#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/07/86/4078678.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_4078678
loop_
_publ_author_name
'Shi, Xiao-Chao'
'Jin, Guo-Xin'
_publ_section_title
;
 Synthesis and Characterization of Nickel(II) and Palladium(II) Complexes
 based on Tridentate [N--NP] and [N--NS] Ligands and Their Applications in
 Norbornene Polymerization
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4748
_journal_paper_doi               10.1021/om3003202
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C31 H32 N2 S'
_chemical_formula_weight         464.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.592(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.590(2)
_cell_length_b                   8.4278(11)
_cell_length_c                   18.031(2)
_cell_measurement_reflns_used    4004
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.25
_cell_measurement_theta_min      2.67
_cell_volume                     2670.3(5)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19483
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.9749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0020(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.4099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1873
_reflns_number_gt                3452
_reflns_number_total             6328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3003202_si_002.cif
_cod_data_source_block           1f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2670.4(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4078678
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
S1 S 0.40941(4) 0.68810(8) 0.08751(4) 0.0692(2) Uani 1 1 d .
N1 N 0.45064(11) 0.5692(2) 0.29419(11) 0.0545(5) Uani 1 1 d .
H1 H 0.4288(16) 0.562(3) 0.2452(16) 0.089(9) Uiso 1 1 d .
N2 N 0.35374(10) 0.4519(2) 0.18616(11) 0.0562(5) Uani 1 1 d .
C1 C 0.40551(11) 0.4945(2) 0.34317(12) 0.0484(5) Uani 1 1 d .
C2 C 0.42400(14) 0.4936(3) 0.41953(13) 0.0614(6) Uani 1 1 d .
H2 H 0.4678 0.5453 0.4375 0.074 Uiso 1 1 calc R
C3 C 0.37855(14) 0.4175(3) 0.46850(14) 0.0663(6) Uani 1 1 d .
H3 H 0.3926 0.4166 0.5188 0.080 Uiso 1 1 calc R
C4 C 0.31232(15) 0.3424(3) 0.44382(16) 0.0704(7) Uani 1 1 d .
H4 H 0.2816 0.2919 0.4772 0.084 Uiso 1 1 calc R
C5 C 0.29274(13) 0.3436(3) 0.37003(15) 0.0634(6) Uani 1 1 d .
H5 H 0.2476 0.2950 0.3536 0.076 Uiso 1 1 calc R
C6 C 0.33847(11) 0.4159(3) 0.31757(12) 0.0515(5) Uani 1 1 d .
C7 C 0.31477(13) 0.4023(3) 0.24030(14) 0.0594(6) Uani 1 1 d .
H7 H 0.2681 0.3544 0.2287 0.071 Uiso 1 1 calc R
C8 C 0.51520(12) 0.6641(3) 0.31611(12) 0.0521(5) Uani 1 1 d .
C9 C 0.58822(12) 0.6038(3) 0.30733(12) 0.0549(5) Uani 1 1 d .
C10 C 0.65003(14) 0.6991(3) 0.32858(15) 0.0715(7) Uani 1 1 d .
H10 H 0.6992 0.6617 0.3229 0.086 Uiso 1 1 calc R
C11 C 0.63957(17) 0.8468(4) 0.35760(17) 0.0855(9) Uani 1 1 d .
H11 H 0.6814 0.9087 0.3721 0.103 Uiso 1 1 calc R
C12 C 0.56661(18) 0.9042(4) 0.36544(17) 0.0885(9) Uani 1 1 d .
H12 H 0.5601 1.0050 0.3852 0.106 Uiso 1 1 calc R
C13 C 0.50373(15) 0.8157(3) 0.34476(15) 0.0676(7) Uani 1 1 d .
C14 C 0.60059(15) 0.4393(3) 0.27624(15) 0.0697(7) Uani 1 1 d .
H14 H 0.5509 0.3972 0.2591 0.084 Uiso 1 1 calc R
C15 C 0.6501(4) 0.4424(6) 0.2119(3) 0.192(3) Uani 1 1 d .
H15A H 0.6985 0.4879 0.2268 0.288 Uiso 1 1 calc R
H15B H 0.6265 0.5052 0.1729 0.288 Uiso 1 1 calc R
H15C H 0.6575 0.3362 0.1945 0.288 Uiso 1 1 calc R
C16 C 0.6333(5) 0.3303(5) 0.3331(3) 0.215(4) Uani 1 1 d .
H16A H 0.6572 0.2428 0.3093 0.323 Uiso 1 1 calc R
H16B H 0.5935 0.2912 0.3630 0.323 Uiso 1 1 calc R
H16C H 0.6703 0.3858 0.3640 0.323 Uiso 1 1 calc R
C17 C 0.42395(16) 0.8853(3) 0.35142(19) 0.0850(9) Uani 1 1 d .
H17 H 0.3879 0.7967 0.3480 0.102 Uiso 1 1 calc R
C18 C 0.4047(2) 0.9958(4) 0.2865(2) 0.1146(12) Uani 1 1 d .
H18A H 0.4397 1.0832 0.2876 0.172 Uiso 1 1 calc R
H18B H 0.3538 1.0351 0.2903 0.172 Uiso 1 1 calc R
H18C H 0.4084 0.9388 0.2407 0.172 Uiso 1 1 calc R
C19 C 0.4136(2) 0.9663(5) 0.4250(2) 0.1290(15) Uani 1 1 d .
H19A H 0.4268 0.8940 0.4647 0.193 Uiso 1 1 calc R
H19B H 0.3614 0.9982 0.4282 0.193 Uiso 1 1 calc R
H19C H 0.4458 1.0580 0.4289 0.193 Uiso 1 1 calc R
C20 C 0.32712(12) 0.4218(3) 0.11252(13) 0.0547(6) Uani 1 1 d .
C21 C 0.28408(14) 0.2892(3) 0.09073(15) 0.0673(7) Uani 1 1 d .
H21 H 0.2705 0.2156 0.1262 0.081 Uiso 1 1 calc R
C22 C 0.26168(15) 0.2661(3) 0.01797(16) 0.0723(7) Uani 1 1 d .
H22 H 0.2329 0.1774 0.0044 0.087 Uiso 1 1 calc R
C23 C 0.28138(14) 0.3730(3) -0.03515(15) 0.0698(7) Uani 1 1 d .
H23 H 0.2652 0.3577 -0.0845 0.084 Uiso 1 1 calc R
C24 C 0.32518(14) 0.5030(3) -0.01525(14) 0.0628(6) Uani 1 1 d .
H24 H 0.3384 0.5751 -0.0515 0.075 Uiso 1 1 calc R
C25 C 0.34984(12) 0.5282(3) 0.05769(13) 0.0541(5) Uani 1 1 d .
C26 C 0.42574(13) 0.7880(3) 0.00234(15) 0.0641(6) Uani 1 1 d .
C27 C 0.38301(18) 0.9169(3) -0.01849(19) 0.0890(9) Uani 1 1 d .
H27 H 0.3444 0.9509 0.0113 0.107 Uiso 1 1 calc R
C28 C 0.3962(2) 0.9971(4) -0.0829(2) 0.1042(11) Uani 1 1 d .
H28 H 0.3667 1.0851 -0.0961 0.125 Uiso 1 1 calc R
C29 C 0.45217(19) 0.9492(4) -0.12781(19) 0.0912(9) Uani 1 1 d .
H29 H 0.4607 1.0031 -0.1717 0.109 Uiso 1 1 calc R
C30 C 0.49505(19) 0.8218(5) -0.1074(2) 0.1037(11) Uani 1 1 d .
H30 H 0.5335 0.7886 -0.1376 0.124 Uiso 1 1 calc R
C31 C 0.48288(16) 0.7404(4) -0.04280(19) 0.0881(9) Uani 1 1 d .
H31 H 0.5131 0.6535 -0.0296 0.106 Uiso 1 1 calc R
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
C25 S1 C26 102.30(11)
C1 N1 C8 123.77(19)
C7 N2 C20 119.3(2)
N1 C1 C2 121.5(2)
N1 C1 C6 120.4(2)
C2 C1 C6 118.17(19)
C3 C2 C1 121.2(2)
C2 C3 C4 120.8(2)
C5 C4 C3 119.0(2)
C4 C5 C6 122.3(2)
C5 C6 C1 118.5(2)
C5 C6 C7 117.8(2)
C1 C6 C7 123.7(2)
N2 C7 C6 124.5(2)
C13 C8 C9 121.6(2)
C13 C8 N1 119.2(2)
C9 C8 N1 119.16(19)
C10 C9 C8 118.0(2)
C10 C9 C14 120.4(2)
C8 C9 C14 121.6(2)
C11 C10 C9 121.0(3)
C10 C11 C12 119.9(2)
C13 C12 C11 121.5(3)
C12 C13 C8 118.0(2)
C12 C13 C17 120.1(2)
C8 C13 C17 121.9(2)
C16 C14 C15 109.3(4)
C16 C14 C9 111.8(3)
C15 C14 C9 111.9(3)
C19 C17 C18 111.6(3)
C19 C17 C13 112.9(3)
C18 C17 C13 110.3(2)
C21 C20 C25 118.7(2)
C21 C20 N2 124.1(2)
C25 C20 N2 117.05(19)
C22 C21 C20 120.9(2)
C21 C22 C23 120.4(2)
C22 C23 C24 119.8(2)
C23 C24 C25 121.2(2)
C24 C25 C20 119.0(2)
C24 C25 S1 124.05(19)
C20 C25 S1 116.98(17)
C27 C26 C31 118.4(3)
C27 C26 S1 120.3(2)
C31 C26 S1 121.3(2)
C26 C27 C28 120.8(3)
C29 C28 C27 120.7(3)
C30 C29 C28 118.8(3)
C29 C30 C31 121.3(3)
C30 C31 C26 119.9(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 C25 1.776(2)
S1 C26 1.786(3)
N1 C1 1.367(3)
N1 C8 1.430(3)
N2 C7 1.288(3)
N2 C20 1.411(3)
C1 C2 1.400(3)
C1 C6 1.412(3)
C2 C3 1.376(3)
C3 C4 1.382(4)
C4 C5 1.359(4)
C5 C6 1.408(3)
C6 C7 1.441(3)
C8 C13 1.396(3)
C8 C9 1.397(3)
C9 C10 1.392(3)
C9 C14 1.515(3)
C10 C11 1.366(4)
C11 C12 1.385(4)
C12 C13 1.372(4)
C13 C17 1.531(4)
C14 C16 1.474(5)
C14 C15 1.482(4)
C17 C19 1.511(5)
C17 C18 1.522(5)
C20 C21 1.396(3)
C20 C25 1.406(3)
C21 C22 1.367(4)
C22 C23 1.370(4)
C23 C24 1.378(3)
C24 C25 1.383(3)
C26 C27 1.364(4)
C26 C31 1.381(4)
C27 C28 1.373(4)
C28 C29 1.363(4)
C29 C30 1.354(5)
C30 C31 1.377(5)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30659843
