#------------------------------------------------------------------------------
#$Date: 2015-07-11 01:21:34 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143678 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/52/7035241.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_7035241
loop_
_publ_author_name
'Yang, Ya-Xiu'
'Li, Yongxin'
'Ganguly, Rakesh'
'So, Cheuk-Wai'
_publ_section_title
;
 Instability of metal 1,3-benzodi(thiophosphinoyl)methandiide complexes:
 formation of hafnium, tin and zirconium complexes of
 1,3-benzodi(thiophosphinoyl)thioketone dianionic ligand
 [1,3-C6H4(PhPS)2CS](2.).
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12633
_journal_page_last               12639
_journal_paper_doi               10.1039/c5dt01212k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C40 H32 Cl4 P4 S6 Sn'
_chemical_formula_weight         1089.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-05-18 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.804(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9643(5)
_cell_length_b                   12.8350(6)
_cell_length_c                   14.6553(5)
_cell_measurement_reflns_used    6697
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.33
_cell_volume                     2250.27(16)
_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      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24725
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         2.699
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4602
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0291P)²+1.9557P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3975
_reflns_number_total             4602
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01212k2.cif
_cod_data_source_block           scw767s
_cod_depositor_comments
'Adding full bibliography for 7035237--7035241.cif.'
_cod_database_code               7035241
_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   0.770
_shelx_estimated_absorpt_t_max   0.805
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Sn1 Sn 0.0000 0.5000 0.0000 0.01312(8) Uani 1 2 d S . P . .
C1 C 0.1015(2) 0.62724(18) 0.16591(16) 0.0131(5) Uani 1 1 d . . . . .
C2 C -0.0789(2) 0.66912(19) 0.29537(15) 0.0140(5) Uani 1 1 d . . . . .
C3 C -0.0175(2) 0.7525(2) 0.33069(17) 0.0235(6) Uani 1 1 d . . . . .
H3 H 0.0602 0.7586 0.3189 0.028 Uiso 1 1 calc R U . . .
C4 C -0.0710(3) 0.8263(2) 0.38296(18) 0.0282(7) Uani 1 1 d . . . . .
H4 H -0.0302 0.8841 0.4065 0.034 Uiso 1 1 calc R U . . .
C5 C -0.1835(2) 0.8166(2) 0.40136(17) 0.0236(6) Uani 1 1 d . . . . .
H5 H -0.2194 0.8668 0.4385 0.028 Uiso 1 1 calc R U . . .
C6 C -0.2437(2) 0.7343(2) 0.36593(17) 0.0233(6) Uani 1 1 d . . . . .
H6 H -0.3213 0.7284 0.3781 0.028 Uiso 1 1 calc R U . . .
C7 C -0.1918(2) 0.6600(2) 0.31268(16) 0.0187(5) Uani 1 1 d . . . . .
H7 H -0.2335 0.6033 0.2882 0.022 Uiso 1 1 calc R U . . .
C8 C 0.0800(2) 0.49650(18) 0.30988(16) 0.0144(5) Uani 1 1 d . . . . .
C9 C 0.0443(2) 0.4521(2) 0.39067(16) 0.0179(5) Uani 1 1 d . . . . .
H9 H -0.0297 0.4631 0.4114 0.021 Uiso 1 1 calc R U . . .
C10 C 0.1184(2) 0.3914(2) 0.44040(17) 0.0202(6) Uani 1 1 d . . . . .
H10 H 0.0951 0.3606 0.4959 0.024 Uiso 1 1 calc R U . . .
C11 C 0.2260(2) 0.3748(2) 0.41048(17) 0.0234(6) Uani 1 1 d . . . . .
H11 H 0.2758 0.3328 0.4457 0.028 Uiso 1 1 calc R U . . .
C12 C 0.2624(2) 0.4189(2) 0.32936(16) 0.0191(5) Uani 1 1 d . . . . .
H12 H 0.3365 0.4077 0.3090 0.023 Uiso 1 1 calc R U . . .
C13 C 0.1880(2) 0.47946(18) 0.27893(16) 0.0146(5) Uani 1 1 d . . . . .
C14 C 0.3468(2) 0.60213(19) 0.17441(16) 0.0160(5) Uani 1 1 d . . . . .
C15 C 0.3648(2) 0.6737(2) 0.24479(18) 0.0216(6) Uani 1 1 d . . . . .
H15 H 0.3078 0.6867 0.2878 0.026 Uiso 1 1 calc R U . . .
C16 C 0.4656(2) 0.7255(2) 0.25173(19) 0.0247(6) Uani 1 1 d . . . . .
H16 H 0.4785 0.7738 0.2998 0.030 Uiso 1 1 calc R U . . .
C17 C 0.5482(2) 0.7067(2) 0.18807(19) 0.0278(6) Uani 1 1 d . . . . .
H17 H 0.6172 0.7431 0.1926 0.033 Uiso 1 1 calc R U . . .
C18 C 0.5315(2) 0.6364(2) 0.11889(19) 0.0269(6) Uani 1 1 d . . . . .
H18 H 0.5888 0.6235 0.0761 0.032 Uiso 1 1 calc R U . . .
C19 C 0.4297(2) 0.5838(2) 0.11172(18) 0.0214(6) Uani 1 1 d . . . . .
H19 H 0.4174 0.5353 0.0636 0.026 Uiso 1 1 calc R U . . .
C20 C 0.6311(18) 0.392(2) 0.4841(17) 0.072(3) Uani 0.160(3) 1 d D U P A 1
H20A H 0.5829 0.3290 0.4827 0.087 Uiso 0.160(3) 1 calc R U P A 1
H20B H 0.6195 0.4261 0.5437 0.087 Uiso 0.160(3) 1 calc R U P A 1
Cl1 Cl 0.5842(13) 0.4727(14) 0.4028(9) 0.087(3) Uani 0.160(3) 1 d D U P A 1
Cl2 Cl 0.7681(12) 0.3501(12) 0.4817(12) 0.050(3) Uani 0.160(3) 1 d D U P A 1
C20A C 0.6753(12) 0.3767(12) 0.3651(9) 0.065(2) Uani 0.594(3) 1 d D U P B 2
H20C H 0.6384 0.3096 0.3503 0.078 Uiso 0.594(3) 1 calc R U P B 2
H20D H 0.7293 0.3915 0.3162 0.078 Uiso 0.594(3) 1 calc R U P B 2
Cl1A Cl 0.5718(2) 0.4769(3) 0.3644(2) 0.0690(8) Uani 0.594(3) 1 d D U P B 2
Cl2A Cl 0.7461(4) 0.3636(4) 0.4644(3) 0.0755(12) Uani 0.594(3) 1 d D U P B 2
C20B C 0.6648(14) 0.3703(19) 0.4723(10) 0.074(3) Uani 0.246(2) 1 d D U P C 3
H20E H 0.6137 0.3122 0.4871 0.089 Uiso 0.246(2) 1 calc R U P C 3
H20F H 0.6383 0.4323 0.5059 0.089 Uiso 0.246(2) 1 calc R U P C 3
Cl1B Cl 0.6505(9) 0.3957(9) 0.3589(6) 0.093(3) Uani 0.246(2) 1 d D U P C 3
Cl2B Cl 0.7960(6) 0.3387(6) 0.5152(4) 0.0534(16) Uani 0.246(2) 1 d D U P C 3
P1 P -0.00398(5) 0.57226(5) 0.23183(4) 0.01197(14) Uani 1 1 d . . . . .
P2 P 0.21302(5) 0.53849(5) 0.16925(4) 0.01299(14) Uani 1 1 d . . . . .
S1 S -0.10907(5) 0.48037(5) 0.15948(4) 0.01535(14) Uani 1 1 d . . . . .
S2 S 0.20224(5) 0.43300(5) 0.06738(4) 0.01696(14) Uani 1 1 d . . . . .
S3 S 0.05928(5) 0.67295(5) 0.05893(4) 0.01462(14) Uani 1 1 d . . . . .
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'
P P 0.1023 0.0942 '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'
Sn Sn -0.6537 1.4246 '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'
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
S3 Sn1 S3 180.0 3_565 .
S3 Sn1 S1 94.499(18) 3_565 .
S3 Sn1 S1 85.502(18) . .
S3 Sn1 S1 85.501(18) 3_565 3_565
S3 Sn1 S1 94.498(18) . 3_565
S1 Sn1 S1 180.000(12) . 3_565
S3 Sn1 S2 95.242(19) 3_565 .
S3 Sn1 S2 84.758(19) . .
S1 Sn1 S2 95.377(19) . .
S1 Sn1 S2 84.623(19) 3_565 .
S3 Sn1 S2 84.757(19) 3_565 3_565
S3 Sn1 S2 95.243(19) . 3_565
S1 Sn1 S2 84.622(19) . 3_565
S1 Sn1 S2 95.378(19) 3_565 3_565
S2 Sn1 S2 180.0 . 3_565
S3 C1 P1 115.51(13) . .
S3 C1 P2 117.03(13) . .
P1 C1 P2 106.08(12) . .
C7 C2 C3 120.5(2) . .
C7 C2 P1 122.11(19) . .
C3 C2 P1 117.29(19) . .
C4 C3 C2 119.1(3) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C3 C4 C5 120.5(3) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
C6 C5 C4 120.1(2) . .
C6 C5 H5 120.0 . .
C4 C5 H5 120.0 . .
C5 C6 C7 120.3(3) . .
C5 C6 H6 119.8 . .
C7 C6 H6 119.8 . .
C2 C7 C6 119.5(2) . .
C2 C7 H7 120.2 . .
C6 C7 H7 120.2 . .
C9 C8 C13 120.7(2) . .
C9 C8 P1 126.2(2) . .
C13 C8 P1 112.98(18) . .
C10 C9 C8 118.7(2) . .
C10 C9 H9 120.7 . .
C8 C9 H9 120.7 . .
C9 C10 C11 120.9(2) . .
C9 C10 H10 119.5 . .
C11 C10 H10 119.5 . .
C10 C11 C12 120.8(2) . .
C10 C11 H11 119.6 . .
C12 C11 H11 119.6 . .
C13 C12 C11 118.5(2) . .
C13 C12 H12 120.8 . .
C11 C12 H12 120.8 . .
C12 C13 C8 120.4(2) . .
C12 C13 P2 126.6(2) . .
C8 C13 P2 112.96(18) . .
C19 C14 C15 119.9(2) . .
C19 C14 P2 122.8(2) . .
C15 C14 P2 117.28(19) . .
C16 C15 C14 119.8(3) . .
C16 C15 H15 120.1 . .
C14 C15 H15 120.1 . .
C15 C16 C17 119.7(3) . .
C15 C16 H16 120.1 . .
C17 C16 H16 120.1 . .
C18 C17 C16 120.9(3) . .
C18 C17 H17 119.6 . .
C16 C17 H17 119.6 . .
C17 C18 C19 119.5(3) . .
C17 C18 H18 120.2 . .
C19 C18 H18 120.2 . .
C14 C19 C18 120.1(3) . .
C14 C19 H19 119.9 . .
C18 C19 H19 119.9 . .
Cl1 C20 Cl2 119.2(15) . .
Cl1 C20 H20A 107.5 . .
Cl2 C20 H20A 107.5 . .
Cl1 C20 H20B 107.5 . .
Cl2 C20 H20B 107.5 . .
H20A C20 H20B 107.0 . .
Cl2A C20A Cl1A 114.7(7) . .
Cl2A C20A H20C 108.6 . .
Cl1A C20A H20C 108.6 . .
Cl2A C20A H20D 108.6 . .
Cl1A C20A H20D 108.6 . .
H20C C20A H20D 107.6 . .
Cl1B C20B Cl2B 118.5(11) . .
Cl1B C20B H20E 107.7 . .
Cl2B C20B H20E 107.7 . .
Cl1B C20B H20F 107.7 . .
Cl2B C20B H20F 107.7 . .
H20E C20B H20F 107.1 . .
C1 P1 C8 99.72(11) . .
C1 P1 C2 112.06(11) . .
C8 P1 C2 108.80(11) . .
C1 P1 S1 113.29(8) . .
C8 P1 S1 110.93(8) . .
C2 P1 S1 111.40(9) . .
C1 P2 C14 112.49(11) . .
C1 P2 C13 99.30(11) . .
C14 P2 C13 108.17(11) . .
C1 P2 S2 111.98(8) . .
C14 P2 S2 112.55(9) . .
C13 P2 S2 111.55(8) . .
P1 S1 Sn1 95.46(3) . .
P2 S2 Sn1 95.91(3) . .
C1 S3 Sn1 95.15(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S3 2.4818(6) 3_565
Sn1 S3 2.4818(6) .
Sn1 S1 2.7045(6) .
Sn1 S1 2.7046(6) 3_565
Sn1 S2 2.7390(6) .
Sn1 S2 2.7390(6) 3_565
C1 S3 1.742(2) .
C1 P1 1.749(2) .
C1 P2 1.755(2) .
C2 C7 1.383(3) .
C2 C3 1.394(4) .
C2 P1 1.800(2) .
C3 C4 1.381(4) .
C3 H3 0.9500 .
C4 C5 1.382(4) .
C4 H4 0.9500 .
C5 C6 1.376(4) .
C5 H5 0.9500 .
C6 C7 1.384(4) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 C9 1.387(3) .
C8 C13 1.393(4) .
C8 P1 1.797(2) .
C9 C10 1.380(4) .
C9 H9 0.9500 .
C10 C11 1.383(4) .
C10 H10 0.9500 .
C11 C12 1.392(4) .
C11 H11 0.9500 .
C12 C13 1.387(3) .
C12 H12 0.9500 .
C13 P2 1.806(2) .
C14 C19 1.382(4) .
C14 C15 1.395(3) .
C14 P2 1.798(2) .
C15 C16 1.380(4) .
C15 H15 0.9500 .
C16 C17 1.390(4) .
C16 H16 0.9500 .
C17 C18 1.370(4) .
C17 H17 0.9500 .
C18 C19 1.395(4) .
C18 H18 0.9500 .
C19 H19 0.9500 .
C20 Cl1 1.672(15) .
C20 Cl2 1.724(15) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C20A Cl2A 1.682(11) .
C20A Cl1A 1.784(10) .
C20A H20C 0.9900 .
C20A H20D 0.9900 .
C20B Cl1B 1.700(12) .
C20B Cl2B 1.731(13) .
C20B H20E 0.9900 .
C20B H20F 0.9900 .
P1 S1 2.0146(9) .
P2 S2 2.0183(9) .
