# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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data_publication_text

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            '[GaH3(7Dipp)]'
_chemical_formula_moiety         'C29 H45 Ga N2'
_chemical_formula_sum            'C29 H45 Ga N2'
_chemical_compound_source        toluene
_chemical_melting_point          '425 (dec.)'

_exptl_crystal_description       octahedron
_exptl_crystal_colour            colourless

_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         491.39

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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+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                   17.0085(7)
_cell_length_b                   9.0804(5)
_cell_length_c                   17.7985(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.882(2)
_cell_angle_gamma                90
_cell_volume                     2745.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.020
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Bruker Quazar Multilayer Optics'
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15454
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.543
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2682
_reflns_number_gt                2474
_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 Apex II software'
_computing_cell_refinement       'Bruker Apex II software'
_computing_data_reduction        X-Seed
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2010'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0418P)²+4.7746P] 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         2682
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0929
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Ga1 Ga 0.5000 0.94900(4) 0.2500 0.02331(14) Uani 1 2 d S T P . .
N1 N 0.52543(10) 0.64113(19) 0.19107(9) 0.0185(4) Uani 1 1 d . . . . .
C1 C 0.5000 0.7165(3) 0.2500 0.0131(5) Uani 1 2 d S T P . .
C4 C 0.53959(11) 0.7174(2) 0.12131(10) 0.0168(4) Uani 1 1 d . . . . .
C5 C 0.61582(12) 0.7684(2) 0.10913(11) 0.0208(4) Uani 1 1 d . . . . .
C6 C 0.62811(13) 0.8335(3) 0.03967(12) 0.0254(5) Uani 1 1 d . . . . .
H6 H 0.6791 0.8687 0.0296 0.030 Uiso 1 1 calc R U . . .
C7 C 0.56785(14) 0.8479(3) -0.01470(12) 0.0266(5) Uani 1 1 d . . . . .
H7 H 0.5776 0.8932 -0.0614 0.032 Uiso 1 1 calc R U . . .
C8 C 0.49348(13) 0.7966(2) -0.00124(11) 0.0226(4) Uani 1 1 d . . . . .
H8 H 0.4523 0.8070 -0.0389 0.027 Uiso 1 1 calc R U . . .
C9 C 0.47790(12) 0.7294(2) 0.06704(11) 0.0179(4) Uani 1 1 d . . . . .
C10 C 0.68372(13) 0.7556(3) 0.16698(13) 0.0345(6) Uani 1 1 d . . . . .
C13 C 0.39554(12) 0.6715(3) 0.07913(12) 0.0234(5) Uani 1 1 d . . . . .
C14 C 0.33619(14) 0.7964(3) 0.08495(18) 0.0462(7) Uani 1 1 d . . . . .
H14A H 0.3538 0.8634 0.1255 0.069 Uiso 1 1 calc R U . . .
H14B H 0.2846 0.7555 0.0958 0.069 Uiso 1 1 calc R U . . .
H14C H 0.3320 0.8505 0.0373 0.069 Uiso 1 1 calc R U . . .
C15 C 0.36873(15) 0.5639(3) 0.01764(15) 0.0350(6) Uani 1 1 d . . . . .
H15A H 0.3643 0.6154 -0.0308 0.052 Uiso 1 1 calc R U . . .
H15B H 0.3174 0.5230 0.0290 0.052 Uiso 1 1 calc R U . . .
H15C H 0.4072 0.4840 0.0150 0.052 Uiso 1 1 calc R U . . .
H1A H 0.511(3) 1.009(6) 0.171(3) 0.038(14) Uiso 0.5 1 d . . P . .
H1B H 0.418(3) 0.990(6) 0.278(3) 0.036(14) Uiso 0.5 1 d . . P . .
H1C H 0.563(4) 1.019(8) 0.311(4) 0.07(2) Uiso 0.5 1 d . . P . .
H10 H 0.6659(13) 0.728(3) 0.2109(14) 0.024(6) Uiso 1 1 d . . . . .
H13 H 0.3951(13) 0.618(3) 0.1247(14) 0.021(6) Uiso 1 1 d . . . . .
C2A C 0.5285(4) 0.4747(6) 0.1791(3) 0.0220(11) Uani 0.5 1 d . . P . .
H2A1 H 0.4752 0.4381 0.1642 0.026 Uiso 0.5 1 calc R U P . .
H2A2 H 0.5636 0.4524 0.1379 0.026 Uiso 0.5 1 calc R U P . .
C3A C 0.5583(3) 0.3972(5) 0.2495(3) 0.0276(10) Uani 0.5 1 d . . P . .
H3A1 H 0.6010 0.4564 0.2743 0.033 Uiso 0.5 1 calc R U P . .
H3A2 H 0.5808 0.3009 0.2357 0.033 Uiso 0.5 1 calc R U P . .
C11A C 0.7142(8) 0.9233(17) 0.1881(8) 0.055(3) Uani 0.54(3) 1 d . . P A 1
H11D H 0.7568 0.9184 0.2271 0.082 Uiso 0.54(3) 1 calc R U P A 1
H11E H 0.6704 0.9807 0.2066 0.082 Uiso 0.54(3) 1 calc R U P A 1
H11F H 0.7335 0.9705 0.1430 0.082 Uiso 0.54(3) 1 calc R U P A 1
C12A C 0.7545(6) 0.6729(18) 0.1416(5) 0.047(2) Uani 0.54(3) 1 d . . P A 1
H12D H 0.7739 0.7202 0.0966 0.070 Uiso 0.54(3) 1 calc R U P A 1
H12E H 0.7396 0.5709 0.1298 0.070 Uiso 0.54(3) 1 calc R U P A 1
H12F H 0.7960 0.6737 0.1818 0.070 Uiso 0.54(3) 1 calc R U P A 1
C2B C 0.5662(3) 0.4942(6) 0.2007(3) 0.0217(10) Uani 0.5 1 d . . P . .
H2B1 H 0.5950 0.4901 0.2504 0.026 Uiso 0.5 1 calc R U P . .
H2B2 H 0.6048 0.4816 0.1613 0.026 Uiso 0.5 1 calc R U P . .
C3B C 0.5059(3) 0.3719(6) 0.1949(3) 0.0293(10) Uani 0.5 1 d . . P . .
H3B1 H 0.5320 0.2763 0.2057 0.035 Uiso 0.5 1 calc R U P . .
H3B2 H 0.4820 0.3683 0.1431 0.035 Uiso 0.5 1 calc R U P . .
C11B C 0.7337(8) 0.8790(18) 0.1761(8) 0.044(3) Uani 0.46(3) 1 d . . P A 2
H11A H 0.7676 0.8856 0.1333 0.066 Uiso 0.46(3) 1 calc R U P A 2
H11B H 0.7664 0.8687 0.2227 0.066 Uiso 0.46(3) 1 calc R U P A 2
H11C H 0.7018 0.9687 0.1785 0.066 Uiso 0.46(3) 1 calc R U P A 2
C12B C 0.7313(8) 0.6102(19) 0.1450(5) 0.040(3) Uani 0.46(3) 1 d . . P A 2
H12A H 0.7486 0.6197 0.0935 0.060 Uiso 0.46(3) 1 calc R U P A 2
H12B H 0.6970 0.5240 0.1483 0.060 Uiso 0.46(3) 1 calc R U P A 2
H12C H 0.7773 0.5983 0.1798 0.060 Uiso 0.46(3) 1 calc R U P A 2


_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
Ga1 C1 2.111(3) . ?
Ga1 H1A 1.52(5) . ?
Ga1 H1B 1.55(5) . ?
Ga1 H1C 1.62(7) . ?
N1 C1 1.342(2) . ?
N1 C4 1.452(2) . ?
N1 C2B 1.510(5) . ?
N1 C2A 1.527(5) . ?
C1 N1 1.342(2) 2_655 ?
C4 C9 1.394(3) . ?
C4 C5 1.404(3) . ?
C5 C6 1.396(3) . ?
C5 C10 1.513(3) . ?
C6 C7 1.380(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.380(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.397(3) . ?
C8 H8 0.9500 . ?
C9 C13 1.522(3) . ?
C10 C11B 1.412(14) . ?
C10 C12A 1.507(8) . ?
C10 C12B 1.606(11) . ?
C10 C11A 1.646(14) . ?
C10 H10 0.89(2) . ?
C13 C15 1.520(3) . ?
C13 C14 1.526(3) . ?
C13 H13 0.94(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C2A C3A 1.502(7) . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C3A C3B 1.528(6) 2_655 ?
C3A H3A1 0.9900 . ?
C3A H3A2 0.9900 . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C2B C3B 1.512(7) . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C3B C3A 1.528(6) 2_655 ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C11B H11A 0.9800 . ?
C11B H11B 0.9800 . ?
C11B H11C 0.9800 . ?
C12B H12A 0.9800 . ?
C12B H12B 0.9800 . ?
C12B 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 Ga1 H1A 111(2) . . ?
C1 Ga1 H1B 104(2) . . ?
H1A Ga1 H1B 112(3) . . ?
C1 Ga1 H1C 113(3) . . ?
H1A Ga1 H1C 111(3) . . ?
H1B Ga1 H1C 105(3) . . ?
C1 N1 C4 119.92(18) . . ?
C1 N1 C2B 121.7(2) . . ?
C4 N1 C2B 115.1(2) . . ?
C1 N1 C2A 128.9(2) . . ?
C4 N1 C2A 110.2(2) . . ?
C2B N1 C2A 28.7(2) . . ?
N1 C1 N1 118.7(3) 2_655 . ?
N1 C1 Ga1 120.66(13) 2_655 . ?
N1 C1 Ga1 120.65(13) . . ?
C9 C4 C5 122.40(18) . . ?
C9 C4 N1 118.58(17) . . ?
C5 C4 N1 118.91(17) . . ?
C6 C5 C4 117.21(19) . . ?
C6 C5 C10 119.51(19) . . ?
C4 C5 C10 123.28(19) . . ?
C7 C6 C5 121.5(2) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C8 120.07(19) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 120.9(2) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C8 117.89(18) . . ?
C4 C9 C13 122.76(18) . . ?
C8 C9 C13 119.35(18) . . ?
C11B C10 C5 116.8(6) . . ?
C12A C10 C5 115.3(4) . . ?
C11B C10 C12B 111.9(5) . . ?
C5 C10 C12B 105.9(4) . . ?
C12A C10 C11A 106.4(5) . . ?
C5 C10 C11A 107.7(5) . . ?
C11B C10 H10 110.8(17) . . ?
C12A C10 H10 115.7(16) . . ?
C5 C10 H10 109.8(15) . . ?
C12B C10 H10 100.2(17) . . ?
C11A C10 H10 100.4(17) . . ?
C15 C13 C9 111.43(17) . . ?
C15 C13 C14 110.6(2) . . ?
C9 C13 C14 111.68(19) . . ?
C15 C13 H13 105.9(15) . . ?
C9 C13 H13 110.2(14) . . ?
C14 C13 H13 106.8(14) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C3A C2A N1 111.1(4) . . ?
C3A C2A H2A1 109.4 . . ?
N1 C2A H2A1 109.4 . . ?
C3A C2A H2A2 109.4 . . ?
N1 C2A H2A2 109.4 . . ?
H2A1 C2A H2A2 108.0 . . ?
C2A C3A C3B 112.9(4) . 2_655 ?
C2A C3A H3A1 109.0 . . ?
C3B C3A H3A1 109.0 2_655 . ?
C2A C3A H3A2 109.0 . . ?
C3B C3A H3A2 109.0 2_655 . ?
H3A1 C3A H3A2 107.8 . . ?
C10 C11A H11D 109.5 . . ?
C10 C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
C10 C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C10 C12A H12D 109.5 . . ?
C10 C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C10 C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
N1 C2B C3B 109.5(4) . . ?
N1 C2B H2B1 109.8 . . ?
C3B C2B H2B1 109.8 . . ?
N1 C2B H2B2 109.8 . . ?
C3B C2B H2B2 109.8 . . ?
H2B1 C2B H2B2 108.2 . . ?
C2B C3B C3A 110.5(4) . 2_655 ?
C2B C3B H3B1 109.6 . . ?
C3A C3B H3B1 109.6 2_655 . ?
C2B C3B H3B2 109.6 . . ?
C3A C3B H3B2 109.6 2_655 . ?
H3B1 C3B H3B2 108.1 . . ?
C10 C11B H11A 109.5 . . ?
C10 C11B H11B 109.5 . . ?
H11A C11B H11B 109.5 . . ?
C10 C11B H11C 109.5 . . ?
H11A C11B H11C 109.5 . . ?
H11B C11B H11C 109.5 . . ?
C10 C12B H12A 109.5 . . ?
C10 C12B H12B 109.5 . . ?
H12A C12B H12B 109.5 . . ?
C10 C12B H12C 109.5 . . ?
H12A C12B H12C 109.5 . . ?
H12B C12B H12C 109.5 . . ?

_refine_diff_density_max         0.352
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.067

_shelxl_version_number           2014-3

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'C 2/c'
_symmetry_int_tables_number      15
_chemical_absolute_configuration ?

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_database_code_depnum_ccdc_archive 'CCDC 1024178'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#
data_C:\Users\Marcus\Desktop\JACSCO~1\GRP13_~1\Other\AIM026~1.THF\work\Pbca

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        ?
_chemical_name_common            '[InBr3(7Dipp)].THF'
_chemical_formula_moiety         'C29 H42 Br3 In N2 .C4 H8 O'
_chemical_formula_sum            'C33 H50 Br3 In N2 O'
_chemical_compound_source        THF
_chemical_melting_point          '503 (dec. 573)'

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless

_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         845.30

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.8412(7)
_cell_length_b                   18.6259(7)
_cell_length_c                   23.2271(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6853.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_F_000             3392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    4.215
_shelx_estimated_absorpt_T_min   0.590
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Bruker Quazar Multilayer Optics'
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            110495
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.902
_diffrn_reflns_theta_max         30.518
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10034
_reflns_number_gt                7116
_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 Apex II software'
_computing_cell_refinement       'Bruker Apex II software'
_computing_data_reduction        X-Seed
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2010'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0120P)²+4.9054P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10034
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0526
_refine_ls_wR_factor_gt          0.0463
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
In1 In 0.23950(2) 0.48993(2) 0.07570(2) 0.01467(4) Uani 1 1 d . . . . .
Br1 Br 0.26372(2) 0.54758(2) -0.02034(2) 0.02669(6) Uani 1 1 d . . . . .
Br2 Br 0.13125(2) 0.57425(2) 0.11711(2) 0.02425(6) Uani 1 1 d . . . . .
Br3 Br 0.36892(2) 0.51488(2) 0.13560(2) 0.02446(6) Uani 1 1 d . . . . .
N1 N 0.26500(10) 0.32445(8) 0.05494(7) 0.0120(3) Uani 1 1 d . . . . .
N2 N 0.18154(10) 0.34837(8) 0.13519(7) 0.0124(4) Uani 1 1 d . . . . .
C1 C 0.22293(12) 0.37042(10) 0.08829(9) 0.0114(4) Uani 1 1 d . . . . .
C2 C 0.25758(13) 0.24381(10) 0.05414(10) 0.0188(5) Uani 1 1 d . . . . .
H2A H 0.2986 0.2238 0.0820 0.023 Uiso 1 1 calc R U . . .
H2B H 0.2737 0.2264 0.0154 0.023 Uiso 1 1 calc R U . . .
C3 C 0.17074(14) 0.21460(11) 0.06848(11) 0.0230(5) Uani 1 1 d . . . . .
H3A H 0.1666 0.1645 0.0546 0.028 Uiso 1 1 calc R U . . .
H3B H 0.1276 0.2432 0.0479 0.028 Uiso 1 1 calc R U . . .
C4 C 0.15197(16) 0.21637(12) 0.13268(11) 0.0284(6) Uani 1 1 d . . . . .
H4A H 0.0904 0.2215 0.1385 0.034 Uiso 1 1 calc R U . . .
H4B H 0.1697 0.1703 0.1502 0.034 Uiso 1 1 calc R U . . .
C5 C 0.19685(15) 0.27730(11) 0.16251(10) 0.0217(5) Uani 1 1 d . . . . .
H5A H 0.1780 0.2793 0.2031 0.026 Uiso 1 1 calc R U . . .
H5B H 0.2583 0.2675 0.1625 0.026 Uiso 1 1 calc R U . . .
C6 C 0.32044(12) 0.35228(10) 0.00977(9) 0.0127(4) Uani 1 1 d . . . . .
C7 C 0.40634(13) 0.36447(10) 0.02269(9) 0.0155(4) Uani 1 1 d . . . . .
C8 C 0.45648(13) 0.39259(11) -0.02145(10) 0.0212(5) Uani 1 1 d . . . . .
H8 H 0.5140 0.4037 -0.0139 0.025 Uiso 1 1 calc R U . . .
C9 C 0.42414(14) 0.40453(12) -0.07574(11) 0.0238(5) Uani 1 1 d . . . . .
H9 H 0.4589 0.4250 -0.1047 0.029 Uiso 1 1 calc R U . . .
C10 C 0.34162(14) 0.38681(11) -0.08805(10) 0.0200(5) Uani 1 1 d . . . . .
H10 H 0.3210 0.3930 -0.1261 0.024 Uiso 1 1 calc R U . . .
C11 C 0.28792(13) 0.35999(10) -0.04579(9) 0.0154(4) Uani 1 1 d . . . . .
C12 C 0.44673(13) 0.34095(11) 0.07878(10) 0.0193(5) Uani 1 1 d . . . . .
H12 H 0.4034 0.3443 0.1100 0.023 Uiso 1 1 calc R U . . .
C13 C 0.52342(14) 0.38575(13) 0.09646(11) 0.0285(6) Uani 1 1 d . . . . .
H13A H 0.5707 0.3752 0.0706 0.043 Uiso 1 1 calc R U . . .
H13B H 0.5394 0.3738 0.1361 0.043 Uiso 1 1 calc R U . . .
H13C H 0.5093 0.4369 0.0940 0.043 Uiso 1 1 calc R U . . .
C14 C 0.47509(15) 0.26213(12) 0.07365(11) 0.0271(5) Uani 1 1 d . . . . .
H14A H 0.4269 0.2323 0.0623 0.041 Uiso 1 1 calc R U . . .
H14B H 0.4968 0.2456 0.1109 0.041 Uiso 1 1 calc R U . . .
H14C H 0.5196 0.2583 0.0445 0.041 Uiso 1 1 calc R U . . .
C15 C 0.19905(13) 0.33721(11) -0.06282(10) 0.0188(5) Uani 1 1 d . . . . .
H15 H 0.1681 0.3227 -0.0271 0.023 Uiso 1 1 calc R U . . .
C16 C 0.14870(15) 0.39683(13) -0.09236(12) 0.0327(6) Uani 1 1 d . . . . .
H16A H 0.1490 0.4399 -0.0681 0.049 Uiso 1 1 calc R U . . .
H16B H 0.0904 0.3808 -0.0982 0.049 Uiso 1 1 calc R U . . .
H16C H 0.1744 0.4080 -0.1297 0.049 Uiso 1 1 calc R U . . .
C17 C 0.20437(16) 0.27174(14) -0.10268(13) 0.0359(7) Uani 1 1 d . . . . .
H17A H 0.2368 0.2843 -0.1372 0.054 Uiso 1 1 calc R U . . .
H17B H 0.1473 0.2569 -0.1139 0.054 Uiso 1 1 calc R U . . .
H17C H 0.2324 0.2322 -0.0825 0.054 Uiso 1 1 calc R U . . .
C18 C 0.11654(12) 0.39143(10) 0.16340(9) 0.0122(4) Uani 1 1 d . . . . .
C19 C 0.13398(13) 0.42114(10) 0.21785(9) 0.0146(4) Uani 1 1 d . . . . .
C20 C 0.06791(13) 0.45487(11) 0.24643(10) 0.0179(5) Uani 1 1 d . . . . .
H20 H 0.0772 0.4739 0.2839 0.021 Uiso 1 1 calc R U . . .
C21 C -0.01113(13) 0.46142(12) 0.22163(10) 0.0223(5) Uani 1 1 d . . . . .
H21 H -0.0552 0.4852 0.2418 0.027 Uiso 1 1 calc R U . . .
C22 C -0.02579(13) 0.43346(11) 0.16779(10) 0.0199(5) Uani 1 1 d . . . . .
H22 H -0.0798 0.4397 0.1507 0.024 Uiso 1 1 calc R U . . .
C23 C 0.03648(13) 0.39623(10) 0.13767(9) 0.0141(4) Uani 1 1 d . . . . .
C24 C 0.22040(13) 0.41951(11) 0.24657(10) 0.0182(5) Uani 1 1 d . . . . .
H24 H 0.2627 0.4025 0.2176 0.022 Uiso 1 1 calc R U . . .
C25 C 0.24599(14) 0.49516(12) 0.26626(11) 0.0275(5) Uani 1 1 d . . . . .
H25A H 0.2428 0.5283 0.2336 0.041 Uiso 1 1 calc R U . . .
H25B H 0.3039 0.4941 0.2811 0.041 Uiso 1 1 calc R U . . .
H25C H 0.2076 0.5113 0.2967 0.041 Uiso 1 1 calc R U . . .
C26 C 0.22300(15) 0.36856(14) 0.29835(11) 0.0316(6) Uani 1 1 d . . . . .
H26A H 0.1868 0.3874 0.3290 0.047 Uiso 1 1 calc R U . . .
H26B H 0.2811 0.3647 0.3124 0.047 Uiso 1 1 calc R U . . .
H26C H 0.2027 0.3210 0.2867 0.047 Uiso 1 1 calc R U . . .
C27 C 0.01421(13) 0.36269(11) 0.08031(10) 0.0188(5) Uani 1 1 d . . . . .
H27 H 0.0639 0.3338 0.0672 0.023 Uiso 1 1 calc R U . . .
C28 C -0.00306(16) 0.41964(14) 0.03502(11) 0.0337(6) Uani 1 1 d . . . . .
H28A H -0.0511 0.4492 0.0471 0.051 Uiso 1 1 calc R U . . .
H28B H -0.0161 0.3964 -0.0018 0.051 Uiso 1 1 calc R U . . .
H28C H 0.0469 0.4501 0.0305 0.051 Uiso 1 1 calc R U . . .
C29 C -0.06140(17) 0.31199(14) 0.08526(12) 0.0351(6) Uani 1 1 d . . . . .
H29A H -0.0498 0.2755 0.1146 0.053 Uiso 1 1 calc R U . . .
H29B H -0.0712 0.2885 0.0481 0.053 Uiso 1 1 calc R U . . .
H29C H -0.1117 0.3395 0.0962 0.053 Uiso 1 1 calc R U . . .
O1S O 0.04922(15) 0.23092(12) 0.27281(10) 0.0632(7) Uani 1 1 d . . . . .
C1S C 0.03125(18) 0.15753(15) 0.26596(13) 0.0456(7) Uani 1 1 d . . . . .
H1S1 H 0.0253 0.1342 0.3040 0.055 Uiso 1 1 calc R U . . .
H1S2 H 0.0775 0.1335 0.2448 0.055 Uiso 1 1 calc R U . . .
C2S C -0.04859(18) 0.15189(14) 0.23326(13) 0.0421(7) Uani 1 1 d . . . . .
H2S1 H -0.0798 0.1076 0.2433 0.051 Uiso 1 1 calc R U . . .
H2S2 H -0.0384 0.1529 0.1912 0.051 Uiso 1 1 calc R U . . .
C3S C -0.0950(2) 0.21814(17) 0.25307(17) 0.0631(10) Uani 1 1 d . . . . .
H3S1 H -0.1361 0.2347 0.2238 0.076 Uiso 1 1 calc R U . . .
H3S2 H -0.1247 0.2097 0.2900 0.076 Uiso 1 1 calc R U . . .
C4S C -0.0236(2) 0.27069(15) 0.26011(14) 0.0578(10) Uani 1 1 d . . . . .
H4S1 H -0.0155 0.2985 0.2242 0.069 Uiso 1 1 calc R U . . .
H4S2 H -0.0361 0.3047 0.2918 0.069 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
In1 C1 2.2603(19) . ?
In1 Br1 2.5054(3) . ?
In1 Br2 2.5163(3) . ?
In1 Br3 2.5209(3) . ?
N1 C1 1.333(2) . ?
N1 C6 1.463(3) . ?
N1 C2 1.507(2) . ?
N2 C1 1.336(3) . ?
N2 C18 1.461(2) . ?
N2 C5 1.488(3) . ?
C2 C3 1.517(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.521(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.508(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C11 1.397(3) . ?
C6 C7 1.412(3) . ?
C7 C8 1.399(3) . ?
C7 C12 1.516(3) . ?
C8 C9 1.379(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.378(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(3) . ?
C10 H10 0.9500 . ?
C11 C15 1.523(3) . ?
C12 C13 1.530(3) . ?
C12 C14 1.540(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.530(3) . ?
C15 C17 1.533(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.405(3) . ?
C18 C19 1.408(3) . ?
C19 C20 1.390(3) . ?
C19 C24 1.523(3) . ?
C20 C21 1.384(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.374(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.394(3) . ?
C22 H22 0.9500 . ?
C23 C27 1.513(3) . ?
C24 C26 1.533(3) . ?
C24 C25 1.536(3) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.519(3) . ?
C27 C29 1.530(3) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O1S C4S 1.402(4) . ?
O1S C1S 1.405(3) . ?
C1S C2S 1.479(4) . ?
C1S H1S1 0.9900 . ?
C1S H1S2 0.9900 . ?
C2S C3S 1.508(4) . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?
C3S C4S 1.505(4) . ?
C3S H3S1 0.9900 . ?
C3S H3S2 0.9900 . ?
C4S H4S1 0.9900 . ?
C4S H4S2 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
C1 In1 Br1 123.71(5) . . ?
C1 In1 Br2 119.08(5) . . ?
Br1 In1 Br2 100.205(9) . . ?
C1 In1 Br3 101.81(5) . . ?
Br1 In1 Br3 106.728(10) . . ?
Br2 In1 Br3 103.190(10) . . ?
C1 N1 C6 119.29(16) . . ?
C1 N1 C2 127.48(16) . . ?
C6 N1 C2 113.02(15) . . ?
C1 N2 C18 122.88(16) . . ?
C1 N2 C5 122.77(17) . . ?
C18 N2 C5 114.33(16) . . ?
N1 C1 N2 121.44(17) . . ?
N1 C1 In1 119.95(14) . . ?
N2 C1 In1 117.72(13) . . ?
N1 C2 C3 115.20(17) . . ?
N1 C2 H2A 108.5 . . ?
C3 C2 H2A 108.5 . . ?
N1 C2 H2B 108.5 . . ?
C3 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
C2 C3 C4 112.6(2) . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 C3 112.01(18) . . ?
C5 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N2 C5 C4 113.38(19) . . ?
N2 C5 H5A 108.9 . . ?
C4 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C11 C6 C7 122.37(19) . . ?
C11 C6 N1 118.53(17) . . ?
C7 C6 N1 118.88(18) . . ?
C8 C7 C6 116.9(2) . . ?
C8 C7 C12 119.90(19) . . ?
C6 C7 C12 122.89(19) . . ?
C9 C8 C7 121.3(2) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C8 120.2(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 121.3(2) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 117.59(19) . . ?
C10 C11 C15 118.8(2) . . ?
C6 C11 C15 123.53(19) . . ?
C7 C12 C13 114.10(19) . . ?
C7 C12 C14 109.40(18) . . ?
C13 C12 C14 108.00(18) . . ?
C7 C12 H12 108.4 . . ?
C13 C12 H12 108.4 . . ?
C14 C12 H12 108.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C16 113.35(18) . . ?
C11 C15 C17 109.12(18) . . ?
C16 C15 C17 109.6(2) . . ?
C11 C15 H15 108.2 . . ?
C16 C15 H15 108.2 . . ?
C17 C15 H15 108.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 122.30(18) . . ?
C23 C18 N2 118.72(18) . . ?
C19 C18 N2 118.72(17) . . ?
C20 C19 C18 117.32(19) . . ?
C20 C19 C24 118.47(19) . . ?
C18 C19 C24 124.20(18) . . ?
C21 C20 C19 121.5(2) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C22 C21 C20 119.9(2) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 121.7(2) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C22 C23 C18 117.19(19) . . ?
C22 C23 C27 118.83(19) . . ?
C18 C23 C27 123.97(18) . . ?
C19 C24 C26 112.34(18) . . ?
C19 C24 C25 110.45(17) . . ?
C26 C24 C25 109.10(19) . . ?
C19 C24 H24 108.3 . . ?
C26 C24 H24 108.3 . . ?
C25 C24 H24 108.3 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 C28 111.32(18) . . ?
C23 C27 C29 111.80(19) . . ?
C28 C27 C29 110.01(19) . . ?
C23 C27 H27 107.9 . . ?
C28 C27 H27 107.9 . . ?
C29 C27 H27 107.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C4S O1S C1S 108.9(2) . . ?
O1S C1S C2S 107.5(2) . . ?
O1S C1S H1S1 110.2 . . ?
C2S C1S H1S1 110.2 . . ?
O1S C1S H1S2 110.2 . . ?
C2S C1S H1S2 110.2 . . ?
H1S1 C1S H1S2 108.5 . . ?
C1S C2S C3S 101.7(2) . . ?
C1S C2S H2S1 111.4 . . ?
C3S C2S H2S1 111.4 . . ?
C1S C2S H2S2 111.4 . . ?
C3S C2S H2S2 111.4 . . ?
H2S1 C2S H2S2 109.3 . . ?
C4S C3S C2S 101.5(3) . . ?
C4S C3S H3S1 111.5 . . ?
C2S C3S H3S1 111.5 . . ?
C4S C3S H3S2 111.5 . . ?
C2S C3S H3S2 111.5 . . ?
H3S1 C3S H3S2 109.3 . . ?
O1S C4S C3S 107.3(2) . . ?
O1S C4S H4S1 110.3 . . ?
C3S C4S H4S1 110.3 . . ?
O1S C4S H4S2 110.3 . . ?
C3S C4S H4S2 110.3 . . ?
H4S1 C4S H4S2 108.5 . . ?

_refine_diff_density_max         0.528
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.109

_shelxl_version_number           2014-3

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_h-m   'P b c a'
_symmetry_int_tables_number      61
_chemical_absolute_configuration ?

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_database_code_depnum_ccdc_archive 'CCDC 1026033'
