#------------------------------------------------------------------------------
#$Date: 2015-06-07 02:17:40 +0200 (dom 07 de jun de 2015) $
#$Revision: 138729 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/50/7035080.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_7035080
loop_
_publ_author_name
'Zhang, Long'
'Yan, Tao'
'Han, Ying-Feng'
'Hahn, F. Ekkehardt'
'Jin, Guo-Xin'
_publ_section_title
;
 Synthesis of a new type of alkene metal complex using face-capping
 thione-alkene ligands.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8797
_journal_page_last               8800
_journal_paper_doi               10.1039/c5dt01311a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C12 H16 N4 S2'
_chemical_formula_weight         280.41
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-03-11 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                87.479(4)
_cell_angle_beta                 65.560(3)
_cell_angle_gamma                78.797(3)
_cell_formula_units_Z            1
_cell_length_a                   7.0196(16)
_cell_length_b                   7.2219(17)
_cell_length_c                   7.4813(18)
_cell_measurement_reflns_used    1352
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.88
_cell_volume                     338.42(14)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0167
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_laue_measured_fraction_full 0.978
_diffrn_reflns_laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2370
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.878
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             148
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[σ²(Fo²)+(0.1606P)²+0.0452P] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.2158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1255
_reflns_number_total             1445
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01311a2.cif
_cod_data_source_block           L1
_cod_depositor_comments
'Adding full bibliography for 7035074--7035080.cif.'
_cod_database_code               7035080
_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   0.935
_shelx_estimated_absorpt_t_max   0.970
_shelxl_version_number           2013-2
_shelx_res_file
; 
TITL L1 in P-1 
CELL 0.71073   7.0196   7.2219   7.4813  87.479  65.560  78.797 
ZERR    1.00   0.0016   0.0017   0.0018   0.004   0.003   0.003 
LATT 1 
SFAC C  H  N  S 
UNIT 12 16 4 2 
OMIT 3 -4 1 
OMIT  -2.00  54.00 
L.S. 4 
ACTA 
BOND 
FMAP 2 
PLAN 1 
SIZE 0.08 0.12 0.18 
TEMP -100 
WGHT    0.160600    0.045200 
FVAR       0.36238 
MOLE 1 
S1    4    0.318333    0.199887    0.788292    11.00000    0.02519    0.02766 = 
         0.03848    0.00193   -0.01304   -0.01244 
N1    3    0.447172    0.538279    0.755561    11.00000    0.02748    0.02017 = 
         0.02579   -0.00062   -0.00938   -0.00562 
N2    3    0.685210    0.301390    0.761012    11.00000    0.02200    0.02649 = 
         0.02121    0.00052   -0.00757   -0.00827 
C1    1    0.483963    0.346575    0.769112    11.00000    0.02393    0.02290 = 
         0.01829    0.00080   -0.00707   -0.00803 
C5    1    0.896060    0.018952    0.555279    11.00000    0.02303    0.02243 = 
         0.02743    0.00378   -0.01122   -0.00562 
AFIX  43 
H5    2    0.803019   -0.011900    0.503226    11.00000   -1.20000 
AFIX   0 
C4    1    0.800129    0.108076    0.758413    11.00000    0.02354    0.03338 = 
         0.02650    0.00277   -0.01080   -0.00548 
AFIX  23 
H4A   2    0.700585    0.032035    0.850171    11.00000   -1.20000 
H4B   2    0.914304    0.110393    0.802928    11.00000   -1.20000 
AFIX   0 
C3    1    0.770619    0.462171    0.741938    11.00000    0.03021    0.03718 = 
         0.02785    0.00155   -0.01036   -0.01916 
AFIX  43 
H3    2    0.908537    0.467284    0.732859    11.00000   -1.20000 
AFIX   0 
C2    1    0.622919    0.609478    0.738621    11.00000    0.03999    0.02700 = 
         0.03230    0.00040   -0.01152   -0.01867 
AFIX  43 
H2    2    0.636398    0.738312    0.726866    11.00000   -1.20000 
AFIX   0 
C6    1    0.249087    0.651084    0.759779    11.00000    0.03311    0.02641 = 
         0.03518    0.00027   -0.01256    0.00045 
AFIX 137 
H6A   2    0.225420    0.612547    0.647809    11.00000   -1.50000 
H6B   2    0.258639    0.785013    0.751934    11.00000   -1.50000 
H6C   2    0.129999    0.631549    0.882430    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  L1 in P-1 
REM R1 =  0.0462 for    1255 Fo > 4sig(Fo)  and  0.0601 for all    1445 data 
REM     83 parameters refined using      0 restraints 
  
END 
  
WGHT      0.1612      0.0402 
  
REM Highest difference peak  0.599,  deepest hole -0.453,  1-sigma level  0.148 
Q1    1   0.6107  0.3176  0.7582  11.00000  0.05    0.60 
;
_shelx_res_checksum              74618
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
S1 S 0.31833(10) 0.19989(9) 0.78829(10) 0.0294(4) Uani 1 1 d . .
N1 N 0.4472(4) 0.5383(3) 0.7556(3) 0.0248(6) Uani 1 1 d . .
N2 N 0.6852(4) 0.3014(3) 0.7610(3) 0.0232(5) Uani 1 1 d . .
C1 C 0.4840(4) 0.3466(4) 0.7691(4) 0.0217(6) Uani 1 1 d . .
C5 C 0.8961(4) 0.0190(4) 0.5553(4) 0.0239(6) Uani 1 1 d . .
H5 H 0.8030 -0.0119 0.5032 0.029 Uiso 1 1 calc R U
C4 C 0.8001(4) 0.1081(4) 0.7584(4) 0.0277(6) Uani 1 1 d . .
H4A H 0.7006 0.0320 0.8502 0.033 Uiso 1 1 calc R U
H4B H 0.9143 0.1104 0.8029 0.033 Uiso 1 1 calc R U
C3 C 0.7706(5) 0.4622(4) 0.7419(4) 0.0304(7) Uani 1 1 d . .
H3 H 0.9085 0.4673 0.7329 0.037 Uiso 1 1 calc R U
C2 C 0.6229(5) 0.6095(4) 0.7386(4) 0.0324(7) Uani 1 1 d . .
H2 H 0.6364 0.7383 0.7269 0.039 Uiso 1 1 calc R U
C6 C 0.2491(5) 0.6511(4) 0.7598(4) 0.0330(7) Uani 1 1 d . .
H6A H 0.2254 0.6125 0.6478 0.049 Uiso 1 1 calc R U
H6B H 0.2586 0.7850 0.7519 0.049 Uiso 1 1 calc R U
H6C H 0.1300 0.6315 0.8824 0.049 Uiso 1 1 calc R U
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
S1 0.0252(5) 0.0277(5) 0.0385(5) 0.0019(3) -0.0130(4) -0.0124(3)
N1 0.0275(12) 0.0202(11) 0.0258(11) -0.0006(9) -0.0094(9) -0.0056(9)
N2 0.0220(11) 0.0265(12) 0.0212(10) 0.0005(8) -0.0076(8) -0.0083(9)
C1 0.0239(13) 0.0229(13) 0.0183(11) 0.0008(9) -0.0071(10) -0.0080(10)
C5 0.0230(13) 0.0224(12) 0.0274(13) 0.0038(10) -0.0112(10) -0.0056(10)
C4 0.0235(13) 0.0334(15) 0.0265(13) 0.0028(11) -0.0108(11) -0.0055(11)
C3 0.0302(15) 0.0372(16) 0.0279(13) 0.0015(11) -0.0104(12) -0.0192(12)
C2 0.0400(17) 0.0270(14) 0.0323(15) 0.0004(12) -0.0115(13) -0.0187(13)
C6 0.0331(16) 0.0264(14) 0.0352(15) 0.0003(12) -0.0126(12) 0.0004(12)
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'
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
C1 N1 C2 110.6(2) .
C1 N1 C6 124.3(2) .
C2 N1 C6 125.1(3) .
C1 N2 C3 110.4(2) .
C1 N2 C4 124.6(2) .
C3 N2 C4 124.9(2) .
N2 C1 N1 104.6(2) .
N2 C1 S1 128.0(2) .
N1 C1 S1 127.4(2) .
C5 C5 C4 123.3(3) 2_756
N2 C4 C5 110.5(2) .
C2 C3 N2 107.4(3) .
C3 C2 N1 107.0(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C1 1.680(3) .
N1 C1 1.365(3) .
N1 C2 1.383(4) .
N1 C6 1.457(4) .
N2 C1 1.363(3) .
N2 C3 1.383(3) .
N2 C4 1.467(4) .
C5 C5 1.325(5) 2_756
C5 C4 1.499(4) .
C3 C2 1.341(5) .
