data_mo_snetoh3_0m
_audit_creation_date              2018-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number            2013-2
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_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. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety          'Br4 Sn, 4(Br), 3(C6 H18 N2), 0.13(H16 O8)'
_chemical_formula_sum             'C18 H51.74 Br8 N6 O Sn'
_chemical_formula_weight          1126.36
_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'
 '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'
 '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            15
_space_group_name_H-M_alt         'C 1 2/c 1'
_space_group_name_Hall            '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                    9.9725(12)
_cell_length_b                    17.532(2)
_cell_length_c                    22.757(3)
_cell_angle_alpha                 90
_cell_angle_beta                  92.739(4)
_cell_angle_gamma                 90
_cell_volume                      3974.2(9)
_cell_formula_units_Z             4
_cell_measurement_reflns_used     5843
_cell_measurement_temperature     150(2)
_cell_measurement_theta_max       25.83
_cell_measurement_theta_min       2.35
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     8.706
_exptl_absorpt_correction_T_max   0.7454
_exptl_absorpt_correction_T_min   0.5380
_exptl_absorpt_correction_type    none
_exptl_absorpt_process_details    ?
_exptl_crystal_colour             ?
_exptl_crystal_density_diffrn     1.882
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_description        block
_exptl_crystal_F_000              2159
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_special_details
;
 ?
;
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0845
_diffrn_reflns_av_unetI/netI      0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_number             21954
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full         25.242
_diffrn_reflns_theta_max          26.592
_diffrn_reflns_theta_min          2.323
_diffrn_ambient_temperature       150.01
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_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                 2578
_reflns_number_total              4125
_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   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max          1.812
_refine_diff_density_min          -0.897
_refine_diff_density_rms          0.190
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.032
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      209
_refine_ls_number_reflns          4125
_refine_ls_number_restraints      230
_refine_ls_R_factor_all           0.1153
_refine_ls_R_factor_gt            0.0640
_refine_ls_restrained_S_all       1.020
_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)+(0.0936P)²+29.9148P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1609
_refine_ls_wR_factor_ref          0.1871
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N2-C5
 2.5 with sigma of 0.02
 C6-C4
 2.5 with sigma of 0.02
 C7-C9
 2.5 with sigma of 0.02
 C9-C9_$1
 1.5 with sigma of 0.01
 N4-C10 = C11-C10 = C12-C11
 1.45 with sigma of 0.01
 C11-N4
 2.5 with sigma of 0.02
 C12-C10
 2.5 with sigma of 0.02
 N3-C7 = C8-C7 = C9-C8 = N2-C4 = C5-C4 = C5-C6
 1.45 with sigma of 0.02
 C8-N3
 2.5 with sigma of 0.02
 N3-C7 = N4-C10
 1.48 with sigma of 0.0001
 C7-C8
 1.5 with sigma of 0.02
 C6_$2-C6_$3
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N3 \\sim C7 \\sim C8 \\sim C9 \\sim C12 \\sim C11 \\sim C10 \\sim N4: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N3, C7, C8, C9, C12, C11, C10, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(N4)=Sof(H4C)=Sof(H4D)=Sof(H4E)=1-FVAR(1)
 Sof(N3)=Sof(H3C)=Sof(H3D)=Sof(H3E)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=
 Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(1)
 Fixed Sof: O1(0.25) H1F(0.25) H1G(0.25) O2(0.25) H2F(0.25) H2G(0.25)
7.a Riding coordinates:
 N3(H3C,H3D,H3E), O1(H1F,H1G), O2(H2F,H2G)
7.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C1(H1D,H1E), C2(H2A,H2B), C3(H3A,H3B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C11(H11A,H11B),
 C10(H10A,H10B)
7.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E), N4(H4C,H4D,H4E)
;
_atom_sites_solution_hydrogens    mixed
_atom_sites_solution_primary      heavy
_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 0.0000 0.52410(5) 0.2500 0.0359(3) Uani 1 2 d S T P . .
 Br2 Br 0.0000 0.18771(7) 0.2500 0.0427(4) Uani 1 2 d S T P . .
 Br3 Br -0.5000 0.35585(7) 0.2500 0.0402(4) Uani 1 2 d S T P . .
 Br4 Br 0.11212(10) 0.64217(6) 0.17978(5) 0.0494(3) Uani 1 1 d . . . . .
 Br5 Br -0.25460(10) 0.52393(6) 0.17774(5) 0.0500(3) Uani 1 1 d . . . . .
 Br6 Br 0.11850(10) 0.39785(6) 0.17088(5) 0.0521(3) Uani 1 1 d . . . . .
 N1 N -0.1952(8) 0.3281(5) 0.1818(3) 0.0402(19) Uani 1 1 d . . . . .
 H1A H -0.1110 0.3442 0.1766 0.048 Uiso 1 1 calc GR . . . .
 H1B H -0.1927 0.2814 0.1983 0.048 Uiso 1 1 calc GR . . . .
 H1C H -0.2364 0.3607 0.2055 0.048 Uiso 1 1 calc GR . . . .
 N2 N -0.1156(9) 0.0204(5) 0.1798(4) 0.049(2) Uani 1 1 d D U . . .
 H2C H -0.1852 -0.0123 0.1792 0.058 Uiso 1 1 calc GR . . . .
 H2D H -0.1325 0.0599 0.2035 0.058 Uiso 1 1 calc GR . . . .
 H2E H -0.0407 -0.0038 0.1933 0.058 Uiso 1 1 calc GR . . . .
 C4 C -0.0968(12) 0.0484(7) 0.1202(5) 0.068(3) Uani 1 1 d D U . . .
 H4A H -0.0233 0.0856 0.1215 0.082 Uiso 1 1 calc R . . . .
 H4B H -0.1786 0.0751 0.1061 0.082 Uiso 1 1 calc R . . . .
 C5 C -0.0666(13) -0.0121(7) 0.0778(5) 0.069(3) Uani 1 1 d D U . . .
 H5A H -0.1455 -0.0446 0.0706 0.083 Uiso 1 1 calc R . . . .
 H5B H 0.0073 -0.0439 0.0938 0.083 Uiso 1 1 calc R . . . .
 C6 C -0.0277(17) 0.0245(7) 0.0212(5) 0.096(5) Uani 1 1 d D U . . .
 H6A H -0.1076 0.0489 0.0029 0.116 Uiso 1 1 calc R . . . .
 H6B H 0.0377 0.0648 0.0308 0.116 Uiso 1 1 calc R . . . .
 C1 C -0.2698(10) 0.3244(6) 0.1245(5) 0.050(3) Uani 1 1 d . . . . .
 H1D H -0.2846 0.3763 0.1094 0.060 Uiso 1 1 calc R . . . .
 H1E H -0.3578 0.3011 0.1296 0.060 Uiso 1 1 calc R . . . .
 C2 C -0.1956(11) 0.2791(6) 0.0809(5) 0.055(3) Uani 1 1 d . . . . .
 H2A H -0.1770 0.2279 0.0964 0.067 Uiso 1 1 calc R . . . .
 H2B H -0.1098 0.3039 0.0737 0.067 Uiso 1 1 calc R . . . .
 C3 C -0.2810(11) 0.2737(7) 0.0231(5) 0.059(3) Uani 1 1 d . . . . .
 H3A H -0.3686 0.2520 0.0314 0.071 Uiso 1 1 calc R . . . .
 H3B H -0.2962 0.3253 0.0076 0.071 Uiso 1 1 calc R . . . .
 N3 N 0.2992(13) 0.2218(10) 0.17885(14) 0.041(4) Uani 0.560(12) 1 d D U . A 1
 H3C H 0.2279 0.1922 0.1857 0.049 Uiso 0.560(12) 1 d R . . A 1
 H3D H 0.2903 0.2671 0.1969 0.049 Uiso 0.560(12) 1 d R . . A 1
 H3E H 0.3747 0.1987 0.1930 0.049 Uiso 0.560(12) 1 d R . . A 1
 C7 C 0.3177(13) 0.2368(8) 0.11576(15) 0.063(3) Uani 0.560(12) 1 d D U . A 1
 H7A H 0.3961 0.2085 0.1033 0.076 Uiso 0.560(12) 1 calc R . . A 1
 H7B H 0.3354 0.2913 0.1103 0.076 Uiso 0.560(12) 1 calc R . . A 1
 C8 C 0.1981(17) 0.2145(14) 0.0779(6) 0.071(3) Uani 0.560(12) 1 d D U . A 1
 H8A H 0.1750 0.1618 0.0874 0.086 Uiso 0.560(12) 1 calc R . . A 1
 H8B H 0.1225 0.2467 0.0885 0.086 Uiso 0.560(12) 1 calc R . . A 1
 C9 C 0.211(2) 0.2199(11) 0.0149(6) 0.082(4) Uani 0.560(12) 1 d D U . A 1
 H9A H 0.1192 0.2227 -0.0025 0.099 Uiso 0.560(12) 1 calc R . . A 1
 H9B H 0.2476 0.1709 0.0025 0.099 Uiso 0.560(12) 1 calc R . . A 1
 C12 C 0.265(3) 0.2781(17) 0.0198(8) 0.080(4) Uani 0.440(12) 1 d D U . A 2
 H12A H 0.1822 0.3059 0.0267 0.096 Uiso 0.440(12) 1 calc R . . A 2
 H12B H 0.3258 0.3139 0.0013 0.096 Uiso 0.440(12) 1 calc R . . A 2
 C11 C 0.327(2) 0.2572(16) 0.0771(7) 0.072(4) Uani 0.440(12) 1 d D U . A 2
 H11A H 0.4054 0.2253 0.0705 0.086 Uiso 0.440(12) 1 calc R . . A 2
 H11B H 0.3593 0.3039 0.0966 0.086 Uiso 0.440(12) 1 calc R . . A 2
 C10 C 0.2426(11) 0.2168(14) 0.11739(15) 0.064(4) Uani 0.440(12) 1 d D U . A 2
 H10A H 0.2339 0.1638 0.1040 0.077 Uiso 0.440(12) 1 calc R . . A 2
 H10B H 0.1528 0.2395 0.1143 0.077 Uiso 0.440(12) 1 calc R . . A 2
 N4 N 0.2880(12) 0.2159(17) 0.18026(15) 0.045(5) Uani 0.440(12) 1 d D U . A 2
 H4C H 0.3161 0.1687 0.1904 0.054 Uiso 0.440(12) 1 calc GR . . A 2
 H4D H 0.2194 0.2294 0.2024 0.054 Uiso 0.440(12) 1 calc GR . . A 2
 H4E H 0.3560 0.2491 0.1863 0.054 Uiso 0.440(12) 1 calc GR . . A 2
 O1 O -0.044(8) 0.457(4) -0.016(3) 0.17(3) Uani 0.25 1 d . U . . .
 H1F H -0.0737 0.4128 -0.0306 0.260 Uiso 0.25 1 d R . . . .
 H1G H -0.0269 0.4838 -0.0419 0.260 Uiso 0.25 1 d R . . . .
 O2 O 0.454(7) 0.005(5) 0.013(3) 0.15(2) Uani 0.25 1 d . U . . .
 H2F H 0.3818 -0.0171 0.0275 0.228 Uiso 0.25 1 d R . . . .
 H2G H 0.4636 0.0404 0.0355 0.228 Uiso 0.25 1 d R . . . .


_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 Br4 2.8739(12) 2 ?
 Sn1 Br4 2.8739(12) . ?
 Sn1 Br5 2.9583(11) 2 ?
 Sn1 Br5 2.9583(11) . ?
 N1 C1 1.471(12) . ?
 N2 C4 1.464(11) . ?
 C4 C5 1.474(12) . ?
 C5 C6 1.507(13) . ?
 C6 C6 1.421(16) 5 ?
 C1 C2 1.495(14) . ?
 C2 C3 1.535(14) . ?
 C3 C3 1.50(2) 7_455 ?
 N3 C7 1.4800(2) . ?
 C7 C8 1.489(12) . ?
 C8 C9 1.450(15) . ?
 C9 C9 1.494(10) 7 ?
 C12 C12 1.36(6) 7 ?
 C12 C11 1.462(10) . ?
 C11 C10 1.456(10) . ?
 C10 N4 1.4800(2) . ?
 O1 O2 1.08(9) 3_455 ?
 O1 O2 1.11(9) 7 ?
 O2 O1 1.08(9) 3_545 ?
 O2 O1 1.11(9) 7 ?
 O2 O2 1.13(12) 5_655 ?

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
 Br4 Sn1 Br4 87.84(5) 2 . ?
 Br4 Sn1 Br5 87.90(3) 2 . ?
 Br4 Sn1 Br5 92.18(3) 2 2 ?
 Br4 Sn1 Br5 87.90(3) . 2 ?
 Br4 Sn1 Br5 92.18(3) . . ?
 Br5 Sn1 Br5 179.89(5) 2 . ?
 N2 C4 C5 113.8(9) . . ?
 C4 C5 C6 108.8(9) . . ?
 C6 C6 C5 116.6(14) 5 . ?
 N1 C1 C2 111.5(8) . . ?
 C1 C2 C3 109.3(9) . . ?
 C3 C3 C2 113.9(12) 7_455 . ?
 N3 C7 C8 112.4(9) . . ?
 C9 C8 C7 116.7(13) . . ?
 C8 C9 C9 124.5(18) . 7 ?
 C12 C12 C11 119(3) 7 . ?
 C10 C11 C12 117.0(14) . . ?
 C11 C10 N4 117.0(12) . . ?
 O2 O1 O2 62(8) 3_455 7 ?
 O1 O2 O1 118(8) 3_545 7 ?
 O1 O2 O2 61(7) 3_545 5_655 ?
 O1 O2 O2 58(7) 7 5_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
