 with sigma of 0.02
 C21B-C22B
 1.54 with sigma of 0.02
 O1A-C22A = O1A-C21A = C23A-C21A = C22A-C20A
 2.38 with sigma of 0.04
 O1B-C21B = O1B-C22B = C20B-C22B = C21B-C23B
 2.38 with sigma of 0.04
 O1B-C21B \\sim O1B-C22B
 with sigma of 0.04
 O1B-C20B \\sim O1B-C23B
 with sigma of 0.02
 C21B-C23B \\sim C20B-C22B
 with sigma of 0.04
 C23A-C22A \\sim C22A-C21A \\sim C21A-C20A
 with sigma of 0.02
 O1A-C23A \\sim O1A-C20A
 with sigma of 0.02
 O1A-C22A \\sim O1A-C21A
 with sigma of 0.04
 C22A-C20A \\sim C23A-C21A
 with sigma of 0.04
 C20B-C21B \\sim C21B-C22B \\sim C22B-C23B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1A \\sim C23A \\sim C22A \\sim C21A \\sim C20A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1B \\sim C20B \\sim C21B \\sim C22B \\sim C23B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(O1A) = Uanis(O1B)
Uanis(C23A) = Uanis(C23B)
Uanis(C22A) = Uanis(C22B)
Uanis(C20B) = Uanis(C20A)
Uanis(C21A) = Uanis(C21B)
4. Rigid body (RIGU) restrains
 O1A, C23A, C22A, C21A, C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1B, C20B, C21B, C22B, C23B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1B)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=Sof(H21C)=Sof(H21D)=
 Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=Sof(H23D)=1-FVAR(1)
 Sof(O1A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C17(H17), C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C23A(H23A,H23B), C22A(H22A,H22B), C21A(H21A,H21B), C20A(H20A,H20B), C20B(H20C,
 H20D), C21B(H21C,H21D), C22B(H22C,H22D), C23B(H23C,H23D)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C1(H1), C3(H3), C10(H10), C12(H12), C11(H11)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Nd1 Nd 0.50962(3) 0.55194(2) 0.39612(2) 0.03477(11) Uani 1 1 d . . . . .
N1 N 0.7479(4) 0.4754(3) 0.4120(2) 0.0366(10) Uani 1 1 d . . . . .
N2 N 0.6638(5) 0.6277(3) 0.3506(2) 0.0394(10) Uani 1 1 d . . . . .
C4 C 0.9869(5) 0.4904(4) 0.4077(3) 0.0418(14) Uani 1 1 d . . . . .
H4 H 1.058113 0.523843 0.394725 0.050 Uiso 1 1 calc R U . . .
C5 C 0.8498(5) 0.5212(4) 0.3935(2) 0.0346(11) Uani 1 1 d . . . . .
C13 C 0.6659(7) 0.7894(4) 0.3544(3) 0.0499(15) Uani 1 1 d . . . . .
C2 C 0.9139(6) 0.3640(4) 0.4583(3) 0.0426(13) Uani 1 1 d . . . . .
H2 H 0.933003 0.308993 0.480384 0.051 Uiso 1 1 calc R U . . .
C1 C 0.7824(6) 0.3975(4) 0.4437(3) 0.0397(12) Uani 1 1 d . . . . .
H1 H 0.710675 0.364370 0.456522 0.048 Uiso 1 1 calc R U . . .
C8 C 0.6272(6) 0.7117(4) 0.3190(3) 0.0404(13) Uani 1 1 d . . . . .
C3 C 1.0180(6) 0.4122(4) 0.4402(3) 0.0434(14) Uani 1 1 d . . . . .
H3 H 1.110980 0.391181 0.450255 0.052 Uiso 1 1 calc R U . . .
C9 C 0.5593(7) 0.7163(4) 0.2508(3) 0.0511(15) Uani 1 1 d . . . . .
C6 C 0.8104(6) 0.6069(4) 0.3566(3) 0.0451(14) Uani 1 1 d . . . . .
H6 H 0.865607 0.654664 0.383605 0.054 Uiso 1 1 calc R U . . .
C10 C 0.5278(8) 0.7982(5) 0.2210(3) 0.066(2) Uani 1 1 d . . . . .
H10 H 0.480706 0.801279 0.175280 0.079 Uiso 1 1 calc R U . . .
C17 C 0.7398(8) 0.7900(4) 0.4285(3) 0.0554(17) Uani 1 1 d . . . . .
H17 H 0.754143 0.727635 0.443970 0.066 Uiso 1 1 calc R U . . .
C12 C 0.6331(8) 0.8702(4) 0.3229(3) 0.0602(18) Uani 1 1 d . . . . .
H12 H 0.658528 0.923124 0.347177 0.072 Uiso 1 1 calc R U . . .
C18 C 0.6469(11) 0.8350(5) 0.4693(4) 0.083(3) Uani 1 1 d . . . . .
H18A H 0.682338 0.822989 0.517040 0.124 Uiso 1 1 calc R U . . .
H18B H 0.551949 0.812219 0.455592 0.124 Uiso 1 1 calc R U . . .
H18C H 0.646674 0.898542 0.461491 0.124 Uiso 1 1 calc R U . . .
C7 C 0.8554(8) 0.6027(5) 0.2886(3) 0.067(2) Uani 1 1 d . . . . .
H7A H 0.806602 0.554335 0.261696 0.100 Uiso 1 1 calc R U . . .
H7B H 0.955860 0.592815 0.296437 0.100 Uiso 1 1 calc R U . . .
H7C H 0.832172 0.658311 0.264547 0.100 Uiso 1 1 calc R U . . .
B2 B 0.4038(7) 0.3997(6) 0.4626(3) 0.0510(18) Uani 1 1 d . . . . .
C19 C 0.8810(8) 0.8343(5) 0.4391(4) 0.074(2) Uani 1 1 d . . . . .
H19A H 0.869917 0.893959 0.420635 0.110 Uiso 1 1 calc R U . . .
H19B H 0.941681 0.800370 0.416279 0.110 Uiso 1 1 calc R U . . .
H19C H 0.922408 0.837024 0.487115 0.110 Uiso 1 1 calc R U . . .
C14 C 0.5106(10) 0.6372(5) 0.2077(4) 0.077(2) Uani 1 1 d . . . . .
H14 H 0.540315 0.584008 0.235883 0.092 Uiso 1 1 calc R U . . .
C11 C 0.5631(8) 0.8740(5) 0.2560(4) 0.067(2) Uani 1 1 d . . . . .
H11 H 0.540229 0.929318 0.234835 0.081 Uiso 1 1 calc R U . . .
B1 B 0.2776(8) 0.6446(6) 0.3706(5) 0.058(2) Uani 1 1 d . . . . .
C15 C 0.3496(12) 0.6328(7) 0.1850(4) 0.110(4) Uani 1 1 d . . . . .
H15A H 0.316187 0.683647 0.156653 0.166 Uiso 1 1 calc R U . . .
H15B H 0.308166 0.633367 0.224502 0.166 Uiso 1 1 calc R U . . .
H15C H 0.322996 0.578549 0.159568 0.166 Uiso 1 1 calc R U . . .
C16 C 0.5748(14) 0.6296(7) 0.1466(4) 0.119(4) Uani 1 1 d . . . . .
H16A H 0.553747 0.571568 0.126002 0.178 Uiso 1 1 calc R U . . .
H16B H 0.675736 0.636932 0.160229 0.178 Uiso 1 1 calc R U . . .
H16C H 0.536315 0.675330 0.114080 0.178 Uiso 1 1 calc R U . . .
O1A O 0.451(3) 0.449(3) 0.304(2) 0.057(2) Uani 0.506(17) 1 d D U P A 1
C23A C 0.548(2) 0.396(2) 0.2757(16) 0.080(4) Uani 0.506(17) 1 d D U P A 1
H23A H 0.589308 0.347873 0.306292 0.096 Uiso 0.506(17) 1 calc R U P A 1
H23B H 0.623041 0.432303 0.264442 0.096 Uiso 0.506(17) 1 calc R U P A 1
C22A C 0.450(2) 0.3601(17) 0.2124(11) 0.119(4) Uani 0.506(17) 1 d D U P A 1
H22A H 0.489830 0.309002 0.193168 0.143 Uiso 0.506(17) 1 calc R U P A 1
H22B H 0.422257 0.405932 0.177710 0.143 Uiso 0.506(17) 1 calc R U P A 1
C21A C 0.326(2) 0.3329(14) 0.2461(13) 0.117(4) Uani 0.506(17) 1 d D U P A 1
H21A H 0.242980 0.313492 0.212913 0.141 Uiso 0.506(17) 1 calc R U P A 1
H21B H 0.353512 0.287484 0.281125 0.141 Uiso 0.506(17) 1 calc R U P A 1
C20A C 0.308(3) 0.4228(17) 0.2749(17) 0.072(3) Uani 0.506(17) 1 d D U P A 1
H20A H 0.263219 0.464419 0.239523 0.086 Uiso 0.506(17) 1 calc R U P A 1
H20B H 0.251551 0.419362 0.309594 0.086 Uiso 0.506(17) 1 calc R U P A 1
O1B O 0.443(3) 0.449(3) 0.298(2) 0.057(2) Uani 0.494(17) 1 d D U P A 2
C20B C 0.306(3) 0.408(2) 0.2786(16) 0.072(3) Uani 0.494(17) 1 d D U P A 2
H20C H 0.230332 0.451724 0.273731 0.086 Uiso 0.494(17) 1 calc R U P A 2
H20D H 0.292707 0.362631 0.311595 0.086 Uiso 0.494(17) 1 calc R U P A 2
C21B C 0.313(2) 0.3662(16) 0.2110(12) 0.117(4) Uani 0.494(17) 1 d D U P A 2
H21C H 0.314249 0.410312 0.175527 0.141 Uiso 0.494(17) 1 calc R U P A 2
H21D H 0.238893 0.322252 0.195636 0.141 Uiso 0.494(17) 1 calc R U P A 2
C22B C 0.461(2) 0.3229(14) 0.2396(13) 0.119(4) Uani 0.494(17) 1 d D U P A 2
H22C H 0.458594 0.280681 0.276131 0.143 Uiso 0.494(17) 1 calc R U P A 2
H22D H 0.498406 0.293439 0.203943 0.143 Uiso 0.494(17) 1 calc R U P A 2
C23B C 0.545(3) 0.407(2) 0.2656(18) 0.080(4) Uani 0.494(17) 1 d D U P A 2
H23C H 0.631990 0.392508 0.298159 0.096 Uiso 0.494(17) 1 calc R U P A 2
H23D H 0.565956 0.442451 0.228671 0.096 Uiso 0.494(17) 1 calc R U P A 2
H1A H 0.327(8) 0.621(5) 0.422(4) 0.08(2) Uiso 1 1 d . . . . .
H1B H 0.365(10) 0.669(6) 0.359(4) 0.11(3) Uiso 1 1 d . . . . .
H1C H 0.272(9) 0.589(6) 0.339(4) 0.09(3) Uiso 1 1 d . . . . .
H1D H 0.193(8) 0.685(5) 0.363(4) 0.07(2) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Nd1 N1 2.579(4) . ?
Nd1 N2 2.260(4) . ?
Nd1 B2 2.985(7) . ?
Nd1 B2 2.923(7) 3_666 ?
Nd1 B1 2.641(8) . ?
Nd1 O1A 2.42(2) . ?
Nd1 O1B 2.52(2) . ?
Nd1 H1A 2.24(7) . ?
Nd1 H1B 2.31(9) . ?
Nd1 H1C 2.45(9) . ?
N1 C5 1.341(7) . ?
N1 C1 1.357(7) . ?
N2 C8 1.442(7) . ?
N2 C6 1.459(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.400(8) . ?
C4 C3 1.364(9) . ?
C5 C6 1.515(8) . ?
C13 C8 1.396(8) . ?
C13 C17 1.533(8) . ?
C13 C12 1.393(8) . ?
C2 H2 0.9500 . ?
C2 C1 1.365(8) . ?
C2 C3 1.374(8) . ?
C1 H1 0.9500 . ?
C8 C9 1.411(8) . ?
C3 H3 0.9500 . ?
C9 C10 1.393(9) . ?
C9 C14 1.508(9) . ?
C6 H6 1.0000 . ?
C6 C7 1.548(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.362(10) . ?
C17 H17 1.0000 . ?
C17 C18 1.527(10) . ?
C17 C19 1.519(10) . ?
C12 H12 0.9500 . ?
C12 C11 1.394(9) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C14 H14 1.0000 . ?
C14 C15 1.556(13) . ?
C14 C16 1.521(12) . ?
C11 H11 0.9500 . ?
B1 H1A 1.11(8) . ?
B1 H1B 1.01(9) . ?
B1 H1C 1.05(9) . ?
B1 H1D 1.02(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O1A C23A 1.460(13) . ?
O1A C20A 1.462(14) . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C23A C22A 1.538(14) . ?
C22A H22A 0.9900 . ?
C22A H22B 0.9900 . ?
C22A C21A 1.577(14) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C21A C20A 1.516(14) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
O1B C20B 1.467(14) . ?
O1B C23B 1.464(13) . ?
C20B H20C 0.9900 . ?
C20B H20D 0.9900 . ?
C20B C21B 1.534(14) . ?
C21B H21C 0.9900 . ?
C21B H21D 0.9900 . ?
C21B C22B 1.596(14) . ?
C22B H22C 0.9900 . ?
C22B H22D 0.9900 . ?
C22B C23B 1.546(14) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?

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 Nd1 B2 89.44(18) . . ?
N1 Nd1 B2 85.68(18) . 3_666 ?
N1 Nd1 B1 172.9(2) . . ?
N1 Nd1 H1A 160(2) . . ?
N1 Nd1 H1B 151(2) . . ?
N1 Nd1 H1C 157(2) . . ?
N2 Nd1 N1 66.89(15) . . ?
N2 Nd1 B2 156.16(19) . . ?
N2 Nd1 B2 101.45(17) . 3_666 ?
N2 Nd1 B1 106.1(2) . . ?
N2 Nd1 O1A 94.6(10) . . ?
N2 Nd1 O1B 94.0(10) . . ?
N2 Nd1 H1A 120(2) . . ?
N2 Nd1 H1B 84(2) . . ?
N2 Nd1 H1C 110(2) . . ?
B2 Nd1 B2 78.6(2) 3_666 . ?
B2 Nd1 H1A 83(2) . . ?
B2 Nd1 H1A 74(2) 3_666 . ?
B2 Nd1 H1B 120(2) . . ?
B2 Nd1 H1B 99(2) 3_666 . ?
B2 Nd1 H1C 90(2) . . ?
B2 Nd1 H1C 117(2) 3_666 . ?
B1 Nd1 B2 96.7(3) . 3_666 ?
B1 Nd1 B2 97.5(2) . . ?
B1 Nd1 H1A 25(2) . . ?
B1 Nd1 H1B 22(2) . . ?
B1 Nd1 H1C 23(2) . . ?
O1A Nd1 N1 82.2(8) . . ?
O1A Nd1 B2 154.2(13) . 3_666 ?
O1A Nd1 B2 78.6(12) . . ?
O1A Nd1 B1 98.1(9) . . ?
O1A Nd1 H1A 115(2) . . ?
O1A Nd1 H1B 103(2) . . ?
O1A Nd1 H1C 75(2) . . ?
O1B Nd1 N1 84.0(8) . . ?
O1B Nd1 B2 156.2(13) . 3_666 ?
O1B Nd1 B2 80.0(12) . . ?
O1B Nd1 B1 96.2(9) . . ?
O1B Nd1 H1A 113(2) . . ?
O1B Nd1 H1B 100(2) . . ?
O1B Nd1 H1C 73(2) . . ?
H1A Nd1 H1B 41(3) . . ?
H1A Nd1 H1C 43(3) . . ?
H1B Nd1 H1C 37(3) . . ?
C5 N1 Nd1 116.5(3) . . ?
C5 N1 C1 117.5(5) . . ?
C1 N1 Nd1 125.6(3) . . ?
C8 N2 Nd1 120.7(4) . . ?
C8 N2 C6 112.2(4) . . ?
C6 N2 Nd1 126.6(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(5) . . ?
N1 C5 C4 121.0(5) . . ?
N1 C5 C6 117.4(5) . . ?
C4 C5 C6 121.6(5) . . ?
C8 C13 C17 122.4(5) . . ?
C12 C13 C8 119.8(5) . . ?
C12 C13 C17 117.7(6) . . ?
C1 C2 H2 121.0 . . ?
C1 C2 C3 118.1(6) . . ?
C3 C2 H2 121.0 . . ?
N1 C1 C2 124.0(5) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C13 C8 N2 120.2(5) . . ?
C13 C8 C9 119.2(5) . . ?
C9 C8 N2 120.4(5) . . ?
C4 C3 C2 119.5(5) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C8 C9 C14 124.2(6) . . ?
C10 C9 C8 119.4(6) . . ?
C10 C9 C14 116.4(6) . . ?
N2 C6 C5 111.8(4) . . ?
N2 C6 H6 107.4 . . ?
N2 C6 C7 113.8(5) . . ?
C5 C6 H6 107.4 . . ?
C5 C6 C7 108.7(5) . . ?
C7 C6 H6 107.4 . . ?
C9 C10 H10 119.4 . . ?
C11 C10 C9 121.3(6) . . ?
C11 C10 H10 119.4 . . ?
C13 C17 H17 108.2 . . ?
C18 C17 C13 109.2(6) . . ?
C18 C17 H17 108.2 . . ?
C19 C17 C13 111.7(5) . . ?
C19 C17 H17 108.2 . . ?
C19 C17 C18 111.2(6) . . ?
C13 C12 H12 119.8 . . ?
C13 C12 C11 120.4(6) . . ?
C11 C12 H12 119.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Nd1 B2 Nd1 101.4(2) 3_666 . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C9 C14 H14 106.9 . . ?
C9 C14 C15 112.6(7) . . ?
C9 C14 C16 113.9(7) . . ?
C15 C14 H14 106.9 . . ?
C16 C14 H14 106.9 . . ?
C16 C14 C15 109.3(7) . . ?
C10 C11 C12 119.8(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
Nd1 B1 H1A 57(4) . . ?
Nd1 B1 H1B 60(5) . . ?
Nd1 B1 H1C 68(5) . . ?
Nd1 B1 H1D 175(4) . . ?
H1A B1 H1B 96(6) . . ?
H1A B1 H1C 105(6) . . ?
H1A B1 H1D 121(6) . . ?
H1B B1 H1C 96(6) . . ?
H1B B1 H1D 117(6) . . ?
H1C B1 H1D 117(6) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C23A O1A Nd1 126.7(16) . . ?
C23A O1A C20A 110.4(16) . . ?
C20A O1A Nd1 122.5(17) . . ?
O1A C23A H23A 111.7 . . ?
O1A C23A H23B 111.7 . . ?
O1A C23A C22A 100.4(15) . . ?
H23A C23A H23B 109.5 . . ?
C22A C23A H23A 111.7 . . ?
C22A C23A H23B 111.7 . . ?
C23A C22A H22A 112.3 . . ?
C23A C22A H22B 112.3 . . ?
C23A C22A C21A 97.5(15) . . ?
H22A C22A H22B 109.9 . . ?
C21A C22A H22A 112.3 . . ?
C21A C22A H22B 112.3 . . ?
C22A C21A H21A 112.6 . . ?
C22A C21A H21B 112.6 . . ?
H21A C21A H21B 110.1 . . ?
C20A C21A C22A 95.9(15) . . ?
C20A C21A H21A 112.6 . . ?
C20A C21A H21B 112.6 . . ?
O1A C20A C21A 102.4(16) . . ?
O1A C20A H20A 111.3 . . ?
O1A C20A H20B 111.3 . . ?
C21A C20A H20A 111.3 . . ?
C21A C20A H20B 111.3 . . ?
H20A C20A H20B 109.2 . . ?
C20B O1B Nd1 123.2(18) . . ?
C23B O1B Nd1 123.2(16) . . ?
C23B O1B C20B 111.7(17) . . ?
O1B C20B H20C 111.5 . . ?
O1B C20B H20D 111.5 . . ?
O1B C20B C21B 101.6(15) . . ?
H20C C20B H20D 109.3 . . ?
C21B C20B H20C 111.5 . . ?
C21B C20B H20D 111.5 . . ?
C20B C21B H21C 113.1 . . ?
C20B C21B H21D 113.1 . . ?
C20B C21B C22B 93.2(14) . . ?
H21C C21B H21D 110.5 . . ?
C22B C21B H21C 113.1 . . ?
C22B C21B H21D 113.1 . . ?
C21B C22B H22C 111.9 . . ?
C21B C22B H22D 111.9 . . ?
H22C C22B H22D 109.6 . . ?
C23B C22B C21B 99.5(15) . . ?
C23B C22B H22C 111.9 . . ?
C23B C22B H22D 111.9 . . ?
O1B C23B C22B 98.9(16) . . ?
O1B C23B H23C 112.0 . . ?
O1B C23B H23D 112.0 . . ?
C22B C23B H23C 112.0 . . ?
C22B C23B H23D 112.0 . . ?
H23C C23B H23D 109.7 . . ?

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
Nd1 N1 C5 C4 171.9(4) . . . . ?
Nd1 N1 C5 C6 -8.4(6) . . . . ?
Nd1 N1 C1 C2 -171.8(4) . . . . ?
Nd1 N2 C8 C13 97.3(6) . . . . ?
Nd1 N2 C8 C9 -86.4(6) . . . . ?
Nd1 N2 C6 C5 4.6(7) . . . . ?
Nd1 N2 C6 C7 128.3(5) . . . . ?
Nd1 O1A C23A C22A -170(3) . . . . ?
Nd1 O1A C20A C21A -154(3) . . . . ?
Nd1 O1B C20B C21B 171(3) . . . . ?
Nd1 O1B C23B C22B 152(3) . . . . ?
N1 C5 C6 N2 3.3(7) . . . . ?
N1 C5 C6 C7 -123.2(6) . . . . ?
N2 C8 C9 C10 -178.6(6) . . . . ?
N2 C8 C9 C14 4.7(10) . . . . ?
C4 C5 C6 N2 -177.0(5) . . . . ?
C4 C5 C6 C7 56.5(7) . . . . ?
C5 N1 C1 C2 0.7(8) . . . . ?
C5 C4 C3 C2 0.5(8) . . . . ?
C13 C8 C9 C10 -2.3(10) . . . . ?
C13 C8 C9 C14 -179.0(7) . . . . ?
C13 C12 C11 C10 -0.6(12) . . . . ?
C1 N1 C5 C4 -1.2(7) . . . . ?
C1 N1 C5 C6 178.5(5) . . . . ?
C1 C2 C3 C4 -1.0(8) . . . . ?
C8 N2 C6 C5 176.6(4) . . . . ?
C8 N2 C6 C7 -59.7(7) . . . . ?
C8 C13 C17 C18 -116.7(7) . . . . ?
C8 C13 C17 C19 119.9(7) . . . . ?
C8 C13 C12 C11 -0.7(11) . . . . ?
C8 C9 C10 C11 1.0(11) . . . . ?
C8 C9 C14 C15 114.2(8) . . . . ?
C8 C9 C14 C16 -120.7(8) . . . . ?
C3 C4 C5 N1 0.7(8) . . . . ?
C3 C4 C5 C6 -179.0(5) . . . . ?
C3 C2 C1 N1 0.4(9) . . . . ?
C9 C10 C11 C12 0.4(12) . . . . ?
C6 N2 C8 C13 -75.2(7) . . . . ?
C6 N2 C8 C9 101.0(6) . . . . ?
C10 C9 C14 C15 -62.7(9) . . . . ?
C10 C9 C14 C16 62.5(10) . . . . ?
C17 C13 C8 N2 -3.8(9) . . . . ?
C17 C13 C8 C9 179.9(6) . . . . ?
C17 C13 C12 C11 -178.6(7) . . . . ?
C12 C13 C8 N2 178.4(6) . . . . ?
C12 C13 C8 C9 2.1(10) . . . . ?
C12 C13 C17 C18 61.2(8) . . . . ?
C12 C13 C17 C19 -62.3(9) . . . . ?
C14 C9 C10 C11 178.0(8) . . . . ?
O1A C23A C22A C21A -45(3) . . . . ?
C23A O1A C20A C21A 18(4) . . . . ?
C23A C22A C21A C20A 56(3) . . . . ?
C22A C21A C20A O1A -45(3) . . . . ?
C20A O1A C23A C22A 18(4) . . . . ?
O1B C20B C21B C22B 48(3) . . . . ?
C20B O1B C23B C22B -13(4) . . . . ?
C20B C21B C22B C23B -57(3) . . . . ?
C21B C22B C23B O1B 43(3) . . . . ?
C23B O1B C20B C21B -24(4) . . . . ?

_platon_squeeze_details          ?
_platon_squeeze_special_details  ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.027 0.000 0.500 300 34 ' '
2 0.016 0.500 1.000 300 34 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene/ pentane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_mbx24b_0m
_database_code_depnum_ccdc_archive 'CCDC 2371043'
loop_
_audit_author_name
_audit_author_address
'Frederic Capet'
;CNRS, UCCS
France
;
_audit_update_record             
;
2024-07-15 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_audit_creation_date             2022-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        (PyA3)2Nd(BH4)2
_chemical_formula_moiety         'C34 H54 B2 N3 Nd'
_chemical_formula_sum            'C34 H54 B2 N3 Nd'
_chemical_formula_weight         670.66
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   13.2907(4)
_cell_length_b                   16.2120(5)
_cell_length_c                   17.2538(5)
_cell_angle_alpha                90
_cell_angle_beta                 110.7420(10)
_cell_angle_gamma                90
_cell_volume                     3476.69(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    100.14
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.71
_shelx_estimated_absorpt_T_max   0.875
_shelx_estimated_absorpt_T_min   0.703
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0852 before and 0.0619 after correction.
The Ratio of minimum to maximum transmission is 0.8660.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            109657
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.270
_diffrn_reflns_theta_min         1.781
_diffrn_ambient_temperature      100.14
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Bruker PHOTON III C14'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker DUO PHOTON III'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7395
_reflns_number_total             8595
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2019.11-0 (Bruker-AXS, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8595
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0338
_refine_ls_restrained_S_all      1.056
_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)+(0.0585P)²+3.9901P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0992
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups, H30A of C30, H33A of C33, H8A of C8, H9A of C9, All H(H,H)
  groups, All C(H,H) groups, All C(H,H,H) groups
 At 1.2 times of:
  H7 of C7, H3 of C3, H27 of C27, H26 of C26, H32 of C32, H4 of C4, H5 of C5,
  H10 of C10
2. Restrained distances
 B1-H1D \\sim B1-H1B \\sim B1-H1C \\sim B2-H2B \\sim B2-H2D \\sim B2-H2C
 with sigma of 0.02
 B1-H1A \\sim B2-H2A
 with sigma of 0.02
 H1D-H1B \\sim H1B-H1C \\sim H1C-H1D \\sim H2D-H2B \\sim H2B-H2C \\sim H2C-H2D
 with sigma of 0.02
 H1A-H1D \\sim H1A-H1B \\sim H1A-H1C \\sim H2A-H2D \\sim H2A-H2B \\sim H2A-H2C
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C32(H32), C29(H29), C7(H7), C10(H10)
3.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C16(H16), C18(H18), C17(H17), C4(H4), C3(H3),
 C5(H5)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C14(H14A,H14B,H14C), C33(H33A,H33B,
 H33C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C30(H30A,H30B,H30C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Nd1 Nd 0.65524(2) 0.70494(2) 0.34426(2) 0.01975(6) Uani 1 1 d . . . . .
N1 N 0.83089(18) 0.72957(14) 0.31187(14) 0.0183(4) Uani 1 1 d . . . . .
N2 N 0.64415(19) 0.79907(13) 0.22586(15) 0.0169(4) Uani 1 1 d . . . . .
N3 N 0.48509(18) 0.72377(14) 0.25567(15) 0.0170(4) Uani 1 1 d . . . . .
C21 C 0.3474(2) 0.80634(18) 0.14349(19) 0.0236(6) Uani 1 1 d . . . . .
H21A H 0.351180 0.770672 0.098734 0.035 Uiso 1 1 calc R U . . .
H21B H 0.329944 0.862750 0.122665 0.035 Uiso 1 1 calc R U . . .
H21C H 0.291534 0.785903 0.163406 0.031(10) Uiso 1 1 calc R . . . .
C15 C 0.7287(2) 0.81840(17) 0.20370(17) 0.0184(5) Uani 1 1 d . . . . .
C20 C 0.4563(2) 0.80584(16) 0.21488(18) 0.0195(5) Uani 1 1 d . . . . .
C22 C 0.4520(3) 0.87204(18) 0.27769(19) 0.0250(6) Uani 1 1 d . . . . .
H22A H 0.389564 0.861994 0.294091 0.037 Uiso 1 1 calc R U . . .
H22B H 0.445657 0.926736 0.252214 0.037 Uiso 1 1 calc R U . . .
H22C H 0.517903 0.869508 0.326722 0.037 Uiso 1 1 calc R U . . .
C25 C 0.2702(2) 0.56904(19) 0.24294(19) 0.0256(6) Uani 1 1 d . . . . .
H25 H 0.223068 0.555252 0.271460 0.026(9) Uiso 1 1 calc R . . . .
C32 C 0.4788(2) 0.62844(17) 0.10811(18) 0.0227(6) Uani 1 1 d . . . . .
H32 H 0.509370 0.684888 0.124210 0.027 Uiso 1 1 calc R U . . .
C26 C 0.2706(3) 0.52112(19) 0.1771(2) 0.0288(6) Uani 1 1 d . . . . .
H26 H 0.224966 0.474274 0.160994 0.035 Uiso 1 1 calc R U . . .
C27 C 0.3380(2) 0.54164(18) 0.13448(19) 0.0250(6) Uani 1 1 d . . . . .
H27 H 0.336992 0.509027 0.088473 0.030 Uiso 1 1 calc R U . . .
C24 C 0.3379(2) 0.63774(17) 0.26864(17) 0.0198(5) Uani 1 1 d . . . . .
C16 C 0.7198(2) 0.87262(18) 0.13982(18) 0.0247(6) Uani 1 1 d . . . . .
H16 H 0.779511 0.883901 0.123427 0.029(9) Uiso 1 1 calc R . . . .
C29 C 0.3324(3) 0.6889(2) 0.3406(2) 0.0260(6) Uani 1 1 d . . . . .
H29 H 0.387457 0.733659 0.351501 0.029(9) Uiso 1 1 calc R . . . .
C18 C 0.5349(2) 0.89151(17) 0.12365(18) 0.0236(6) Uani 1 1 d . . . . .
H18 H 0.467690 0.918314 0.098102 0.028(9) Uiso 1 1 calc R . . . .
C2 C 0.9423(2) 0.60632(19) 0.3508(2) 0.0281(6) Uani 1 1 d . . . . .
C17 C 0.6207(3) 0.91015(19) 0.10027(19) 0.0277(6) Uani 1 1 d . . . . .
H17 H 0.612475 0.948750 0.057021 0.026(9) Uiso 1 1 calc R . . . .
C14 C 0.9284(3) 0.7959(2) 0.2305(3) 0.0369(8) Uani 1 1 d . . . . .
H14A H 0.988457 0.760726 0.262895 0.049(12) Uiso 1 1 calc R . . . .
H14B H 0.948427 0.853994 0.242419 0.074 Uiso 1 1 calc R U . . .
H14C H 0.911334 0.785316 0.171268 0.034(11) Uiso 1 1 calc R . . . .
C7 C 0.8682(3) 0.5619(2) 0.2750(2) 0.0338(7) Uani 1 1 d . . . . .
H7 H 0.797422 0.591142 0.257180 0.041 Uiso 1 1 calc R U . . .
C4 C 1.1008(3) 0.6076(3) 0.4752(2) 0.0452(9) Uani 1 1 d . . . . .
H4 H 1.159777 0.579031 0.513737 0.054 Uiso 1 1 calc R U . . .
C33 C 0.5728(3) 0.5675(2) 0.1285(2) 0.0377(8) Uani 1 1 d . . . . .
H33A H 0.610046 0.565094 0.188705 0.056 Uiso 1 1 calc R U . . .
H33B H 0.623155 0.585750 0.102075 0.033(10) Uiso 1 1 calc R . . . .
H33C H 0.545314 0.512566 0.107859 0.050 Uiso 1 1 calc R U . . .
C6 C 0.9985(2) 0.7336(2) 0.4337(2) 0.0301(7) Uani 1 1 d . . . . .
C31 C 0.3578(3) 0.6385(2) 0.4195(2) 0.0352(8) Uani 1 1 d . . . . .
H31A H 0.304087 0.594782 0.410839 0.036(10) Uiso 1 1 calc R . . . .
H31B H 0.356444 0.674479 0.464781 0.054 Uiso 1 1 calc R U . . .
H31C H 0.429448 0.613849 0.433787 0.054 Uiso 1 1 calc R U . . .
C34 C 0.4172(3) 0.6282(3) 0.0142(2) 0.0386(8) Uani 1 1 d . . . . .
H34A H 0.464309 0.648270 -0.014371 0.032(10) Uiso 1 1 calc R . . . .
H34B H 0.354158 0.664242 0.001200 0.061(14) Uiso 1 1 calc R . . . .
H34C H 0.393742 0.571895 -0.004147 0.091 Uiso 1 1 calc R U . . .
C3 C 1.0313(3) 0.5659(2) 0.4074(3) 0.0415(9) Uani 1 1 d . . . . .
H3 H 1.044090 0.509539 0.399171 0.050 Uiso 1 1 calc R U . . .
C5 C 1.0858(3) 0.6891(3) 0.4876(2) 0.0418(9) Uani 1 1 d . . . . .
H5 H 1.135903 0.716474 0.534019 0.050 Uiso 1 1 calc R U . . .
C30 C 0.2223(3) 0.7298(2) 0.3190(2) 0.0364(8) Uani 1 1 d . . . . .
H30A H 0.206195 0.761682 0.267818 0.055 Uiso 1 1 calc R U . . .
H30B H 0.222905 0.766628 0.364227 0.062(14) Uiso 1 1 calc R . . . .
H30C H 0.167181 0.687249 0.311228 0.092 Uiso 1 1 calc R U . . .
C10 C 0.9860(3) 0.8239(2) 0.4509(2) 0.0348(7) Uani 1 1 d . . . . .
H10 H 0.914970 0.843087 0.411074 0.042 Uiso 1 1 calc R U . . .
C23 C 0.4096(2) 0.65758(16) 0.22692(16) 0.0160(5) Uani 1 1 d . . . . .
C19 C 0.5476(2) 0.83258(15) 0.18554(16) 0.0171(5) Uani 1 1 d . . . . .
C28 C 0.4069(2) 0.60896(17) 0.15766(17) 0.0194(5) Uani 1 1 d . . . . .
C13 C 0.8321(2) 0.77733(18) 0.25305(18) 0.0208(5) Uani 1 1 d . . . . .
C1 C 0.9275(2) 0.68959(19) 0.36557(19) 0.0227(6) Uani 1 1 d . . . . .
C11 C 1.0737(4) 0.8761(3) 0.4372(3) 0.0550(11) Uani 1 1 d . . . . .
H11A H 1.143758 0.861211 0.478269 0.084(19) Uiso 1 1 calc R . . . .
H11B H 1.059373 0.934637 0.443091 0.065(15) Uiso 1 1 calc R . . . .
H11C H 1.074343 0.866050 0.381346 0.063(15) Uiso 1 1 calc R . . . .
C12 C 0.9878(4) 0.8400(3) 0.5383(3) 0.0527(11) Uani 1 1 d . . . . .
H12A H 0.930526 0.808148 0.547740 0.080(19) Uiso 1 1 calc R . . . .
H12B H 0.976479 0.898907 0.544953 0.075(17) Uiso 1 1 calc R . . . .
H12C H 1.057651 0.823257 0.578550 0.113 Uiso 1 1 calc R U . . .
C9 C 0.8469(3) 0.4717(2) 0.2905(3) 0.0429(9) Uani 1 1 d . . . . .
H9A H 0.914217 0.440371 0.305797 0.064 Uiso 1 1 calc R U . . .
H9B H 0.794378 0.448181 0.239991 0.035(10) Uiso 1 1 calc R . . . .
H9C H 0.818394 0.468670 0.335611 0.052 Uiso 1 1 calc R U . . .
C8 C 0.9093(4) 0.5677(3) 0.2044(3) 0.0553(11) Uani 1 1 d . . . . .
H8A H 0.912864 0.625782 0.189775 0.083 Uiso 1 1 calc R U . . .
H8B H 0.860613 0.537892 0.156386 0.061(15) Uiso 1 1 calc R . . . .
H8C H 0.981346 0.543289 0.221149 0.092 Uiso 1 1 calc R U . . .
B2 B 0.6741(3) 0.5568(2) 0.4072(2) 0.0300(7) Uani 1 1 d D . . . .
H2A H 0.679(2) 0.504(2) 0.434(2) 0.052(13) Uiso 1 1 d D . . . .
H2B H 0.611(2) 0.5966(19) 0.417(2) 0.048(12) Uiso 1 1 d D . . . .
H2C H 0.751(2) 0.592(2) 0.431(2) 0.051(12) Uiso 1 1 d D . . . .
B1 B 0.7020(3) 0.8009(3) 0.4724(3) 0.0367(9) Uani 1 1 d D . . . .
H1A H 0.712(3) 0.837(2) 0.518(2) 0.067(15) Uiso 1 1 d D . . . .
H1B H 0.709(3) 0.834(2) 0.4172(17) 0.046(12) Uiso 1 1 d D . . . .
H1C H 0.758(2) 0.7474(17) 0.487(2) 0.041(11) Uiso 1 1 d D . . . .
H1D H 0.618(2) 0.773(2) 0.450(2) 0.055(13) Uiso 1 1 d D . . . .
H2D H 0.652(3) 0.550(3) 0.3390(14) 0.12(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Nd1 N1 2.616(2) . ?
Nd1 N2 2.512(2) . ?
Nd1 N3 2.257(2) . ?
Nd1 H2B 2.36(4) . ?
Nd1 H2C 2.42(4) . ?
Nd1 H1B 2.41(4) . ?
Nd1 H1C 2.45(3) . ?
Nd1 H1D 2.33(4) . ?
Nd1 H2D 2.51(5) . ?
N1 C13 1.281(4) . ?
N1 C1 1.444(4) . ?
N2 C15 1.346(4) . ?
N2 C19 1.339(3) . ?
N3 C20 1.490(3) . ?
N3 C23 1.433(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 C20 1.532(4) . ?
C15 C16 1.382(4) . ?
C15 C13 1.493(4) . ?
C20 C22 1.541(4) . ?
C20 C19 1.534(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C25 H25 0.9500 . ?
C25 C26 1.378(5) . ?
C25 C24 1.402(4) . ?
C32 H32 1.0000 . ?
C32 C33 1.533(4) . ?
C32 C34 1.535(4) . ?
C32 C28 1.523(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.385(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.390(4) . ?
C24 C29 1.517(4) . ?
C24 C23 1.419(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.390(4) . ?
C29 H29 1.0000 . ?
C29 C31 1.519(4) . ?
C29 C30 1.527(4) . ?
C18 H18 0.9500 . ?
C18 C17 1.371(4) . ?
C18 C19 1.398(4) . ?
C2 C7 1.512(5) . ?
C2 C3 1.402(5) . ?
C2 C1 1.400(4) . ?
C17 H17 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 C13 1.494(4) . ?
C7 H7 1.0000 . ?
C7 C9 1.532(5) . ?
C7 C8 1.504(6) . ?
C4 H4 0.9500 . ?
C4 C3 1.382(6) . ?
C4 C5 1.365(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C6 C5 1.403(5) . ?
C6 C10 1.515(5) . ?
C6 C1 1.412(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C3 H3 0.9500 . ?
C5 H5 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.526(6) . ?
C10 C12 1.522(5) . ?
C23 C28 1.422(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
B2 H2A 0.96(4) . ?
B2 H2B 1.12(2) . ?
B2 H2C 1.12(2) . ?
B2 H2D 1.11(2) . ?
B1 H1A 0.95(4) . ?
B1 H1B 1.12(2) . ?
B1 H1C 1.11(2) . ?
B1 H1D 1.14(2) . ?

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 Nd1 H2B 129.7(6) . . ?
N1 Nd1 H2C 86.1(7) . . ?
N1 Nd1 H1B 81.9(7) . . ?
N1 Nd1 H1C 87.1(7) . . ?
N1 Nd1 H1D 123.3(6) . . ?
N1 Nd1 H2D 98.5(8) . . ?
N2 Nd1 N1 62.19(7) . . ?
N2 Nd1 H2B 159.2(8) . . ?
N2 Nd1 H2C 145.8(8) . . ?
N2 Nd1 H1B 79.7(5) . . ?
N2 Nd1 H1C 119.8(7) . . ?
N2 Nd1 H1D 112.5(8) . . ?
N2 Nd1 H2D 125.6(5) . . ?
N3 Nd1 N1 126.19(8) . . ?
N3 Nd1 N2 67.11(8) . . ?
N3 Nd1 H2B 94.8(7) . . ?
N3 Nd1 H2C 134.6(5) . . ?
N3 Nd1 H1B 106.0(7) . . ?
N3 Nd1 H1C 135.3(6) . . ?
N3 Nd1 H1D 91.6(7) . . ?
N3 Nd1 H2D 96.4(8) . . ?
H2B Nd1 H2C 44.2(9) . . ?
H2B Nd1 H1B 116.6(8) . . ?
H2B Nd1 H1C 80.1(11) . . ?
H2B Nd1 H1D 76.6(11) . . ?
H2B Nd1 H2D 43.2(9) . . ?
H2C Nd1 H1B 109.9(8) . . ?
H2C Nd1 H1C 67.0(10) . . ?
H2C Nd1 H1D 94.9(12) . . ?
H2C Nd1 H2D 42.6(8) . . ?
H1B Nd1 H1C 43.7(8) . . ?
H1B Nd1 H1D 44.5(9) . . ?
H1B Nd1 H2D 151.9(10) . . ?
H1C Nd1 H1D 43.8(9) . . ?
H1C Nd1 H2D 108.2(6) . . ?
H1D Nd1 H2D 119.7(9) . . ?
C13 N1 Nd1 121.61(19) . . ?
C13 N1 C1 121.4(2) . . ?
C1 N1 Nd1 116.91(17) . . ?
C15 N2 Nd1 123.91(18) . . ?
C19 N2 Nd1 116.01(18) . . ?
C19 N2 C15 120.1(2) . . ?
C20 N3 Nd1 117.96(17) . . ?
C23 N3 Nd1 122.98(16) . . ?
C23 N3 C20 118.3(2) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
N2 C15 C16 122.0(3) . . ?
N2 C15 C13 115.3(2) . . ?
C16 C15 C13 122.7(3) . . ?
N3 C20 C21 113.3(2) . . ?
N3 C20 C22 110.9(2) . . ?
N3 C20 C19 107.9(2) . . ?
C21 C20 C22 107.6(2) . . ?
C21 C20 C19 111.4(2) . . ?
C19 C20 C22 105.4(2) . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C26 C25 H25 119.4 . . ?
C26 C25 C24 121.3(3) . . ?
C24 C25 H25 119.4 . . ?
C33 C32 H32 107.9 . . ?
C33 C32 C34 109.1(3) . . ?
C34 C32 H32 107.9 . . ?
C28 C32 H32 107.9 . . ?
C28 C32 C33 111.1(2) . . ?
C28 C32 C34 112.7(3) . . ?
C25 C26 H26 120.2 . . ?
C25 C26 C27 119.6(3) . . ?
C27 C26 H26 120.2 . . ?
C26 C27 H27 119.3 . . ?
C26 C27 C28 121.3(3) . . ?
C28 C27 H27 119.3 . . ?
C25 C24 C29 118.8(3) . . ?
C25 C24 C23 119.4(3) . . ?
C23 C24 C29 121.8(3) . . ?
C15 C16 H16 121.0 . . ?
C15 C16 C17 118.0(3) . . ?
C17 C16 H16 121.0 . . ?
C24 C29 H29 107.8 . . ?
C24 C29 C31 112.3(3) . . ?
C24 C29 C30 111.0(3) . . ?
C31 C29 H29 107.8 . . ?
C31 C29 C30 110.0(3) . . ?
C30 C29 H29 107.8 . . ?
C17 C18 H18 120.4 . . ?
C17 C18 C19 119.2(3) . . ?
C19 C18 H18 120.4 . . ?
C3 C2 C7 120.7(3) . . ?
C1 C2 C7 121.7(3) . . ?
C1 C2 C3 117.5(3) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 120.0 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
C2 C7 H7 107.1 . . ?
C2 C7 C9 114.1(3) . . ?
C9 C7 H7 107.1 . . ?
C8 C7 C2 111.1(3) . . ?
C8 C7 H7 107.1 . . ?
C8 C7 C9 110.1(3) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C5 C4 C3 121.0(3) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C5 C6 C10 119.3(3) . . ?
C5 C6 C1 116.4(3) . . ?
C1 C6 C10 124.4(3) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.8 . . ?
C4 C5 C6 121.7(4) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C6 C10 H10 107.9 . . ?
C6 C10 C11 111.3(3) . . ?
C6 C10 C12 113.3(3) . . ?
C11 C10 H10 107.9 . . ?
C12 C10 H10 107.9 . . ?
C12 C10 C11 108.3(3) . . ?
C24 C23 N3 120.5(2) . . ?
C24 C23 C28 118.7(2) . . ?
C28 C23 N3 120.8(2) . . ?
N2 C19 C20 116.0(2) . . ?
N2 C19 C18 120.6(3) . . ?
C18 C19 C20 123.3(2) . . ?
C27 C28 C32 118.8(3) . . ?
C27 C28 C23 119.6(3) . . ?
C23 C28 C32 121.5(2) . . ?
N1 C13 C15 117.0(3) . . ?
N1 C13 C14 125.5(3) . . ?
C15 C13 C14 117.5(3) . . ?
C2 C1 N1 117.8(3) . . ?
C2 C1 C6 122.9(3) . . ?
C6 C1 N1 119.1(3) . . ?
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 . . ?
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 . . ?
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 . . ?
H2A B2 H2B 111.1(18) . . ?
H2A B2 H2C 112.6(18) . . ?
H2A B2 H2D 112.0(19) . . ?
H2B B2 H2C 107.0(17) . . ?
H2B B2 H2D 106.9(18) . . ?
H2C B2 H2D 107.0(18) . . ?
H1A B1 H1B 112.5(18) . . ?
H1A B1 H1C 113.9(18) . . ?
H1A B1 H1D 111.3(18) . . ?
H1B B1 H1C 108.1(17) . . ?
H1B B1 H1D 105.4(17) . . ?
H1C B1 H1D 105.2(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
Nd1 N1 C13 C15 0.0(3) . . . . ?
Nd1 N1 C13 C14 179.3(3) . . . . ?
Nd1 N1 C1 C2 80.8(3) . . . . ?
Nd1 N1 C1 C6 -94.6(3) . . . . ?
Nd1 N2 C15 C16 -177.8(2) . . . . ?
Nd1 N2 C15 C13 2.0(3) . . . . ?
Nd1 N2 C19 C20 -2.6(3) . . . . ?
Nd1 N2 C19 C18 174.2(2) . . . . ?
Nd1 N3 C20 C21 168.08(19) . . . . ?
Nd1 N3 C20 C22 -70.8(3) . . . . ?
Nd1 N3 C20 C19 44.2(3) . . . . ?
Nd1 N3 C23 C24 93.2(3) . . . . ?
Nd1 N3 C23 C28 -84.9(3) . . . . ?
N2 C15 C16 C17 2.6(4) . . . . ?
N2 C15 C13 N1 -1.3(4) . . . . ?
N2 C15 C13 C14 179.4(3) . . . . ?
N3 C20 C19 N2 -24.1(3) . . . . ?
N3 C20 C19 C18 159.3(2) . . . . ?
N3 C23 C28 C32 -3.9(4) . . . . ?
N3 C23 C28 C27 175.6(2) . . . . ?
C21 C20 C19 N2 -149.1(2) . . . . ?
C21 C20 C19 C18 34.3(4) . . . . ?
C15 N2 C19 C20 179.3(2) . . . . ?
C15 N2 C19 C18 -3.9(4) . . . . ?
C15 C16 C17 C18 -1.5(4) . . . . ?
C20 N3 C23 C24 -97.2(3) . . . . ?
C20 N3 C23 C28 84.7(3) . . . . ?
C22 C20 C19 N2 94.5(3) . . . . ?
C22 C20 C19 C18 -82.2(3) . . . . ?
C25 C26 C27 C28 1.2(5) . . . . ?
C25 C24 C29 C31 59.5(4) . . . . ?
C25 C24 C29 C30 -64.1(4) . . . . ?
C25 C24 C23 N3 -175.4(2) . . . . ?
C25 C24 C23 C28 2.7(4) . . . . ?
C26 C25 C24 C29 179.0(3) . . . . ?
C26 C25 C24 C23 -1.0(4) . . . . ?
C26 C27 C28 C32 -179.8(3) . . . . ?
C26 C27 C28 C23 0.6(4) . . . . ?
C24 C25 C26 C27 -1.0(5) . . . . ?
C24 C23 C28 C32 177.9(2) . . . . ?
C24 C23 C28 C27 -2.5(4) . . . . ?
C16 C15 C13 N1 178.6(3) . . . . ?
C16 C15 C13 C14 -0.7(4) . . . . ?
C29 C24 C23 N3 4.6(4) . . . . ?
C29 C24 C23 C28 -177.2(3) . . . . ?
C17 C18 C19 N2 4.9(4) . . . . ?
C17 C18 C19 C20 -178.6(3) . . . . ?
C7 C2 C3 C4 177.9(3) . . . . ?
C7 C2 C1 N1 8.1(4) . . . . ?
C7 C2 C1 C6 -176.8(3) . . . . ?
C33 C32 C28 C27 -74.9(4) . . . . ?
C33 C32 C28 C23 104.6(3) . . . . ?
C34 C32 C28 C27 47.8(4) . . . . ?
C34 C32 C28 C23 -132.6(3) . . . . ?
C3 C2 C7 C9 38.7(4) . . . . ?
C3 C2 C7 C8 -86.5(4) . . . . ?
C3 C2 C1 N1 -174.5(3) . . . . ?
C3 C2 C1 C6 0.6(5) . . . . ?
C3 C4 C5 C6 1.6(6) . . . . ?
C5 C4 C3 C2 -1.5(6) . . . . ?
C5 C6 C10 C11 69.3(5) . . . . ?
C5 C6 C10 C12 -53.0(4) . . . . ?
C5 C6 C1 N1 174.5(3) . . . . ?
C5 C6 C1 C2 -0.6(5) . . . . ?
C10 C6 C5 C4 179.8(4) . . . . ?
C10 C6 C1 N1 -5.8(5) . . . . ?
C10 C6 C1 C2 179.1(3) . . . . ?
C23 N3 C20 C21 -2.0(3) . . . . ?
C23 N3 C20 C22 119.1(3) . . . . ?
C23 N3 C20 C19 -125.9(2) . . . . ?
C23 C24 C29 C31 -120.6(3) . . . . ?
C23 C24 C29 C30 115.9(3) . . . . ?
C19 N2 C15 C16 0.1(4) . . . . ?
C19 N2 C15 C13 180.0(2) . . . . ?
C19 C18 C17 C16 -2.1(5) . . . . ?
C13 N1 C1 C2 -101.8(3) . . . . ?
C13 N1 C1 C6 82.9(4) . . . . ?
C13 C15 C16 C17 -177.3(3) . . . . ?
C1 N1 C13 C15 -177.3(2) . . . . ?
C1 N1 C13 C14 2.0(5) . . . . ?
C1 C2 C7 C9 -144.0(3) . . . . ?
C1 C2 C7 C8 90.9(4) . . . . ?
C1 C2 C3 C4 0.4(5) . . . . ?
C1 C6 C5 C4 -0.5(6) . . . . ?
C1 C6 C10 C11 -110.4(4) . . . . ?
C1 C6 C10 C12 127.3(4) . . . . ?

