#------------------------------------------------------------------------------
#$Date: 2022-03-11 01:02:18 +0200 (Fri, 11 Mar 2022) $
#$Revision: 273620 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/98/7129809.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_7129809
loop_
_publ_author_name
'Shlian, Daniel G.'
'Amemiya, Erika'
'Parkin, Gerard'
_publ_section_title
;
 Synthesis of bis(2-pyridylthio)methyl zinc hydride and catalytic
 hydrosilylation and hydroboration of CO2
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06963B
_journal_year                    2022
_chemical_formula_sum            'C11 H9 I N2 S2 Zn'
_chemical_formula_weight         425.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-12-07 deposited with the CCDC.	2022-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3876(7)
_cell_length_b                   12.6862(6)
_cell_length_c                   7.5630(4)
_cell_measurement_reflns_used    8933
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      32.57
_cell_measurement_theta_min      2.83
_cell_volume                     1380.43(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_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_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16856
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         33.039
_diffrn_reflns_theta_min         2.831
_exptl_absorpt_coefficient_mu    4.296
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5771
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.587
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         2645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0273
_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)+(0.0267P)²+0.3399P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2193
_reflns_number_total             2645
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc06963b2.cif
_cod_data_source_block           bpzis10
_cod_database_code               7129809
_shelx_shelxl_version_number     2014/7
_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. 
;
_shelx_estimated_absorpt_t_min   0.272
_shelx_estimated_absorpt_t_max   0.413
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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_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
I I 0.17666(2) 0.2500 0.20286(3) 0.03806(7) Uani 1 2 d S T P . .
Zn Zn 0.02515(2) 0.2500 0.37440(4) 0.02710(8) Uani 1 2 d S T P . .
S S -0.08484(4) 0.13191(5) 0.66555(7) 0.03612(12) Uani 1 1 d . . . . .
N N -0.05672(11) 0.12277(13) 0.3141(2) 0.0276(3) Uani 1 1 d . . . . .
C1 C -0.0178(2) 0.2500 0.6310(4) 0.0312(5) Uani 1 2 d S T P . .
H1 H 0.027(3) 0.2500 0.716(4) 0.033(9) Uiso 1 2 d S . P . .
C11 C -0.09823(13) 0.07767(15) 0.4532(3) 0.0288(4) Uani 1 1 d . . . . .
C12 C -0.15273(13) -0.01335(17) 0.4339(3) 0.0378(5) Uani 1 1 d . . . . .
H12A H -0.1802 -0.0457 0.5328 0.045 Uiso 1 1 calc R U . . .
C13 C -0.16505(16) -0.05415(19) 0.2670(4) 0.0442(5) Uani 1 1 d . . . . .
H13A H -0.2012 -0.1151 0.2511 0.053 Uiso 1 1 calc R U . . .
C14 C -0.12435(16) -0.00565(18) 0.1225(3) 0.0420(5) Uani 1 1 d . . . . .
H14A H -0.1336 -0.0318 0.0076 0.050 Uiso 1 1 calc R U . . .
C15 C -0.07032(15) 0.08148(17) 0.1517(3) 0.0352(4) Uani 1 1 d . . . . .
H15A H -0.0414 0.1139 0.0544 0.042 Uiso 1 1 calc R U . . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'
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
C1 Zn N 92.17(7) . 7_565 ?
C1 Zn N 92.17(7) . . ?
N Zn N 103.91(9) 7_565 . ?
C1 Zn I 138.41(8) . . ?
N Zn I 112.33(5) 7_565 . ?
N Zn I 112.33(5) . . ?
C11 S C1 104.58(11) . . ?
C11 N C15 118.99(18) . . ?
C11 N Zn 114.72(13) . . ?
C15 N Zn 126.28(14) . . ?
S C1 S 112.56(16) 7_565 . ?
S C1 Zn 107.50(10) 7_565 . ?
S C1 Zn 107.50(10) . . ?
N C11 C12 121.30(19) . . ?
N C11 S 120.13(15) . . ?
C12 C11 S 118.57(16) . . ?
C13 C12 C11 118.5(2) . . ?
C12 C13 C14 120.2(2) . . ?
C15 C14 C13 118.2(2) . . ?
N C15 C14 122.8(2) . . ?
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
I Zn 2.5368(4) . ?
Zn C1 2.037(3) . ?
Zn N 2.0495(17) 7_565 ?
Zn N 2.0495(17) . ?
S C11 1.758(2) . ?
S C1 1.8011(17) . ?
N C11 1.338(2) . ?
N C15 1.349(3) . ?
C1 S 1.8011(17) 7_565 ?
C11 C12 1.403(3) . ?
C12 C13 1.376(4) . ?
C13 C14 1.384(4) . ?
C14 C15 1.369(3) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 S C1 S 109.81(14) . . . 7_565 ?
C11 S C1 Zn -8.38(14) . . . . ?
C15 N C11 C12 2.2(3) . . . . ?
Zn N C11 C12 -176.80(14) . . . . ?
C15 N C11 S -178.04(15) . . . . ?
Zn N C11 S 2.98(19) . . . . ?
C1 S C11 N 3.78(19) . . . . ?
C1 S C11 C12 -176.44(16) . . . . ?
N C11 C12 C13 -1.8(3) . . . . ?
S C11 C12 C13 178.39(16) . . . . ?
C11 C12 C13 C14 -0.1(3) . . . . ?
C12 C13 C14 C15 1.6(3) . . . . ?
C11 N C15 C14 -0.6(3) . . . . ?
Zn N C15 C14 178.25(16) . . . . ?
C13 C14 C15 N -1.3(3) . . . . ?
