data_mo_njz_hexdiaminesn3_0m
_audit_creation_date               2018-02-01
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.01.22 svn.r3481 for OlexSys, GUI svn.r5457)
;
_shelx_SHELXL_version_number       '2014/7'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety          
 '0.5(Br6 Sn), Br, 1.5(C6 H18 N2), 0.13(C4 H8 Cl4)'
_chemical_formula_sum              'C9.50 H28 Br4 Cl0.50 N3 Sn0.50'
_chemical_formula_weight           581.06
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Br' 'Br' -0.2901 2.4595
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl' 'Cl' 0.1484 0.1585 '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'
 'Sn' 'Sn' -0.6537 1.4246
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             12
_space_group_name_H-M_alt          'C 1 2/m 1'
_space_group_name_Hall             '-C 2y'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, -y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z'

_cell_length_a                     9.7441(7)
_cell_length_b                     17.8506(13)
_cell_length_c                     11.6010(10)
_cell_angle_alpha                  90
_cell_angle_beta                   94.837(3)
_cell_angle_gamma                  90
_cell_volume                       2010.7(3)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      3260
_cell_measurement_temperature      150(2)
_cell_measurement_theta_max        26.15
_cell_measurement_theta_min        2.39
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      8.670
_exptl_absorpt_correction_T_max    0.7454
_exptl_absorpt_correction_T_min    0.4593
_exptl_absorpt_correction_type    
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1191 before and 0.0770 after correction.
The Ratio of minimum to maximum transmission is 0.6162.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              ?
_exptl_crystal_density_diffrn      1.919
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1118
_exptl_crystal_size_max            ?
_exptl_crystal_size_mid            ?
_exptl_crystal_size_min            ?
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0959
_diffrn_reflns_av_unetI/netI       0.0559
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.998
_diffrn_reflns_limit_h_max         12
_diffrn_reflns_limit_h_min         -12
_diffrn_reflns_limit_k_max         22
_diffrn_reflns_limit_k_min         -22
_diffrn_reflns_limit_l_max         14
_diffrn_reflns_limit_l_min         -14
_diffrn_reflns_number              13980
_diffrn_reflns_point_group_measured_fraction_full  0.999
_diffrn_reflns_point_group_measured_fraction_max  0.998
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           26.400
_diffrn_reflns_theta_min           2.282
_diffrn_ambient_temperature        150.0
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.998
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  1623
_reflns_number_total               2138
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection         ?
_computing_data_reduction          'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'XL (Sheldrick, 2008)'
_computing_structure_solution      'XT (Sheldrick, 2015)'
_refine_diff_density_max           1.615
_refine_diff_density_min           -0.864
_refine_diff_density_rms           0.230
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.063
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       113
_refine_ls_number_reflns           2138
_refine_ls_number_restraints       41
_refine_ls_R_factor_all            0.0770
_refine_ls_R_factor_gt             0.0540
_refine_ls_restrained_S_all        1.070
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0925P)²+15.4623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1479
_refine_ls_wR_factor_ref           0.1605
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C5-C4
 1.49 with sigma of 0.01
 C5-C6
 1.49 with sigma of 0.01
 H6B-C6
 0.99 with sigma of 0.02
 H6A-C6
 0.99 with sigma of 0.02
 C4-N2
 1.47 with sigma of 0.01
 H6B-C5 \\sim H6B-C6_$1 \\sim H6A-C5 \\sim H6A-C6_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 Cl1, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl1(0.25) C7(0.25) H7A(0.25) H7B(0.25) H2C(0.5) H2D(0.5) H2E(0.5)
 C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C4(H4A,H4B), C5(H5A,H5B)
6.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Sn1 Sn 1.0000 0.5000 0.5000 0.0214(3) Uani 1 4 d S T P . .
 Br1 Br 0.73668(12) 0.5000 0.35939(12) 0.0338(4) Uani 1 2 d S T P . .
 Br2 Br 1.11100(8) 0.37969(5) 0.35153(8) 0.0336(3) Uani 1 1 d . . . . .
 Br3 Br 1.0000 0.16378(6) 0.5000 0.0245(3) Uani 1 2 d S T P . .
 N1 N 0.7963(7) 0.3045(4) 0.3683(6) 0.0261(15) Uani 1 1 d . . . . .
 H1A H 0.8712 0.3349 0.3674 0.031 Uiso 1 1 calc GR . . . .
 H1B H 0.8243 0.2569 0.3858 0.031 Uiso 1 1 calc GR . . . .
 H1C H 0.7412 0.3212 0.4224 0.031 Uiso 1 1 calc GR . . . .
 C1 C 0.7191(8) 0.3054(5) 0.2539(7) 0.0258(17) Uani 1 1 d . . . . .
 H1D H 0.7012 0.3579 0.2296 0.031 Uiso 1 1 calc R . . . .
 H1E H 0.6291 0.2803 0.2587 0.031 Uiso 1 1 calc R . . . .
 C2 C 0.7964(8) 0.2668(5) 0.1662(7) 0.0287(18) Uani 1 1 d . . . . .
 H2A H 0.8143 0.2142 0.1901 0.034 Uiso 1 1 calc R . . . .
 H2B H 0.8862 0.2919 0.1608 0.034 Uiso 1 1 calc R . . . .
 C3 C 0.7141(9) 0.2685(6) 0.0489(7) 0.036(2) Uani 1 1 d . . . . .
 H3A H 0.6940 0.3213 0.0277 0.044 Uiso 1 1 calc R . . . .
 H3B H 0.6250 0.2429 0.0557 0.044 Uiso 1 1 calc R . . . .
 Cl1 Cl 1.0000 0.4222(6) 0.0000 0.124(5) Uani 0.5 2 d S TU P . .
 C7 C 1.015(5) 0.5000 -0.054(4) 0.092(10) Uani 0.5 2 d S TU P . .
 H7A H 1.1083 0.5000 -0.0818 0.110 Uiso 0.5 2 calc RS T P . .
 H7B H 0.9498 0.5000 -0.1238 0.110 Uiso 0.5 2 calc RS T P . .
 N2 N 0.8851(9) 0.0000 0.3481(8) 0.024(2) Uani 1 2 d DS TU P . .
 H2C H 0.9628 -0.0266 0.3693 0.029 Uiso 0.5 1 calc GR . . A .
 H2D H 0.8108 -0.0311 0.3452 0.029 Uiso 0.5 1 calc GR . . . .
 H2E H 0.8747 0.0370 0.4007 0.029 Uiso 0.5 1 calc GR . . . .
 C4 C 0.8963(17) 0.0336(9) 0.2328(10) 0.038(4) Uani 0.5 1 d D U . A -1
 H4A H 0.9683 0.0728 0.2393 0.046 Uiso 0.5 1 calc R . . A -1
 H4B H 0.8078 0.0580 0.2069 0.046 Uiso 0.5 1 calc R . . A -1
 C5 C 0.931(2) -0.0221(9) 0.1442(13) 0.049(5) Uani 0.5 1 d D U . A -1
 H5A H 0.8527 -0.0569 0.1266 0.058 Uiso 0.5 1 calc R . . A -1
 H5B H 1.0126 -0.0517 0.1727 0.058 Uiso 0.5 1 calc R . . A -1
 C6 C 0.960(3) 0.0212(10) 0.0371(16) 0.073(8) Uani 0.5 1 d D U . A -1
 H6A H 0.872(7) 0.041(10) 0.000(5) 0.087 Uiso 0.5 1 d DR . . B -1
 H6B H 1.000(16) 0.070(5) 0.062(8) 0.087 Uiso 0.5 1 d DR . . C -1


_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
 Sn1 Br1 2.9220(12) . ?
 Sn1 Br1 2.9220(12) 5_766 ?
 Sn1 Br2 3.0104(9) . ?
 Sn1 Br2 3.0104(9) 2_756 ?
 Sn1 Br2 3.0104(9) 5_766 ?
 Sn1 Br2 3.0104(9) 6_565 ?
 N1 H1A 0.9100 . ?
 N1 H1B 0.9100 . ?
 N1 H1C 0.9100 . ?
 N1 C1 1.470(10) . ?
 C1 H1D 0.9900 . ?
 C1 H1E 0.9900 . ?
 C1 C2 1.485(11) . ?
 C2 H2A 0.9900 . ?
 C2 H2B 0.9900 . ?
 C2 C3 1.521(12) . ?
 C3 C3 1.532(17) 7_655 ?
 C3 H3A 0.9900 . ?
 C3 H3B 0.9900 . ?
 Cl1 C7 1.53(2) 2_755 ?
 Cl1 C7 1.53(2) . ?
 Cl1 C7 1.53(2) 5_765 ?
 C7 Cl1 1.53(2) 5_765 ?
 C7 H7A 0.9900 . ?
 C7 H7B 0.9900 . ?
 N2 H2C 0.9100 . ?
 N2 H2D 0.9100 . ?
 N2 H2E 0.9100 . ?
 N2 C4 1.478(9) . ?
 C4 H4A 0.9900 . ?
 C4 H4B 0.9900 . ?
 C4 C5 1.490(10) . ?
 C5 H5A 0.9900 . ?
 C5 H5B 0.9900 . ?
 C5 C6 1.511(10) . ?
 C6 C6 1.43(4) 5_755 ?
 C6 H6A 0.99(2) . ?
 C6 H6B 0.99(2) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 Br1 Sn1 Br1 180.0 . 5_766 ?
 Br1 Sn1 Br2 88.77(3) 5_766 6_565 ?
 Br1 Sn1 Br2 91.23(3) . . ?
 Br1 Sn1 Br2 88.77(3) . 5_766 ?
 Br1 Sn1 Br2 88.77(3) . 2_756 ?
 Br1 Sn1 Br2 91.23(3) 5_766 5_766 ?
 Br1 Sn1 Br2 88.77(3) 5_766 . ?
 Br1 Sn1 Br2 91.23(3) . 6_565 ?
 Br1 Sn1 Br2 91.23(3) 5_766 2_756 ?
 Br2 Sn1 Br2 180.00(2) 6_565 2_756 ?
 Br2 Sn1 Br2 91.02(4) 6_565 . ?
 Br2 Sn1 Br2 180.00(2) 5_766 . ?
 Br2 Sn1 Br2 88.98(4) 5_766 6_565 ?
 Br2 Sn1 Br2 91.02(4) 5_766 2_756 ?
 Br2 Sn1 Br2 88.98(4) 2_756 . ?
 H1A N1 H1B 109.5 . . ?
 H1A N1 H1C 109.5 . . ?
 H1B N1 H1C 109.5 . . ?
 C1 N1 H1A 109.5 . . ?
 C1 N1 H1B 109.5 . . ?
 C1 N1 H1C 109.5 . . ?
 N1 C1 H1D 109.4 . . ?
 N1 C1 H1E 109.4 . . ?
 N1 C1 C2 111.3(6) . . ?
 H1D C1 H1E 108.0 . . ?
 C2 C1 H1D 109.4 . . ?
 C2 C1 H1E 109.4 . . ?
 C1 C2 H2A 109.6 . . ?
 C1 C2 H2B 109.6 . . ?
 C1 C2 C3 110.1(7) . . ?
 H2A C2 H2B 108.1 . . ?
 C3 C2 H2A 109.6 . . ?
 C3 C2 H2B 109.6 . . ?
 C2 C3 C3 114.6(9) . 7_655 ?
 C2 C3 H3A 108.6 . . ?
 C2 C3 H3B 108.6 . . ?
 C3 C3 H3A 108.6 7_655 . ?
 C3 C3 H3B 108.6 7_655 . ?
 H3A C3 H3B 107.6 . . ?
 C7 Cl1 C7 0(5) 2_755 5_765 ?
 C7 Cl1 C7 50(3) 2_755 . ?
 C7 Cl1 C7 50(3) 5_765 . ?
 Cl1 C7 Cl1 130(3) 5_765 . ?
 Cl1 C7 H7A 104.8 . . ?
 Cl1 C7 H7A 104.8 5_765 . ?
 Cl1 C7 H7B 104.8 5_765 . ?
 Cl1 C7 H7B 104.8 . . ?
 H7A C7 H7B 105.8 . . ?
 H2C N2 H2D 109.5 . . ?
 H2C N2 H2E 109.5 . . ?
 H2D N2 H2E 109.5 . . ?
 C4 N2 H2C 109.5 . . ?
 C4 N2 H2D 109.5 . . ?
 C4 N2 H2E 109.5 . . ?
 N2 C4 H4A 109.0 . . ?
 N2 C4 H4B 109.0 . . ?
 N2 C4 C5 113.1(11) . . ?
 H4A C4 H4B 107.8 . . ?
 C5 C4 H4A 109.0 . . ?
 C5 C4 H4B 109.0 . . ?
 C4 C5 H5A 110.3 . . ?
 C4 C5 H5B 110.3 . . ?
 C4 C5 C6 107.1(12) . . ?
 H5A C5 H5B 108.5 . . ?
 C6 C5 H5A 110.3 . . ?
 C6 C5 H5B 110.3 . . ?
 C5 C6 H6A 109(5) . . ?
 C5 C6 H6B 108(5) . . ?
 C6 C6 C5 111.9(18) 5_755 . ?
 C6 C6 H6A 115(5) 5_755 . ?
 C6 C6 H6B 115(5) 5_755 . ?
 H6A C6 H6B 97(10) . . ?


_olex2_submission_special_instructions  'No special instructions were received'
