#------------------------------------------------------------------------------
#$Date: 2016-05-06 04:00:04 +0200 (vie 06 de may de 2016) $
#$Revision: 182757 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/88/7038864.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_7038864
loop_
_publ_author_name
'Karwasara, Surendar'
'Jha, Chandan Kumar'
'Sinhababu, Soumen'
'Nagendran, Selvarajan'
_publ_section_title
;
 O,S-Heterocyclic stannylenes: synthesis and reactivity.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7200
_journal_page_last               7204
_journal_paper_doi               10.1039/c6dt01013j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C5 H4 Cl Ge N O S'
_chemical_formula_sum            'C5 H4 Cl Ge N O S'
_chemical_formula_weight         234.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-10-13 deposited with the CCDC.
2016-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.608(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4885(19)
_cell_length_b                   13.237(4)
_cell_length_c                   9.119(3)
_cell_measurement_reflns_used    1347
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.27
_cell_volume                     764.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3888
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    4.554
_exptl_absorpt_correction_T_max  0.200
_exptl_absorpt_correction_T_min  0.132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456.0
_exptl_crystal_size_max          0.476
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.353
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0513
_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)+(0.0455P)²+6.7757P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                1266
_reflns_number_total             1347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01013j2.cif
_cod_data_source_block           sursn18m
_cod_depositor_comments
'Adding full bibliography for 7038861--7038866.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7038864
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Ge1 Ge 0.57109(10) 0.12799(5) 0.36286(8) 0.0168(3) Uani 1 1 d .
S1 S 0.2310(3) 0.07501(14) 0.4089(2) 0.0266(5) Uani 1 1 d .
Cl1 Cl 0.4333(3) 0.25408(14) 0.1722(2) 0.0327(5) Uani 1 1 d .
O1 O 0.5063(8) 0.0165(4) 0.2079(6) 0.0283(12) Uani 1 1 d .
N1 N 0.3158(9) -0.0301(4) 0.1780(6) 0.0227(13) Uani 1 1 d .
C5 C 0.2792(12) -0.0953(6) 0.0614(8) 0.0272(16) Uani 1 1 d .
H5 H 0.3798 -0.1038 0.0037 0.033 Uiso 1 1 calc R
C1 C 0.1752(11) -0.0139(5) 0.2658(8) 0.0247(15) Uani 1 1 d .
C3 C -0.0500(12) -0.1373(6) 0.1177(9) 0.0314(18) Uani 1 1 d .
H3 H -0.1742 -0.1749 0.0982 0.038 Uiso 1 1 calc R
C2 C -0.0111(12) -0.0710(6) 0.2350(9) 0.0302(17) Uani 1 1 d .
H2 H -0.1091 -0.0636 0.2949 0.036 Uiso 1 1 calc R
C4 C 0.0949(13) -0.1491(5) 0.0276(9) 0.0316(17) Uani 1 1 d .
H4 H 0.0673 -0.1927 -0.0543 0.038 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0205(4) 0.0129(4) 0.0184(4) 0.0026(3) 0.0076(3) 0.0008(3)
S1 0.0307(10) 0.0273(10) 0.0248(10) -0.0022(7) 0.0125(8) 0.0007(7)
Cl1 0.0387(10) 0.0293(10) 0.0275(10) 0.0007(7) 0.0015(8) 0.0013(8)
O1 0.024(2) 0.025(3) 0.037(3) -0.003(2) 0.010(2) -0.004(2)
N1 0.022(3) 0.025(3) 0.022(3) 0.001(2) 0.007(2) 0.000(2)
C5 0.038(4) 0.028(4) 0.018(4) -0.002(3) 0.011(3) 0.004(3)
C1 0.028(4) 0.028(4) 0.019(4) 0.001(3) 0.009(3) 0.005(3)
C3 0.024(4) 0.031(4) 0.040(5) 0.001(3) 0.007(3) -0.004(3)
C2 0.027(4) 0.031(4) 0.035(4) 0.006(3) 0.011(3) 0.000(3)
C4 0.040(4) 0.024(4) 0.029(4) -0.002(3) 0.004(3) -0.002(3)
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'
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'
Ge Ge 0.1547 1.8001 '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
O1 Ge1 Cl1 90.78(16)
O1 Ge1 S1 81.51(15)
Cl1 Ge1 S1 96.60(7)
C1 S1 Ge1 96.6(2)
N1 O1 Ge1 120.9(4)
C5 N1 O1 116.5(6)
C5 N1 C1 122.7(6)
O1 N1 C1 120.8(6)
N1 C5 C4 120.3(7)
N1 C5 H5 119.8
C4 C5 H5 119.8
N1 C1 C2 117.3(7)
N1 C1 S1 119.6(5)
C2 C1 S1 123.1(6)
C2 C3 C4 120.2(7)
C2 C3 H3 119.9
C4 C3 H3 119.9
C3 C2 C1 120.6(7)
C3 C2 H2 119.7
C1 C2 H2 119.7
C5 C4 C3 118.8(7)
C5 C4 H4 120.6
C3 C4 H4 120.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ge1 O1 2.023(5)
Ge1 Cl1 2.435(2)
Ge1 S1 2.437(2)
S1 C1 1.736(7)
O1 N1 1.354(7)
N1 C5 1.350(9)
N1 C1 1.356(9)
C5 C4 1.368(11)
C5 H5 0.9300
C1 C2 1.401(11)
C3 C2 1.364(11)
C3 C4 1.386(12)
C3 H3 0.9300
C2 H2 0.9300
C4 H4 0.9300
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O1 Ge1 S1 C1 -3.8(3)
Cl1 Ge1 S1 C1 86.0(2)
Cl1 Ge1 O1 N1 -88.9(4)
S1 Ge1 O1 N1 7.6(4)
Ge1 O1 N1 C5 172.8(5)
Ge1 O1 N1 C1 -9.9(8)
O1 N1 C5 C4 177.0(6)
C1 N1 C5 C4 -0.3(11)
C5 N1 C1 C2 2.3(10)
O1 N1 C1 C2 -174.9(6)
C5 N1 C1 S1 -177.5(5)
O1 N1 C1 S1 5.3(9)
Ge1 S1 C1 N1 0.6(6)
Ge1 S1 C1 C2 -179.2(6)
C4 C3 C2 C1 0.0(12)
N1 C1 C2 C3 -2.1(11)
S1 C1 C2 C3 177.7(6)
N1 C5 C4 C3 -1.8(11)
C2 C3 C4 C5 2.0(12)
