# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_Sb_NMP_H_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1910947'
loop_
_audit_author_name
_audit_author_address
'Shiv Pal'
;Indian Institute of Science Education and Research, Pune , India
India
;
_audit_update_record             
;
2019-04-18 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H30 I8 N4 O4 Sb2'
_chemical_formula_sum            'C16 H30 I8 N4 O4 Sb2'
_chemical_formula_weight         1601.14

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'
I I -0.4742 1.8119 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   16.8665(6)
_cell_length_b                   10.9079(4)
_cell_length_c                   20.9932(7)
_cell_angle_alpha                90
_cell_angle_beta                 107.1020(10)
_cell_angle_gamma                90
_cell_volume                     3691.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9973
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      26.72

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.881
_exptl_crystal_F_000             2848
_exptl_transmission_factor_min   0.5133
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    8.180
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'Krause, L., Herbst-Irmer,R.,SheldrickG.M. &StalkeD.,J.Appl.Cryst.48(2015)3-10'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75431
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.254
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6671
_reflns_number_gt                4899
_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'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0203P)²+18.2590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6671
_refine_ls_number_parameters     307
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0577
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_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
Sb2 Sb 0.48844(3) 0.47443(5) 0.10960(2) 0.01953(12) Uani 1 1 d . . . . .
I3 I 0.57218(3) 0.31363(4) 0.01087(2) 0.02206(12) Uani 1 1 d . . . . .
Sb1 Sb 0.74489(3) 0.44640(5) 0.06667(2) 0.01993(12) Uani 1 1 d . . . . .
I2 I 0.88651(3) 0.60761(5) 0.12138(2) 0.02527(13) Uani 1 1 d . . . . .
I5 I 0.65355(3) 0.60483(5) 0.15423(3) 0.02564(13) Uani 1 1 d . . . . .
I6 I 0.54534(4) 0.28753(5) 0.20383(2) 0.02915(14) Uani 1 1 d . . . . .
I8 I 0.32189(3) 0.35075(5) 0.05979(3) 0.03221(14) Uani 1 1 d . . . . .
I4 I 0.79939(4) 0.28781(5) 0.17596(3) 0.03322(15) Uani 1 1 d . . . . .
I7 I 0.43278(4) 0.62091(6) 0.19896(3) 0.03954(16) Uani 1 1 d . . . . .
I1 I 0.81896(4) 0.30027(6) -0.01415(3) 0.04036(16) Uani 1 1 d . . . . .
C4 C 0.7319(5) 0.4442(8) 0.3480(4) 0.029(2) Uani 1 1 d . . . . .
H4A H 0.7460 0.5070 0.3205 0.035 Uiso 1 1 calc R U . . .
H4B H 0.7405 0.3642 0.3311 0.035 Uiso 1 1 calc R U . . .
C5 C 0.9396(5) 0.5234(6) 0.6823(4) 0.0221(18) Uani 1 1 d . . . . .
C1 C 0.6393(5) 0.4527(7) 0.4093(4) 0.0226(18) Uani 1 1 d . . . . .
C2 C 0.7192(5) 0.4422(8) 0.4610(4) 0.029(2) Uani 1 1 d . . . . .
H2A H 0.7251 0.3626 0.4825 0.035 Uiso 1 1 calc R U . . .
H2B H 0.7254 0.5056 0.4945 0.035 Uiso 1 1 calc R U . . .
C9 C 0.7044(5) 0.5866(8) 0.6713(4) 0.028(2) Uani 1 1 d . . . . .
C3 C 0.7831(5) 0.4588(8) 0.4214(4) 0.036(2) Uani 1 1 d . . . . .
H3A H 0.8086 0.5393 0.4293 0.043 Uiso 1 1 calc R U . . .
H3B H 0.8262 0.3970 0.4339 0.043 Uiso 1 1 calc R U . . .
C13 C 0.5712(5) 0.3186(8) 0.5607(4) 0.030(2) Uani 1 1 d . . . . .
C6 C 0.9159(6) 0.5175(8) 0.6080(4) 0.037(2) Uani 1 1 d . . . . .
H6A H 0.8852 0.5901 0.5882 0.044 Uiso 1 1 calc R U . . .
H6B H 0.8824 0.4455 0.5914 0.044 Uiso 1 1 calc R U . . .
C8 C 1.0644(6) 0.5437(8) 0.6577(5) 0.044(3) Uani 1 1 d . . . . .
H8A H 1.1097 0.4852 0.6682 0.053 Uiso 1 1 calc R U . . .
H8B H 1.0864 0.6252 0.6554 0.053 Uiso 1 1 calc R U . . .
C7 C 0.9994(6) 0.5105(8) 0.5930(5) 0.048(3) Uani 1 1 d . . . . .
H7A H 1.0089 0.4285 0.5790 0.058 Uiso 1 1 calc R U . . .
H7B H 1.0008 0.5678 0.5580 0.058 Uiso 1 1 calc R U . . .
N4 N 0.5651(7) 0.3016(8) 0.6286(4) 0.075(3) Uani 1 1 d . . . . .
H4 H 0.5706 0.3563 0.6591 0.090 Uiso 1 1 calc R U . . .
C10 C 0.7345(6) 0.6728(9) 0.7269(5) 0.054(3) Uani 1 1 d . . . . .
H10A H 0.7832 0.7165 0.7235 0.065 Uiso 1 1 calc R U . . .
H10B H 0.7482 0.6304 0.7694 0.065 Uiso 1 1 calc R U . . .
C12 C 0.5906(5) 0.7088(9) 0.6647(5) 0.051(3) Uani 1 1 d . . . . .
H12A H 0.5460 0.6825 0.6820 0.062 Uiso 1 1 calc R U . . .
H12B H 0.5694 0.7695 0.6301 0.062 Uiso 1 1 calc R U . . .
C11 C 0.6632(7) 0.7586(12) 0.7197(6) 0.080(4) Uani 1 1 d . U . . .
H11A H 0.6776 0.8401 0.7082 0.096 Uiso 1 1 calc R U . . .
H11B H 0.6490 0.7635 0.7612 0.096 Uiso 1 1 calc R U . . .
C15 C 0.5472(7) 0.1670(9) 0.6328(5) 0.057(3) Uani 1 1 d . . . . .
H15A H 0.5784 0.1335 0.6756 0.069 Uiso 1 1 calc R U . . .
H15B H 0.4885 0.1532 0.6262 0.069 Uiso 1 1 calc R U . . .
C16 C 0.5744(7) 0.1106(10) 0.5772(6) 0.067(3) Uani 1 1 d . . . . .
H16A H 0.6296 0.0760 0.5940 0.080 Uiso 1 1 calc R U . . .
H16B H 0.5363 0.0466 0.5550 0.080 Uiso 1 1 calc R U . . .
O8 O 0.5726(3) 0.4233(5) 0.5362(3) 0.0312(14) Uani 1 1 d . . . . .
O5 O 0.5673(3) 0.4558(5) 0.4191(2) 0.0316(14) Uani 1 1 d . . . . .
H5 H 0.5728 0.4509 0.4591 0.047 Uiso 1 1 calc R U . . .
O6 O 0.8913(3) 0.5169(5) 0.7184(3) 0.0335(14) Uani 1 1 d . . . . .
H6 H 0.8434 0.5085 0.6946 0.050 Uiso 1 1 calc R U . . .
O7 O 0.7460(3) 0.4997(5) 0.6562(3) 0.0419(16) Uani 1 1 d . . . . .
N1 N 0.6473(4) 0.4582(6) 0.3501(3) 0.0278(16) Uani 1 1 d . . . . .
H1 H 0.6061 0.4691 0.3150 0.033 Uiso 1 1 calc R U . . .
N2 N 1.0187(4) 0.5385(6) 0.7066(3) 0.0266(16) Uani 1 1 d . . . . .
H2 H 1.0426 0.5451 0.7487 0.032 Uiso 1 1 calc R U . . .
N3 N 0.6270(4) 0.6056(6) 0.6399(3) 0.0274(16) Uani 1 1 d . . . . .
H3 H 0.5995 0.5608 0.6071 0.033 Uiso 1 1 calc R U . . .
C14 C 0.5737(5) 0.2122(7) 0.5316(4) 0.0229(18) Uani 1 1 d . . . . .
H4C H 0.6231 0.2083 0.5170 0.027 Uiso 1 1 calc R U . . .
H4D H 0.5258 0.2047 0.4926 0.027 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
Sb2 I6 2.8059(7) . ?
Sb2 I7 2.8265(7) . ?
Sb2 I8 3.0128(7) . ?
Sb2 I5 3.0202(7) . ?
I3 Sb1 3.1542(7) . ?
Sb1 I4 2.8037(7) . ?
Sb1 I1 2.8683(8) . ?
Sb1 I2 2.9160(7) . ?
Sb1 I5 3.2253(7) . ?
C4 N1 1.447(10) . ?
C4 C3 1.536(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O6 1.267(9) . ?
C5 N2 1.291(9) . ?
C5 C6 1.492(11) . ?
C1 O5 1.290(9) . ?
C1 N1 1.291(9) . ?
C1 C2 1.466(10) . ?
C2 C3 1.554(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C9 O7 1.274(10) . ?
C9 N3 1.294(9) . ?
C9 C10 1.469(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C13 O8 1.256(9) . ?
C13 C14 1.319(11) . ?
C13 N4 1.470(11) . ?
C6 C7 1.534(12) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C8 N2 1.455(10) . ?
C8 C7 1.516(13) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
N4 C15 1.507(12) . ?
N4 H4 0.8600 . ?
C10 C11 1.496(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 N3 1.450(10) . ?
C12 C11 1.516(14) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C15 C16 1.505(14) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C14 1.461(13) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
O5 H5 0.8200 . ?
O6 H6 0.8200 . ?
N1 H1 0.8600 . ?
N2 H2 0.8600 . ?
N3 H3 0.8600 . ?
C14 H4C 0.9700 . ?
C14 H4D 0.9700 . ?

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
I6 Sb2 I7 93.11(2) . . ?
I6 Sb2 I8 90.58(2) . . ?
I7 Sb2 I8 91.47(2) . . ?
I6 Sb2 I5 91.75(2) . . ?
I7 Sb2 I5 89.08(2) . . ?
I8 Sb2 I5 177.58(2) . . ?
I4 Sb1 I1 92.64(2) . . ?
I4 Sb1 I2 90.93(2) . . ?
I1 Sb1 I2 96.85(2) . . ?
I4 Sb1 I3 93.75(2) . . ?
I1 Sb1 I3 92.32(2) . . ?
I2 Sb1 I3 169.50(2) . . ?
I4 Sb1 I5 87.76(2) . . ?
I1 Sb1 I5 177.37(2) . . ?
I2 Sb1 I5 85.737(19) . . ?
I3 Sb1 I5 85.063(18) . . ?
Sb2 I5 Sb1 97.025(19) . . ?
N1 C4 C3 103.2(6) . . ?
N1 C4 H4A 111.1 . . ?
C3 C4 H4A 111.1 . . ?
N1 C4 H4B 111.1 . . ?
C3 C4 H4B 111.1 . . ?
H4A C4 H4B 109.1 . . ?
O6 C5 N2 122.8(7) . . ?
O6 C5 C6 126.9(7) . . ?
N2 C5 C6 110.2(7) . . ?
O5 C1 N1 121.5(7) . . ?
O5 C1 C2 126.0(7) . . ?
N1 C1 C2 112.5(7) . . ?
C1 C2 C3 103.0(6) . . ?
C1 C2 H2A 111.2 . . ?
C3 C2 H2A 111.2 . . ?
C1 C2 H2B 111.2 . . ?
C3 C2 H2B 111.2 . . ?
H2A C2 H2B 109.1 . . ?
O7 C9 N3 122.6(8) . . ?
O7 C9 C10 126.0(8) . . ?
N3 C9 C10 111.3(8) . . ?
C4 C3 C2 104.5(7) . . ?
C4 C3 H3A 110.8 . . ?
C2 C3 H3A 110.8 . . ?
C4 C3 H3B 110.8 . . ?
C2 C3 H3B 110.8 . . ?
H3A C3 H3B 108.9 . . ?
O8 C13 C14 127.1(8) . . ?
O8 C13 N4 121.9(8) . . ?
C14 C13 N4 111.0(8) . . ?
C5 C6 C7 103.8(7) . . ?
C5 C6 H6A 111.0 . . ?
C7 C6 H6A 111.0 . . ?
C5 C6 H6B 111.0 . . ?
C7 C6 H6B 111.0 . . ?
H6A C6 H6B 109.0 . . ?
N2 C8 C7 103.3(7) . . ?
N2 C8 H8A 111.1 . . ?
C7 C8 H8A 111.1 . . ?
N2 C8 H8B 111.1 . . ?
C7 C8 H8B 111.1 . . ?
H8A C8 H8B 109.1 . . ?
C8 C7 C6 105.6(7) . . ?
C8 C7 H7A 110.6 . . ?
C6 C7 H7A 110.6 . . ?
C8 C7 H7B 110.6 . . ?
C6 C7 H7B 110.6 . . ?
H7A C7 H7B 108.8 . . ?
C13 N4 C15 104.6(8) . . ?
C13 N4 H4 127.7 . . ?
C15 N4 H4 127.7 . . ?
C9 C10 C11 103.9(8) . . ?
C9 C10 H10A 111.0 . . ?
C11 C10 H10A 111.0 . . ?
C9 C10 H10B 111.0 . . ?
C11 C10 H10B 111.0 . . ?
H10A C10 H10B 109.0 . . ?
N3 C12 C11 102.6(8) . . ?
N3 C12 H12A 111.2 . . ?
C11 C12 H12A 111.2 . . ?
N3 C12 H12B 111.2 . . ?
C11 C12 H12B 111.2 . . ?
H12A C12 H12B 109.2 . . ?
C10 C11 C12 107.4(9) . . ?
C10 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
C10 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
C16 C15 N4 104.0(8) . . ?
C16 C15 H15A 111.0 . . ?
N4 C15 H15A 111.0 . . ?
C16 C15 H15B 111.0 . . ?
N4 C15 H15B 111.0 . . ?
H15A C15 H15B 109.0 . . ?
C14 C16 C15 104.6(8) . . ?
C14 C16 H16A 110.8 . . ?
C15 C16 H16A 110.8 . . ?
C14 C16 H16B 110.8 . . ?
C15 C16 H16B 110.8 . . ?
H16A C16 H16B 108.9 . . ?
C1 O5 H5 109.5 . . ?
C5 O6 H6 109.5 . . ?
C1 N1 C4 114.1(7) . . ?
C1 N1 H1 123.0 . . ?
C4 N1 H1 123.0 . . ?
C5 N2 C8 115.2(7) . . ?
C5 N2 H2 122.4 . . ?
C8 N2 H2 122.4 . . ?
C9 N3 C12 114.3(7) . . ?
C9 N3 H3 122.8 . . ?
C12 N3 H3 122.8 . . ?
C13 C14 C16 111.1(8) . . ?
C13 C14 H4C 109.4 . . ?
C16 C14 H4C 109.4 . . ?
C13 C14 H4D 109.4 . . ?
C16 C14 H4D 109.4 . . ?
H4C C14 H4D 108.0 . . ?

_refine_diff_density_max         0.988
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.241


_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_A1A1AQ_a_a
_database_code_depnum_ccdc_archive 'CCDC 1910950'
loop_
_audit_author_name
_audit_author_address
'Shiv Pal'
;Indian Institute of Science Education and Research, Pune , India
India
;
_audit_update_record             
;
2019-04-25 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H57 I12 N6 O6 Sb3'
_chemical_formula_weight         2485.86

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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'

_cell_length_a                   28.114(5)
_cell_length_b                   11.329(2)
_cell_length_c                   19.332(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6157.3(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9798
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      26.82

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.678
_exptl_crystal_F_000             4452
_exptl_transmission_factor_min   0.4877
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    7.361
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            167392
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_av_R_equivalents  0.1635
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.206
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11146
_reflns_number_gt                8068
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0190P)²+2.3795P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11146
_refine_ls_number_parameters     522
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.0676
_refine_ls_wR_factor_gt          0.0583
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_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
I8 I 0.73455(4) 0.90959(11) 0.27778(6) 0.0242(3) Uani 1 1 d . . . . .
I6 I 0.60341(4) 1.10247(11) 0.28440(6) 0.0237(3) Uani 1 1 d . . . . .
I7 I 0.72695(4) 1.21574(9) 0.39797(7) 0.0246(3) Uani 1 1 d . . . . .
I4 I 0.60733(4) 0.77596(9) 0.38289(7) 0.0247(3) Uani 1 1 d . . . . .
I9 I 0.73455(4) 0.88776(12) 0.49707(6) 0.0257(3) Uani 1 1 d . . . . .
I5 I 0.60650(4) 1.09901(11) 0.50229(6) 0.0277(3) Uani 1 1 d . . . . .
I3 I 0.47185(4) 1.19858(10) 0.41605(7) 0.0359(3) Uani 1 1 d . . . . .
I2 I 0.47942(4) 0.87945(10) 0.51138(6) 0.0330(3) Uani 1 1 d . . . . .
I1 I 0.46602(4) 0.89663(11) 0.29601(6) 0.0359(3) Uani 1 1 d . . . . .
I10 I 0.86443(4) 0.13068(11) 0.28985(6) 0.0348(3) Uani 1 1 d . . . . .
I12 I 0.86669(4) -0.19722(9) 0.38499(7) 0.0354(3) Uani 1 1 d . . . . .
I11 I 0.86497(4) 0.10373(11) 0.50158(6) 0.0329(3) Uani 1 1 d . . . . .
C1 C 0.7859(8) 0.5304(18) 0.3457(9) 0.062(7) Uani 1 1 d . . . . .
H1A H 0.7885 0.4680 0.3116 0.075 Uiso 1 1 calc R U . . .
H1B H 0.8047 0.5975 0.3308 0.075 Uiso 1 1 calc R U . . .
C2 C 0.5312(8) 0.4828(17) 0.3388(9) 0.055(6) Uani 1 1 d . . . . .
H2A H 0.5214 0.4098 0.3167 0.066 Uiso 1 1 calc R U . . .
H2B H 0.5459 0.5336 0.3046 0.066 Uiso 1 1 calc R U . . .
C3 C 0.7335(8) 0.5656(18) 0.3572(11) 0.068(7) Uani 1 1 d . . . . .
H3A H 0.7285 0.6474 0.3445 0.082 Uiso 1 1 calc R U . . .
H3B H 0.7126 0.5164 0.3296 0.082 Uiso 1 1 calc R U . . .
C4 C 0.5475(7) 0.4941(14) 0.4531(9) 0.028(4) Uani 1 1 d . . . . .
C5 C 0.7239(8) 0.5474(16) 0.4337(9) 0.054(6) Uani 1 1 d . . . . .
H5A H 0.7168 0.6218 0.4563 0.065 Uiso 1 1 calc R U . . .
H5B H 0.6975 0.4936 0.4408 0.065 Uiso 1 1 calc R U . . .
C6 C 0.8654(6) 0.2155(14) 0.6812(8) 0.031(5) Uani 1 1 d . . . . .
H6A H 0.8587 0.2228 0.7302 0.037 Uiso 1 1 calc R U . . .
H6B H 0.8386 0.1769 0.6591 0.037 Uiso 1 1 calc R U . . .
C7 C 0.6087(6) 0.4062(15) 0.3836(12) 0.069(7) Uani 1 1 d . . . . .
H7A H 0.6297 0.4624 0.3624 0.104 Uiso 1 1 calc R U . . .
H7B H 0.6051 0.3392 0.3536 0.104 Uiso 1 1 calc R U . . .
H7C H 0.6218 0.3811 0.4270 0.104 Uiso 1 1 calc R U . . .
C8 C 0.7603(7) 0.7897(18) 0.7031(10) 0.055(7) Uani 1 1 d . . . . .
H8A H 0.7667 0.8477 0.7380 0.083 Uiso 1 1 calc R U . . .
H8B H 0.7506 0.7172 0.7246 0.083 Uiso 1 1 calc R U . . .
H8C H 0.7353 0.8176 0.6734 0.083 Uiso 1 1 calc R U . . .
C9 C 0.8474(6) 0.4440(16) 0.4223(9) 0.048(6) Uani 1 1 d . . . . .
H9A H 0.8704 0.5047 0.4132 0.072 Uiso 1 1 calc R U . . .
H9B H 0.8524 0.3793 0.3910 0.072 Uiso 1 1 calc R U . . .
H9C H 0.8509 0.4169 0.4690 0.072 Uiso 1 1 calc R U . . .
C10 C 0.6118(7) 0.7159(19) 0.5877(10) 0.052(7) Uani 1 1 d . . . . .
H10A H 0.6075 0.7345 0.5391 0.062 Uiso 1 1 calc R U . . .
H10B H 0.6347 0.6521 0.5918 0.062 Uiso 1 1 calc R U . . .
C11 C 0.7380(8) 0.235(2) 0.6087(10) 0.069(7) Uani 1 1 d . . . . .
H11A H 0.7684 0.2661 0.6235 0.082 Uiso 1 1 calc R U . . .
H11B H 0.7412 0.2046 0.5619 0.082 Uiso 1 1 calc R U . . .
C12 C 0.5849(6) 0.8639(15) 0.6671(9) 0.037(5) Uani 1 1 d . . . . .
H12A H 0.5927 0.8824 0.7148 0.045 Uiso 1 1 calc R U . . .
H12B H 0.5706 0.9327 0.6456 0.045 Uiso 1 1 calc R U . . .
C13 C 0.8391(6) 0.8361(16) 0.6615(10) 0.033(5) Uani 1 1 d . . . . .
C14 C 0.5004(7) 0.5458(16) 0.4489(10) 0.052(6) Uani 1 1 d . . . . .
H14A H 0.5003 0.6261 0.4663 0.062 Uiso 1 1 calc R U . . .
H14B H 0.4774 0.4995 0.4747 0.062 Uiso 1 1 calc R U . . .
C15 C 0.7014(8) 0.326(2) 0.6116(10) 0.040(6) Uani 1 1 d . . . . .
C16 C 0.9094(7) 0.1463(16) 0.6702(8) 0.028(5) Uani 1 1 d . . . . .
C17 C 0.8058(7) 0.6678(16) 0.6193(9) 0.041(6) Uani 1 1 d . . . . .
H17A H 0.7806 0.6682 0.5849 0.050 Uiso 1 1 calc R U . . .
H17B H 0.8031 0.5961 0.6465 0.050 Uiso 1 1 calc R U . . .
C18 C 0.8738(6) 0.3347(14) 0.6498(9) 0.035(5) Uani 1 1 d . . . . .
H18A H 0.8628 0.3970 0.6803 0.042 Uiso 1 1 calc R U . . .
H18B H 0.8578 0.3419 0.6056 0.042 Uiso 1 1 calc R U . . .
C19 C 0.9284(7) 0.3389(15) 0.6410(11) 0.045(5) Uani 1 1 d . . . . .
H19A H 0.9372 0.3706 0.5962 0.054 Uiso 1 1 calc R U . . .
H19B H 0.9431 0.3862 0.6769 0.054 Uiso 1 1 calc R U . . .
C20 C 0.6712(8) 0.1718(18) 0.6775(9) 0.053(7) Uani 1 1 d . . . . .
H20A H 0.6481 0.1176 0.6579 0.064 Uiso 1 1 calc R U . . .
H20B H 0.6674 0.1734 0.7274 0.064 Uiso 1 1 calc R U . . .
C21 C 0.8752(7) 0.7908(15) 0.6124(8) 0.040(6) Uani 1 1 d . . . . .
H21A H 0.9053 0.7759 0.6355 0.048 Uiso 1 1 calc R U . . .
H21B H 0.8805 0.8460 0.5748 0.048 Uiso 1 1 calc R U . . .
C22 C 0.7215(8) 0.1374(17) 0.6575(11) 0.057(7) Uani 1 1 d . . . . .
H22A H 0.7219 0.0613 0.6344 0.069 Uiso 1 1 calc R U . . .
H22B H 0.7419 0.1334 0.6980 0.069 Uiso 1 1 calc R U . . .
C23 C 0.5659(8) 0.6831(19) 0.6202(8) 0.038(6) Uani 1 1 d . . . . .
C24 C 0.6224(7) 0.3540(19) 0.6585(10) 0.069(7) Uani 1 1 d . . . . .
H24A H 0.6282 0.4369 0.6527 0.104 Uiso 1 1 calc R U . . .
H24B H 0.6107 0.3395 0.7043 0.104 Uiso 1 1 calc R U . . .
H24C H 0.5991 0.3285 0.6252 0.104 Uiso 1 1 calc R U . . .
C25 C 0.9905(6) 0.1794(16) 0.6341(11) 0.057(6) Uani 1 1 d . . . . .
H25A H 0.9922 0.0948 0.6349 0.085 Uiso 1 1 calc R U . . .
H25B H 1.0110 0.2111 0.6693 0.085 Uiso 1 1 calc R U . . .
H25C H 1.0006 0.2078 0.5896 0.085 Uiso 1 1 calc R U . . .
C26 C 0.5078(7) 0.7630(18) 0.6995(9) 0.058(6) Uani 1 1 d . . . . .
H26A H 0.4979 0.6832 0.7081 0.087 Uiso 1 1 calc R U . . .
H26B H 0.4844 0.8021 0.6716 0.087 Uiso 1 1 calc R U . . .
H26C H 0.5113 0.8040 0.7426 0.087 Uiso 1 1 calc R U . . .
C27 C 0.8529(8) 0.6745(18) 0.5856(11) 0.068(7) Uani 1 1 d . . . . .
H27A H 0.8496 0.6762 0.5356 0.082 Uiso 1 1 calc R U . . .
H27B H 0.8724 0.6072 0.5983 0.082 Uiso 1 1 calc R U . . .
C28 C 0.7696(6) 0.4956(16) 0.4607(10) 0.035(5) Uani 1 1 d . . . . .
C29 C 0.6285(7) 0.8247(17) 0.6279(10) 0.051(6) Uani 1 1 d . . . . .
H29A H 0.6541 0.8046 0.6594 0.061 Uiso 1 1 calc R U . . .
H29B H 0.6394 0.8860 0.5967 0.061 Uiso 1 1 calc R U . . .
C30 C 0.4901(8) 0.5423(17) 0.3723(12) 0.064(7) Uani 1 1 d . . . . .
H30A H 0.4610 0.4988 0.3634 0.077 Uiso 1 1 calc R U . . .
H30B H 0.4865 0.6218 0.3543 0.077 Uiso 1 1 calc R U . . .
Sb2 Sb 0.66864(4) 0.99729(9) 0.39008(7) 0.0154(2) Uani 1 1 d . . . . .
Sb1 Sb 0.52476(3) 0.99219(9) 0.40073(6) 0.0191(3) Uani 1 1 d . . . . .
Sb3 Sb 0.81270(3) 0.00813(8) 0.39162(6) 0.0173(2) Uani 1 1 d . . . . .
O1 O 0.7753(4) 0.4608(10) 0.5209(6) 0.046(3) Uani 1 1 d . . . . .
O2 O 0.8418(4) 0.9320(10) 0.6976(6) 0.044(3) Uani 1 1 d . . . . .
H2 H 0.8670 0.9655 0.6894 0.066 Uiso 1 1 calc R U . . .
O3 O 0.5724(4) 0.4806(10) 0.5083(6) 0.055(4) Uani 1 1 d . . . . .
H3 H 0.5575 0.5056 0.5417 0.083 Uiso 1 1 calc R U . . .
O4 O 0.7013(5) 0.4281(12) 0.5838(7) 0.050(4) Uani 1 1 d . . . . .
H4 H 0.7265 0.4385 0.5633 0.076 Uiso 1 1 calc R U . . .
O5 O 0.5425(5) 0.5914(11) 0.6069(6) 0.057(4) Uani 1 1 d . . . . .
O6 O 0.9160(4) 0.0389(10) 0.6800(6) 0.042(3) Uani 1 1 d . . . . .
N1 N 0.5631(4) 0.4600(10) 0.3950(9) 0.037(4) Uani 1 1 d . . . . .
N2 N 0.8008(6) 0.4900(13) 0.4128(9) 0.051(5) Uani 1 1 d . . . . .
N3 N 0.9418(5) 0.2168(12) 0.6470(9) 0.036(4) Uani 1 1 d . . . . .
N4 N 0.8022(6) 0.7698(14) 0.6632(7) 0.035(4) Uani 1 1 d . . . . .
N5 N 0.5532(5) 0.7624(14) 0.6631(7) 0.035(4) Uani 1 1 d . . . . .
N6 N 0.6661(6) 0.2892(14) 0.6481(8) 0.042(4) Uani 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
I8 Sb2 3.0222(17) . ?
I6 Sb2 2.9927(17) . ?
I7 Sb2 2.9726(15) . ?
I4 Sb2 3.0458(15) . ?
I9 Sb2 3.0418(17) . ?
I5 Sb2 3.0143(17) . ?
I3 Sb1 2.7871(15) . ?
I2 Sb1 2.7985(16) . ?
I1 Sb1 2.8280(17) . ?
I10 Sb3 2.8131(16) . ?
I12 Sb3 2.7807(14) . ?
I11 Sb3 2.8021(16) . ?
C1 N2 1.44(2) . ?
C1 C3 1.54(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.43(2) . ?
C2 C30 1.49(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C5 1.52(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.266(19) . ?
C4 O3 1.287(18) . ?
C4 C14 1.45(2) . ?
C5 C28 1.51(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C16 1.48(2) . ?
C6 C18 1.50(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N1 1.438(18) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N4 1.43(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N2 1.42(2) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C23 1.48(3) . ?
C10 C29 1.53(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C15 1.46(3) . ?
C11 C22 1.52(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N5 1.46(2) . ?
C12 C29 1.51(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N4 1.28(2) . ?
C13 O2 1.29(2) . ?
C13 C21 1.48(2) . ?
C14 C30 1.51(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 O4 1.28(2) . ?
C15 N6 1.28(2) . ?
C16 O6 1.245(18) . ?
C16 N3 1.29(2) . ?
C17 N4 1.44(2) . ?
C17 C27 1.48(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.55(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N3 1.438(19) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N6 1.45(2) . ?
C20 C22 1.52(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C27 1.55(2) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 O5 1.26(2) . ?
C23 N5 1.27(2) . ?
C24 N6 1.45(2) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 N3 1.45(2) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 N5 1.46(2) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 O1 1.24(2) . ?
C28 N2 1.28(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
O2 H2 0.8200 . ?
O3 H3 0.8200 . ?
O4 H4 0.8200 . ?

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 C1 C3 103.3(17) . . ?
N2 C1 H1A 111.1 . . ?
C3 C1 H1A 111.1 . . ?
N2 C1 H1B 111.1 . . ?
C3 C1 H1B 111.1 . . ?
H1A C1 H1B 109.1 . . ?
N1 C2 C30 103.8(15) . . ?
N1 C2 H2A 111.0 . . ?
C30 C2 H2A 111.0 . . ?
N1 C2 H2B 111.0 . . ?
C30 C2 H2B 111.0 . . ?
H2A C2 H2B 109.0 . . ?
C5 C3 C1 106.0(17) . . ?
C5 C3 H3A 110.5 . . ?
C1 C3 H3A 110.5 . . ?
C5 C3 H3B 110.5 . . ?
C1 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N1 C4 O3 120.7(18) . . ?
N1 C4 C14 113.0(16) . . ?
O3 C4 C14 126.2(17) . . ?
C28 C5 C3 103.8(19) . . ?
C28 C5 H5A 111.0 . . ?
C3 C5 H5A 111.0 . . ?
C28 C5 H5B 111.0 . . ?
C3 C5 H5B 111.0 . . ?
H5A C5 H5B 109.0 . . ?
C16 C6 C18 106.8(15) . . ?
C16 C6 H6A 110.4 . . ?
C18 C6 H6A 110.4 . . ?
C16 C6 H6B 110.4 . . ?
C18 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C23 C10 C29 104.7(17) . . ?
C23 C10 H10A 110.8 . . ?
C29 C10 H10A 110.8 . . ?
C23 C10 H10B 110.8 . . ?
C29 C10 H10B 110.8 . . ?
H10A C10 H10B 108.9 . . ?
C15 C11 C22 105.9(18) . . ?
C15 C11 H11A 110.6 . . ?
C22 C11 H11A 110.6 . . ?
C15 C11 H11B 110.6 . . ?
C22 C11 H11B 110.6 . . ?
H11A C11 H11B 108.7 . . ?
N5 C12 C29 103.8(15) . . ?
N5 C12 H12A 111.0 . . ?
C29 C12 H12A 111.0 . . ?
N5 C12 H12B 111.0 . . ?
C29 C12 H12B 111.0 . . ?
H12A C12 H12B 109.0 . . ?
N4 C13 O2 121.6(19) . . ?
N4 C13 C21 111.6(18) . . ?
O2 C13 C21 126.7(16) . . ?
C4 C14 C30 102.6(16) . . ?
C4 C14 H14A 111.2 . . ?
C30 C14 H14A 111.2 . . ?
C4 C14 H14B 111.2 . . ?
C30 C14 H14B 111.2 . . ?
H14A C14 H14B 109.2 . . ?
O4 C15 N6 121(2) . . ?
O4 C15 C11 129(2) . . ?
N6 C15 C11 110(2) . . ?
O6 C16 N3 123.6(18) . . ?
O6 C16 C6 128.2(18) . . ?
N3 C16 C6 108.2(16) . . ?
N4 C17 C27 106.4(17) . . ?
N4 C17 H17A 110.5 . . ?
C27 C17 H17A 110.5 . . ?
N4 C17 H17B 110.5 . . ?
C27 C17 H17B 110.5 . . ?
H17A C17 H17B 108.6 . . ?
C6 C18 C19 103.1(14) . . ?
C6 C18 H18A 111.1 . . ?
C19 C18 H18A 111.1 . . ?
C6 C18 H18B 111.1 . . ?
C19 C18 H18B 111.1 . . ?
H18A C18 H18B 109.1 . . ?
N3 C19 C18 102.8(14) . . ?
N3 C19 H19A 111.2 . . ?
C18 C19 H19A 111.2 . . ?
N3 C19 H19B 111.2 . . ?
C18 C19 H19B 111.2 . . ?
H19A C19 H19B 109.1 . . ?
N6 C20 C22 103.0(17) . . ?
N6 C20 H20A 111.2 . . ?
C22 C20 H20A 111.2 . . ?
N6 C20 H20B 111.2 . . ?
C22 C20 H20B 111.2 . . ?
H20A C20 H20B 109.1 . . ?
C13 C21 C27 103.4(16) . . ?
C13 C21 H21A 111.1 . . ?
C27 C21 H21A 111.1 . . ?
C13 C21 H21B 111.1 . . ?
C27 C21 H21B 111.1 . . ?
H21A C21 H21B 109.0 . . ?
C20 C22 C11 104.8(17) . . ?
C20 C22 H22A 110.8 . . ?
C11 C22 H22A 110.8 . . ?
C20 C22 H22B 110.8 . . ?
C11 C22 H22B 110.8 . . ?
H22A C22 H22B 108.9 . . ?
O5 C23 N5 125(2) . . ?
O5 C23 C10 125.2(19) . . ?
N5 C23 C10 110.0(19) . . ?
N6 C24 H24A 109.5 . . ?
N6 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N6 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 H26A 109.5 . . ?
N5 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N5 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C17 C27 C21 105.0(16) . . ?
C17 C27 H27A 110.7 . . ?
C21 C27 H27A 110.7 . . ?
C17 C27 H27B 110.7 . . ?
C21 C27 H27B 110.7 . . ?
H27A C27 H27B 108.8 . . ?
O1 C28 N2 125.1(19) . . ?
O1 C28 C5 124.2(18) . . ?
N2 C28 C5 110.7(19) . . ?
C12 C29 C10 104.1(16) . . ?
C12 C29 H29A 110.9 . . ?
C10 C29 H29A 110.9 . . ?
C12 C29 H29B 110.9 . . ?
C10 C29 H29B 110.9 . . ?
H29A C29 H29B 109.0 . . ?
C2 C30 C14 106.9(17) . . ?
C2 C30 H30A 110.4 . . ?
C14 C30 H30A 110.4 . . ?
C2 C30 H30B 110.4 . . ?
C14 C30 H30B 110.4 . . ?
H30A C30 H30B 108.6 . . ?
I7 Sb2 I6 92.38(5) . . ?
I7 Sb2 I5 87.96(5) . . ?
I6 Sb2 I5 89.08(4) . . ?
I7 Sb2 I8 88.42(5) . . ?
I6 Sb2 I8 90.94(5) . . ?
I5 Sb2 I8 176.38(6) . . ?
I7 Sb2 I9 88.21(5) . . ?
I6 Sb2 I9 179.38(6) . . ?
I5 Sb2 I9 91.13(5) . . ?
I8 Sb2 I9 88.90(4) . . ?
I7 Sb2 I4 178.96(5) . . ?
I6 Sb2 I4 87.13(4) . . ?
I5 Sb2 I4 91.12(5) . . ?
I8 Sb2 I4 92.50(5) . . ?
I9 Sb2 I4 92.29(5) . . ?
I3 Sb1 I2 93.36(5) . . ?
I3 Sb1 I1 94.91(5) . . ?
I2 Sb1 I1 96.11(5) . . ?
I12 Sb3 I11 94.13(5) . . ?
I12 Sb3 I10 95.65(5) . . ?
I11 Sb3 I10 93.94(4) . . ?
C13 O2 H2 109.5 . . ?
C4 O3 H3 109.5 . . ?
C15 O4 H4 109.5 . . ?
C4 N1 C2 113.6(15) . . ?
C4 N1 C7 125.1(18) . . ?
C2 N1 C7 121.2(19) . . ?
C28 N2 C9 123.9(19) . . ?
C28 N2 C1 116.0(19) . . ?
C9 N2 C1 120.1(17) . . ?
C16 N3 C19 115.9(16) . . ?
C16 N3 C25 122.9(16) . . ?
C19 N3 C25 120.9(16) . . ?
C13 N4 C8 126.2(19) . . ?
C13 N4 C17 113.5(17) . . ?
C8 N4 C17 120.3(18) . . ?
C23 N5 C12 114.9(17) . . ?
C23 N5 C26 124.2(18) . . ?
C12 N5 C26 120.4(16) . . ?
C15 N6 C24 124.7(19) . . ?
C15 N6 C20 115.7(19) . . ?
C24 N6 C20 119(2) . . ?

_refine_diff_density_max         0.849
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.220

####################################################################### 
# 
# 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_aaa1_a_sqd
_database_code_depnum_ccdc_archive 'CCDC 1910951'
loop_
_audit_author_name
_audit_author_address
'Shiv Pal'
;Indian Institute of Science Education and Research, Pune , India
India
;
_audit_update_record             
;
2019-04-18 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'I9 Sb2, 2(C3 H7 N O), 2(C3 H8 N O)'
_chemical_formula_sum            'C12 H30 I9 N4 O4 Sb2'
_chemical_formula_weight         1680.00

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'
I I -0.4742 1.8119 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   15.1734(8)
_cell_length_b                   30.0131(16)
_cell_length_c                   9.0791(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4134.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7666
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      28.19

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.699
_exptl_crystal_F_000             2964
_exptl_transmission_factor_min   0.5043
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.011
_exptl_absorpt_coefficient_mu    8.047
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'SADABS 2016/2: Krause, L.,Herbst-Irmer,R.,Sheldrick G.M. & Stalke D.,J. Appl.Cryst.48 (2015)3-10'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22566
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.344
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3819
_reflns_number_gt                2833
_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'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0251P)²+13.6427P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3819
_refine_ls_number_parameters     161
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0707
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
I4 I 0.02565(4) 0.7500 0.29333(7) 0.02796(17) Uani 1 2 d S T P A 1
I5 I 0.28656(4) 0.7500 0.45430(8) 0.03353(19) Uani 1 2 d S T P A 1
Sb3 Sb 0.13063(3) 0.68234(2) 0.48824(5) 0.02482(13) Uani 1 1 d . . . A 1
I3 I 0.23559(3) 0.62815(2) 0.68905(6) 0.04042(16) Uani 1 1 d . . . A 1
I2 I -0.02910(3) 0.62901(2) 0.53233(6) 0.04286(16) Uani 1 1 d . . . A 1
I6 I 0.07737(5) 0.7500 0.75028(8) 0.0427(2) Uani 1 2 d S T P A 1
I1B I 0.1777(4) 0.6247(4) 0.2545(10) 0.0369(14) Uani 0.45(2) 1 d . U P B 2
I1 I 0.1928(3) 0.6396(3) 0.2205(7) 0.0362(11) Uani 0.55(2) 1 d . . P A 1
O1 O 0.1310(4) 0.51184(17) 0.7170(6) 0.0463(14) Uani 1 1 d . . . . .
N2 N 0.9758(3) 0.60600(19) 0.0040(6) 0.0262(14) Uani 1 1 d . . . . .
O3 O 1.0381(4) 0.54606(16) -0.0949(6) 0.0470(15) Uani 1 1 d . . . . .
H3 H 1.0712 0.5400 -0.1634 0.071 Uiso 1 1 calc R U . . .
C4 C 1.0301(5) 0.5880(2) -0.0849(8) 0.0305(17) Uani 1 1 d . . . . .
H4 H 1.0649 0.6061 -0.1443 0.037 Uiso 1 1 calc R U . . .
N5 N 0.1489(4) 0.4966(2) 0.4757(7) 0.0386(16) Uani 1 1 d . . . . .
C6 C 0.1133(5) 0.5183(2) 0.5864(11) 0.044(2) Uani 1 1 d . . . . .
H6 H 0.0718 0.5401 0.5646 0.053 Uiso 1 1 calc R U . . .
C7 C 0.9676(5) 0.6545(2) 0.0165(10) 0.055(3) Uani 1 1 d . . . . .
H7A H 1.0089 0.6686 -0.0487 0.082 Uiso 1 1 calc R U . . .
H7B H 0.9796 0.6634 0.1160 0.082 Uiso 1 1 calc R U . . .
H7C H 0.9088 0.6633 -0.0098 0.082 Uiso 1 1 calc R U . . .
C8 C 0.9202(5) 0.5790(3) 0.1018(8) 0.050(2) Uani 1 1 d . . . . .
H8A H 0.9241 0.5483 0.0736 0.075 Uiso 1 1 calc R U . . .
H8B H 0.8601 0.5888 0.0942 0.075 Uiso 1 1 calc R U . . .
H8C H 0.9400 0.5824 0.2016 0.075 Uiso 1 1 calc R U . . .
C9 C 0.2145(5) 0.4626(3) 0.5039(9) 0.053(2) Uani 1 1 d . . . . .
H9A H 0.2718 0.4738 0.4792 0.080 Uiso 1 1 calc R U . . .
H9B H 0.2019 0.4368 0.4448 0.080 Uiso 1 1 calc R U . . .
H9C H 0.2131 0.4545 0.6062 0.080 Uiso 1 1 calc R U . . .
C10B C 0.1267(7) 0.5044(4) 0.3231(9) 0.083(4) Uani 1.00(2) 1 d . . P C 2
H10A H 0.1054 0.4772 0.2800 0.124 Uiso 1.00(2) 1 calc R U P C 2
H10B H 0.1782 0.5142 0.2709 0.124 Uiso 1.00(2) 1 calc R U P C 2
H10C H 0.0819 0.5269 0.3170 0.124 Uiso 1.00(2) 1 calc R U P C 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
I4 Sb3 3.1292(7) . ?
I4 Sb3 3.1293(7) 8_575 ?
I5 Sb3 3.1329(7) . ?
I5 Sb3 3.1329(7) 8_575 ?
Sb3 I1 2.905(4) . ?
Sb3 I3 2.9165(7) . ?
Sb3 I2 2.9321(7) . ?
Sb3 I6 3.2306(7) . ?
I6 Sb3 3.2306(7) 8_575 ?
O1 C6 1.231(9) . ?
N2 C4 1.275(8) . ?
N2 C7 1.466(9) . ?
N2 C8 1.468(9) . ?
O3 C4 1.266(8) . ?
N5 C6 1.314(10) . ?
N5 C10B 1.445(10) . ?
N5 C9 1.449(9) . ?

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
Sb3 I4 Sb3 80.92(2) . 8_575 ?
Sb3 I5 Sb3 80.80(2) . 8_575 ?
I1 Sb3 I3 95.71(14) . . ?
I1 Sb3 I2 98.1(2) . . ?
I3 Sb3 I2 93.53(2) . . ?
I1 Sb3 I4 88.77(15) . . ?
I3 Sb3 I4 173.40(2) . . ?
I2 Sb3 I4 90.612(19) . . ?
I1 Sb3 I5 87.6(2) . . ?
I3 Sb3 I5 90.607(19) . . ?
I2 Sb3 I5 172.52(2) . . ?
I4 Sb3 I5 84.735(18) . . ?
I1 Sb3 I6 167.1(2) . . ?
I3 Sb3 I6 91.53(2) . . ?
I2 Sb3 I6 92.05(2) . . ?
I4 Sb3 I6 83.179(19) . . ?
I5 Sb3 I6 81.604(19) . . ?
Sb3 I6 Sb3 77.89(2) . 8_575 ?
C4 N2 C7 121.7(7) . . ?
C4 N2 C8 121.4(6) . . ?
C7 N2 C8 116.9(6) . . ?
O3 C4 N2 121.9(7) . . ?
C6 N5 C10B 124.0(8) . . ?
C6 N5 C9 119.8(7) . . ?
C10B N5 C9 116.2(7) . . ?
O1 C6 N5 124.7(7) . . ?

_refine_diff_density_max         1.167
_refine_diff_density_min         -2.052
_refine_diff_density_rms         0.174

####################################################################### 
# 
# 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_a2_a_sqd
_database_code_depnum_ccdc_archive 'CCDC 1910948'
loop_
_audit_author_name
_audit_author_address
'Shiv Pal'
;Indian Institute of Science Education and Research, Pune , India
India
;
_audit_update_record             
;
2019-04-18 deposited with the CCDC.	2019-06-03 downloaded from the CCDC.
;

#============================================================================
# start Validation Reply Form
#============================================================================
_vrf_PLAT990_a2_a_sqd            
;
PROBLEM:Deprecated .res/.hkl Input Style SQUEEZE Job
RESPONSE:There is a highly disordered solvent molecule which could not be 
properly solved and so it was removed by using  SQUEEZE Job.
The SQUEEZE details are given in CIF.
;
#============================================================================
# End Validation Reply Form
#============================================================================

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H38 I9 N4 O4 Sb2'
_chemical_formula_sum            'C16 H38 I9 N4 O4 Sb2'
_chemical_formula_weight         1736.10

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'
I I -0.4742 1.8119 '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'
Sb Sb -0.5866 1.5461 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   15.6538(5)
_cell_length_b                   28.4872(10)
_cell_length_c                   10.8182(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4824.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9891
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      27.38

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.390
_exptl_crystal_F_000             3092
_exptl_transmission_factor_min   0.5173
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.016
_exptl_absorpt_coefficient_mu    6.901
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'Krause, L., Herbst-Irmer,R.,SheldrickG.M. &StalkeD.,J.Appl.Cryst.48(2015)3-10'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70909
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.288
_diffrn_reflns_theta_max         28.329
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6124
_reflns_number_gt                4284
_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'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0354P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6124
_refine_ls_number_parameters     174
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0774
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001

# SQUEEZE RESULTS (Version = 121217)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.226 0.250 0.038 205 59 ' '
2 0.774 0.750 -0.038 206 59 ' '
3 0.726 0.250 0.462 205 59 ' '
4 0.935 0.521 0.167 8 0 ' '
5 0.935 0.979 0.167 9 0 ' '
6 0.435 0.521 0.333 8 0 ' '
7 0.274 0.750 0.538 206 59 ' '
8 0.435 0.979 0.333 8 0 ' '
9 0.565 0.021 0.667 8 0 ' '
10 0.565 0.479 0.667 8 0 ' '
11 0.065 0.021 0.833 8 0 ' '
12 0.065 0.479 0.833 8 0 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 2 0 1.430
0 1 1 2.014
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL A2_a.res in Pnma
CELL   15.6538   28.4872   10.8182     90.00     90.00     90.00
SPGR Pnma
# Solvent Accessible Volume =       879
# Electrons Found in S.A.V. =       234
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.787 0.748 0.000 !      11.28 eA-3
C102 0.294 0.249 0.203 !       6.22 eA-3
C103 0.296 0.679 0.597 !       6.11 eA-3
C104 0.259 0.725 0.605 !       4.71 eA-3
C105 0.851 0.751 0.094 !       4.44 eA-3
C106 0.739 0.304 0.493 !       4.00 eA-3
C107 0.277 0.249 0.000 !       2.39 eA-3
Q108 0.749 0.750 0.234 !       2.37 eA-3
Q109 0.516 0.753 0.000 !       2.13 eA-3
Q110 0.952 0.750 0.297 !       2.01 eA-3
Q111 0.375 0.748 0.937 !       1.88 eA-3
Q112 0.810 0.250 0.781 !       1.86 eA-3
Q113 0.296 0.248 0.344 !       1.81 eA-3
Q114 0.096 0.681 0.312 !       1.78 eA-3
Q115 0.189 0.016 0.012 !       1.76 eA-3
Q116 0.621 0.235 0.764 !       1.74 eA-3
Q117 0.699 0.610 0.654 !       1.72 eA-3
Q118 0.198 0.248 0.406 !       1.70 eA-3
C119 0.159 0.735 0.679 !       1.64 eA-3
Q120 0.297 0.352 0.615 !       1.64 eA-3
Q121 0.273 0.187 0.120 !       1.62 eA-3
Q122 0.832 0.751 0.188 !       1.62 eA-3
Q123 0.484 0.677 0.533 !       1.57 eA-3
Q124 0.266 0.335 0.329 !       1.56 eA-3
Q125 0.485 0.237 0.059 !       1.55 eA-3
Q126 0.501 0.323 0.564 !       1.55 eA-3
Q127 0.843 0.751 0.328 !       1.54 eA-3
Q128 0.566 0.437 0.414 !       1.54 eA-3
C129 0.261 0.680 0.390 !       1.53 eA-3
Q130 0.372 0.202 0.154 !       1.53 eA-3
Q131 0.621 0.436 0.456 !       1.52 eA-3
Q132 0.377 0.024 0.120 !       1.52 eA-3
Q133 0.046 0.737 0.623 !       1.52 eA-3
Q134 0.323 0.749 0.672 !       1.52 eA-3
Q135 0.530 0.210 0.154 !       1.51 eA-3
Q136 0.119 0.234 0.202 !       1.49 eA-3
Q137 0.888 0.555 0.721 !       1.49 eA-3
Q138 0.611 0.632 0.471 !       1.49 eA-3
Q139 0.676 0.800 0.190 !       1.49 eA-3
Q140 0.062 0.062-0.002 !       1.49 eA-3
C141 0.220 0.709 0.709 !       1.49 eA-3
Q142 0.158 0.639 0.390 !       1.47 eA-3
Q143 0.926 0.805 0.941 !       1.47 eA-3
Q144 0.275 0.950 0.099 !       1.47 eA-3
Q145 0.572 0.134 0.968 !       1.44 eA-3
Q146 0.207 0.062 0.974 !       1.44 eA-3
C147 0.693 0.283 0.529 !       1.44 eA-3
C148 0.629 0.300 0.534 !       1.43 eA-3
Q149 0.745 0.672 0.377 !       1.43 eA-3
Q150 0.719 0.252 0.672 !       1.42 eA-3
Q151 0.755 0.914 0.908 !       1.41 eA-3
Q152 0.398 0.749 0.156 !       1.41 eA-3
Q153 0.582 0.877 0.253 !       1.41 eA-3
Q154 0.391 0.948 0.076 !       1.40 eA-3
Q155 0.869 0.151 0.044 !       1.40 eA-3
Q156 0.294 0.813 0.970 !       1.39 eA-3
Q157 0.744 0.343 0.408 !       1.38 eA-3
Q158 0.065 0.169 0.988 !       1.37 eA-3
Q159 0.375 0.752 0.016 !       1.37 eA-3
Q160 0.917 0.751 0.516 !       1.37 eA-3
Q161 0.120 0.251 0.109 !       1.35 eA-3
Q162 0.593 0.120 0.125 !       1.35 eA-3
Q163 0.579 0.594 0.612 !       1.35 eA-3
Q164 0.668 0.025 0.156 !       1.35 eA-3
Q165 0.298 0.335 0.706 !       1.34 eA-3
Q166 0.486 0.219 0.219 !       1.34 eA-3
Q167 0.036 0.837 0.051 !       1.33 eA-3
Q168 0.112 0.931 0.051 !       1.33 eA-3
Q169 0.241 0.561 0.455 !       1.33 eA-3
Q170 0.437 0.311 0.560 !       1.33 eA-3
Q171 0.597 0.249 0.484 !       1.32 eA-3
Q172 0.699 0.297 0.701 !       1.32 eA-3
Q173 0.794 0.750 0.547 !       1.32 eA-3
C174 0.551 0.250 0.562 !       1.32 eA-3
C175 0.780 0.807 0.093 !       1.31 eA-3
Q176 0.993 0.662 0.987 !       1.31 eA-3
Q177 0.539 0.749 0.328 !       1.31 eA-3
Q178 0.108 0.662 0.391 !       1.31 eA-3
Q179 0.755 0.820 0.214 !       1.31 eA-3
Q180 0.651 0.471 0.537 !       1.30 eA-3
Q181 0.256 0.525 0.316 !       1.30 eA-3
Q182 0.097 0.202 0.878 !       1.30 eA-3
Q183 0.029 0.573 0.309 !       1.30 eA-3
Q184 0.237 0.640 0.268 !       1.30 eA-3
C185 0.622 0.269 0.678 !       1.30 eA-3
Q186 1.005 0.641 0.300 !       1.29 eA-3
Q187 0.860 0.601 0.756 !       1.29 eA-3
Q188 0.204 0.423 0.510 !       1.29 eA-3
Q189 0.981 0.335 0.387 !       1.29 eA-3
Q190 0.344 0.108 0.910 !       1.29 eA-3
Q191 0.378 0.213 0.069 !       1.29 eA-3
Q192 0.175 0.936 0.227 !       1.29 eA-3
C193 0.651 0.275 0.474 !       1.29 eA-3
Q194 0.507 0.293 0.643 !       1.29 eA-3
Q195 0.810 0.650 0.486 !       1.29 eA-3
Q196 0.080 0.834 0.891 !       1.28 eA-3
Q197 0.159 0.071 0.219 !       1.28 eA-3
Q198 0.420 0.662 0.562 !       1.28 eA-3
Q199 0.987 0.882 0.928 !       1.28 eA-3
;

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
I5 I 0.44932(3) 0.7500 0.77962(5) 0.02505(13) Uani 1 2 d S T P A 1
Sb1 Sb 0.42031(2) 0.82209(2) 1.00236(4) 0.02290(10) Uani 1 1 d . . . A 1
I6 I 0.27147(3) 0.7500 1.06619(5) 0.02787(14) Uani 1 2 d S T P A 1
I4 I 0.53609(4) 0.7500 1.14296(6) 0.03186(15) Uani 1 2 d S T P A 1
I3 I 0.39836(3) 0.87527(2) 1.22623(4) 0.03257(11) Uani 1 1 d . . . A 1
I1 I 0.29803(3) 0.88050(2) 0.85774(4) 0.03513(12) Uani 1 1 d . . . A 1
I2 I 0.56707(3) 0.87675(2) 0.93024(4) 0.03806(12) Uani 1 1 d . . . A 1
O2 O 0.6985(3) 0.54541(16) 0.2084(4) 0.0420(12) Uani 1 1 d . . . B 1
O1 O 0.6133(3) 0.56022(16) 0.3911(4) 0.0418(12) Uani 1 1 d . . . C 1
N2 N 0.7024(3) 0.52018(18) 0.0131(5) 0.0341(13) Uani 1 1 d . . . B 1
N1 N 0.5558(4) 0.6138(2) 0.5136(5) 0.0458(15) Uani 1 1 d . . . C 1
C3 C 0.6011(4) 0.6040(2) 0.4158(6) 0.0368(16) Uani 1 1 d . . . C 1
C7 C 0.6620(4) 0.5241(2) 0.1181(6) 0.0306(15) Uani 1 1 d . . . B 1
C4 C 0.6380(4) 0.6406(2) 0.3348(7) 0.0454(18) Uani 1 1 d . . . . .
H4A H 0.6771 0.6596 0.3817 0.068 Uiso 1 1 calc R U . C 1
H4B H 0.5931 0.6600 0.3028 0.068 Uiso 1 1 calc R U . C 1
H4C H 0.6679 0.6260 0.2676 0.068 Uiso 1 1 calc R U . C 1
C8 C 0.5746(4) 0.5043(2) 0.1373(6) 0.0403(17) Uani 1 1 d . . . . .
H8A H 0.5746 0.4716 0.1161 0.060 Uiso 1 1 calc R U . B 1
H8B H 0.5346 0.5207 0.0857 0.060 Uiso 1 1 calc R U . B 1
H8C H 0.5585 0.5079 0.2223 0.060 Uiso 1 1 calc R U . B 1
C6 C 0.7859(4) 0.5426(3) -0.0044(7) 0.052(2) Uani 1 1 d . . . . .
H6A H 0.7955 0.5650 0.0605 0.077 Uiso 1 1 calc R U . B 1
H6B H 0.7870 0.5583 -0.0828 0.077 Uiso 1 1 calc R U . B 1
H6C H 0.8299 0.5191 -0.0024 0.077 Uiso 1 1 calc R U . B 1
C5 C 0.6652(5) 0.4968(3) -0.0931(7) 0.057(2) Uani 1 1 d . . . . .
H5A H 0.6105 0.4841 -0.0709 0.085 Uiso 1 1 calc R U . B 1
H5B H 0.7022 0.4719 -0.1196 0.085 Uiso 1 1 calc R U . B 1
H5C H 0.6582 0.5190 -0.1591 0.085 Uiso 1 1 calc R U . B 1
C2 C 0.5387(6) 0.6617(3) 0.5524(9) 0.078(3) Uani 1 1 d . . . . .
H2A H 0.5917 0.6780 0.5637 0.117 Uiso 1 1 calc R U . C 1
H2B H 0.5076 0.6613 0.6288 0.117 Uiso 1 1 calc R U . C 1
H2C H 0.5054 0.6773 0.4902 0.117 Uiso 1 1 calc R U . C 1
C1 C 0.5193(6) 0.5751(3) 0.5881(8) 0.080(3) Uani 1 1 d . . . . .
H1A H 0.4973 0.5513 0.5341 0.120 Uiso 1 1 calc R U . C 1
H1B H 0.4740 0.5871 0.6389 0.120 Uiso 1 1 calc R U . C 1
H1C H 0.5630 0.5619 0.6397 0.120 Uiso 1 1 calc R U . C 1
H1 H 0.657(7) 0.550(3) 0.334(10) 0.12(4) 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
I5 Sb1 3.1984(6) . ?
I5 Sb1 3.1984(6) 7_575 ?
Sb1 I3 2.8772(5) . ?
Sb1 I2 2.8830(5) . ?
Sb1 I1 2.9801(6) . ?
Sb1 I4 3.1330(6) . ?
Sb1 I6 3.1816(6) . ?
I6 Sb1 3.1816(6) 7_575 ?
I4 Sb1 3.1330(6) 7_575 ?
O2 C7 1.284(7) . ?
O1 C3 1.289(7) . ?
O1 H1 0.96(11) . ?
N2 C7 1.305(8) . ?
N2 C5 1.450(8) . ?
N2 C6 1.467(8) . ?
N1 C3 1.303(8) . ?
N1 C2 1.452(10) . ?
N1 C1 1.479(10) . ?
C3 C4 1.481(9) . ?
C7 C8 1.494(9) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?

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
Sb1 I5 Sb1 79.895(18) . 7_575 ?
I3 Sb1 I2 92.209(17) . . ?
I3 Sb1 I1 94.083(16) . . ?
I2 Sb1 I1 93.909(17) . . ?
I3 Sb1 I4 90.317(16) . . ?
I2 Sb1 I4 91.402(17) . . ?
I1 Sb1 I4 172.964(17) . . ?
I3 Sb1 I6 93.997(17) . . ?
I2 Sb1 I6 172.280(18) . . ?
I1 Sb1 I6 90.229(16) . . ?
I4 Sb1 I6 83.982(15) . . ?
I3 Sb1 I5 171.557(18) . . ?
I2 Sb1 I5 91.708(16) . . ?
I1 Sb1 I5 93.108(16) . . ?
I4 Sb1 I5 82.112(15) . . ?
I6 Sb1 I5 81.550(15) . . ?
Sb1 I6 Sb1 80.401(18) . 7_575 ?
Sb1 I4 Sb1 81.912(19) 7_575 . ?
C3 O1 H1 122(6) . . ?
C7 N2 C5 122.3(6) . . ?
C7 N2 C6 120.5(6) . . ?
C5 N2 C6 117.1(6) . . ?
C3 N1 C2 122.4(7) . . ?
C3 N1 C1 119.5(6) . . ?
C2 N1 C1 118.0(7) . . ?
O1 C3 N1 117.1(6) . . ?
O1 C3 C4 120.1(6) . . ?
N1 C3 C4 122.8(6) . . ?
O2 C7 N2 119.1(6) . . ?
O2 C7 C8 118.7(6) . . ?
N2 C7 C8 122.2(6) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

_refine_diff_density_max         0.851
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.196

