#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/61/4076197.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4076197
loop_
_publ_author_name
'Foreman, Mark R. St.-J.'
'Hill, Anthony F.'
'Smith, Matthew K.'
'Tshabang, Never'
_publ_section_title
;
 Novel Heterobimetallic Coordination of the H2B(mt)2Ligand:  The
 Complex [Mo(SnMe2Cl)(CO)3{\m-S:\k3-H,S,S&#x2018;-H2B(mt)2}] (mt =
 methimazolyl)
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5224
_journal_paper_doi               10.1021/om050778z
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C5.5 H9 B0.5 Cl N2 S Sn0.5'
_chemical_formula_weight         235.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.91(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.690(3)
_cell_length_b                   13.430(3)
_cell_length_c                   9.6120(19)
_cell_measurement_temperature    173(2)
_cell_volume                     1763.1(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18133
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.986
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             932
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.0096(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0609P)²+3.9136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                1849
_reflns_number_total             2121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050778zsi20050907_100853.cif
_cod_data_source_block
c:\docume~1\admini~1\desktop\newxta~1\mks28\mks28
_cod_original_cell_volume        1763.1(6)
_cod_original_formula_sum        'C5.50 H9 B0.50 Cl N2 S Sn0.50'
_cod_database_code               4076197
loop_
_symmetry_equiv_pos_as_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'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 0.57589(2) 0.5000 0.22255(3) 0.03325(17) Uani 1 2 d S
Cl2 Cl 0.41846(14) 0.0000 -0.1065(2) 0.0792(6) Uani 1 2 d S
Cl1 Cl 0.5000 0.35787(10) 0.0000 0.0488(4) Uani 1 2 d S
C2 C 0.4280(3) 0.5000 0.2731(5) 0.0320(10) Uani 1 2 d S
H2A H 0.4251 0.5000 0.3747 0.048 Uiso 1 2 calc SR
H2B H 0.3951 0.4404 0.2341 0.048 Uiso 0.50 1 calc PR
H2C H 0.3951 0.5596 0.2341 0.048 Uiso 0.50 1 calc PR
B1 B 0.8227(4) 0.5000 0.5001(6) 0.0320(11) Uani 1 2 d S
C1 C 0.6995(4) 0.5000 0.1002(5) 0.0357(11) Uani 1 2 d S
H1A H 0.7596 0.5000 0.1617 0.054 Uiso 1 2 calc SR
H1B H 0.6980 0.5596 0.0412 0.054 Uiso 0.50 1 calc PR
H1C H 0.6980 0.4404 0.0412 0.054 Uiso 0.50 1 calc PR
C3 C 0.5000 -0.0662(15) 0.0000 0.241(12) Uani 1 2 d S
S11 S 0.62600(6) 0.64221(6) 0.39043(9) 0.0333(2) Uani 1 1 d .
N11 N 0.8234(2) 0.5948(2) 0.4033(3) 0.0313(6) Uani 1 1 d .
C11 C 0.7486(2) 0.6529(2) 0.3572(3) 0.0307(7) Uani 1 1 d .
N12 N 0.7827(2) 0.7238(2) 0.2733(3) 0.0379(7) Uani 1 1 d .
C12 C 0.9065(3) 0.6313(3) 0.3472(4) 0.0398(8) Uani 1 1 d .
H12 H 0.9706 0.6046 0.3628 0.048 Uiso 1 1 calc R
C13 C 0.8821(3) 0.7108(3) 0.2671(4) 0.0455(9) Uani 1 1 d .
H13 H 0.9249 0.7502 0.2163 0.055 Uiso 1 1 calc R
C14 C 0.7244(3) 0.8022(3) 0.2036(5) 0.0507(10) Uani 1 1 d .
H14A H 0.6662 0.7729 0.1545 0.076 Uiso 1 1 calc R
H14B H 0.7636 0.8362 0.1364 0.076 Uiso 1 1 calc R
H14C H 0.7042 0.8501 0.2729 0.076 Uiso 1 1 calc R
H1BA H 0.754(5) 0.5000 0.555(7) 0.054(19) Uiso 1 2 d S
H1BB H 0.888(4) 0.5000 0.568(6) 0.040(15) Uiso 1 2 d S
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'
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 '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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 Sn1 C1 159.75(19) . .
C2 Sn1 S11 94.28(9) . .
C1 Sn1 S11 99.17(9) . .
C2 Sn1 S11 94.28(9) . 6_565
C1 Sn1 S11 99.17(9) . 6_565
S11 Sn1 S11 96.33(5) . 6_565
C2 Sn1 Cl1 82.73(10) . .
C1 Sn1 Cl1 81.69(11) . .
S11 Sn1 Cl1 171.09(3) . .
S11 Sn1 Cl1 92.27(3) 6_565 .
C3 Cl2 C3 62.6(12) 5_655 .
N11 B1 N11 107.6(4) 6_565 .
Cl2 C3 Cl2 117.4(12) 5_655 .
C11 S11 Sn1 99.58(11) . .
C11 N11 C12 107.2(3) . .
C11 N11 B1 129.1(3) . .
C12 N11 B1 123.7(3) . .
N11 C11 N12 108.7(3) . .
N11 C11 S11 128.2(3) . .
N12 C11 S11 123.0(3) . .
C11 N12 C13 108.6(3) . .
C11 N12 C14 125.7(3) . .
C13 N12 C14 125.7(3) . .
C13 C12 N11 109.0(3) . .
C12 C13 N12 106.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 C2 2.115(4) .
Sn1 C1 2.126(5) .
Sn1 S11 2.5635(10) .
Sn1 S11 2.5635(10) 6_565
Sn1 Cl1 2.9993(10) .
Cl2 C3 1.711(11) 5_655
Cl2 C3 1.711(11) .
B1 N11 1.578(4) 6_565
B1 N11 1.578(4) .
C3 Cl2 1.711(11) 5_655
S11 C11 1.736(3) .
N11 C11 1.338(4) .
N11 C12 1.382(4) .
C11 N12 1.352(4) .
N12 C13 1.377(5) .
N12 C14 1.456(5) .
C12 C13 1.345(6) .
