 
data_PDMAI2
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety         'C8 H14 N2, 2(I)'
_chemical_formula_sum
 'C8 H14 I2 N2' 
_chemical_formula_weight          392.01

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'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    4.534(4)
_cell_length_b                    6.307(6)
_cell_length_c                    10.575(9)
_cell_angle_alpha                 102.06(3)
_cell_angle_beta                  101.10(3)
_cell_angle_gamma                 95.60(3)
_cell_volume                      287.2(4)
_cell_formula_units_Z             1
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used   1435
_cell_measurement_theta_min     3.47
_cell_measurement_theta_max     36.16
 
_exptl_crystal_description        block
_exptl_crystal_colour             yellow
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.267          
_exptl_crystal_F_000              182
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.480
_exptl_crystal_size_mid           0.290
_exptl_crystal_size_min           0.250
_exptl_absorpt_coefficient_mu     5.432
_shelx_estimated_absorpt_T_min    0.180
_shelx_estimated_absorpt_T_max    0.344
_exptl_absorpt_correction_T_min   0.237
_exptl_absorpt_correction_T_max   0.398
_exptl_absorpt_correction_type            analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'KM4 diffractometer with Sappire CCD detector'
_diffrn_measurement_method        ω
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             2136
_diffrn_reflns_av_unetI/netI      0.0709
_diffrn_reflns_av_R_equivalents   0.0673
_diffrn_reflns_limit_h_min        -5
_diffrn_reflns_limit_h_max        5
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.338
_diffrn_reflns_theta_max          25.992
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.992
_diffrn_measured_fraction_theta_full  0.992
_diffrn_reflns_Laue_measured_fraction_max    0.992
_diffrn_reflns_Laue_measured_fraction_full   0.992
_diffrn_reflns_point_group_measured_fraction_max   0.992
_diffrn_reflns_point_group_measured_fraction_full  0.992
_reflns_number_total              1114
_reflns_number_gt                 1050
_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     'CrysAlis CCD 1.171.13(Oxford Diffraction ,2003)'
_computing_cell_refinement     'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction      'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution   'SHELXS (Sheldrick, 2018)'
_computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   'SHELXL-2018/1 (Sheldrick, 2018)'
_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)+(0.1129P)²] 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          1114
_refine_ls_number_parameters      56
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0643
_refine_ls_R_factor_gt            0.0619
_refine_ls_wR_factor_ref          0.1645
_refine_ls_wR_factor_gt           0.1580
_refine_ls_goodness_of_fit_ref    1.118
_refine_ls_restrained_S_all       1.118
_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
I1 I 0.87077(10) 0.19843(7) 0.36304(4) 0.0209(3) Uani 1 1 d . . . . .
N1 N 0.5296(18) 0.3234(12) 0.6456(7) 0.0230(15) Uani 1 1 d . . . . .
H1A H 0.622517 0.295187 0.576169 0.028 Uiso 1 1 calc R U . . .
H1B H 0.454076 0.452392 0.648573 0.028 Uiso 1 1 calc R U . . .
H1C H 0.375101 0.213327 0.635317 0.028 Uiso 1 1 calc R U . . .
C1 C 0.6217(18) 0.4215(14) 0.8903(8) 0.0178(16) Uani 1 1 d . . . . .
C4 C 0.7536(19) 0.3384(15) 0.7713(9) 0.0219(18) Uani 1 1 d . . . . .
H4A H 0.938456 0.438884 0.774751 0.026 Uiso 1 1 calc R U . . .
H4B H 0.812576 0.192078 0.773882 0.026 Uiso 1 1 calc R U . . .
C3 C 0.514(2) 0.7242(13) 1.0476(8) 0.0223(18) Uani 1 1 d . . . . .
H3 H 0.520209 0.877477 1.078909 0.027 Uiso 1 1 calc R U . . .
C2 C 0.640(2) 0.6465(14) 0.9407(9) 0.0247(19) Uani 1 1 d . . . . .
H2 H 0.739353 0.746821 0.901452 0.030 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
N1 C4 1.489(11) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C1 C2 1.396(12) . ?
C1 C3 1.398(12) 2_667 ?
C1 C4 1.513(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C3 C2 1.383(12) . ?
C3 H3 0.9500 . ?
C2 H2 0.9500 . ?
 
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
C4 N1 H1A 109.5 . . ?
C4 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C4 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 C1 C3 119.2(8) . 2_667 ?
C2 C1 C4 119.9(7) . . ?
C3 C1 C4 120.9(8) 2_667 . ?
N1 C4 C1 110.9(7) . . ?
N1 C4 H4A 109.5 . . ?
C1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
C2 C3 C1 120.4(8) . 2_667 ?
C2 C3 H3 119.8 . . ?
C1 C3 H3 119.8 2_667 . ?
C3 C2 C1 120.4(8) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
 _geom_hbond_publ_flag
N1 H1A I1  0.91 2.69 3.603(8) 177.0 . yes
N1 H1B I1  0.91 2.78 3.677(8) 170.2 2_666 yes
N1 H1C I1  0.91 2.73 3.575(8) 155.0 2_656 yes
 
_refine_diff_density_max    1.829
_refine_diff_density_min   -3.062
_refine_diff_density_rms    0.395



