#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:48:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178535 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/41/4064185.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_4064185
loop_
_publ_author_name
'Tan, Runyu'
'Song, Datong'
_publ_section_title
;
 C−H and C−S Activations of Quinoline-Functionalized
 Thiophenes by Platinum Complexes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1637
_journal_paper_doi               10.1021/om101171s
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C27 H41 N P2 Pt S'
_chemical_formula_weight         668.70
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.411(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3049(6)
_cell_length_b                   9.9102(3)
_cell_length_c                   16.1325(8)
_cell_measurement_reflns_used    6241
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.38
_cell_volume                     2721.10(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23965
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    5.367
_exptl_absorpt_correction_T_max  0.8140
_exptl_absorpt_correction_T_min  0.5652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'bruker apex 2'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0291P)²+0.6194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                5109
_reflns_number_total             6246
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101171s_si_002.cif
_cod_data_source_block           4a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064185
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
C1 C 0.2127(2) -0.0593(4) 0.2042(2) 0.0199(8) Uani 1 1 d .
C2 C 0.2757(2) -0.1367(4) 0.1947(3) 0.0242(8) Uani 1 1 d .
H2A H 0.2769 -0.2246 0.2183 0.029 Uiso 1 1 calc R
C3 C 0.3397(2) -0.1036(4) 0.1541(3) 0.0266(9) Uani 1 1 d .
H3A H 0.3771 -0.1739 0.1540 0.032 Uiso 1 1 calc R
C4 C 0.3559(2) 0.0108(4) 0.1160(2) 0.0235(8) Uani 1 1 d .
H4A H 0.4042 0.0114 0.0957 0.028 Uiso 1 1 calc R
C5 C 0.2484(3) -0.3114(4) 0.4202(3) 0.0306(9) Uani 1 1 d .
H5A H 0.3009 -0.3288 0.4472 0.037 Uiso 1 1 calc R
C6 C 0.1880(3) -0.3759(4) 0.4532(3) 0.0349(10) Uani 1 1 d .
H6A H 0.1993 -0.4362 0.4996 0.042 Uiso 1 1 calc R
C7 C 0.1128(3) -0.3482(4) 0.4159(3) 0.0331(10) Uani 1 1 d .
H7A H 0.0704 -0.3895 0.4365 0.040 Uiso 1 1 calc R
C8 C 0.0970(2) -0.2589(4) 0.3470(3) 0.0260(9) Uani 1 1 d .
C9 C 0.0199(2) -0.2241(4) 0.3084(3) 0.0295(10) Uani 1 1 d .
H9A H -0.0235 -0.2634 0.3280 0.035 Uiso 1 1 calc R
C10 C 0.0072(2) -0.1348(4) 0.2434(3) 0.0302(9) Uani 1 1 d .
H10A H -0.0448 -0.1083 0.2195 0.036 Uiso 1 1 calc R
C11 C 0.0716(2) -0.0818(4) 0.2118(3) 0.0273(9) Uani 1 1 d .
H11A H 0.0615 -0.0210 0.1655 0.033 Uiso 1 1 calc R
C12 C 0.1487(2) -0.1138(4) 0.2447(2) 0.0203(8) Uani 1 1 d .
C13 C 0.1630(2) -0.2025(3) 0.3164(2) 0.0215(8) Uani 1 1 d .
C14 C 0.3474(2) 0.4435(4) -0.0114(3) 0.0271(9) Uani 1 1 d .
H14A H 0.3908 0.5097 -0.0064 0.032 Uiso 1 1 calc R
H14B H 0.3280 0.4270 -0.0721 0.032 Uiso 1 1 calc R
C15 C 0.2804(2) 0.5039(4) 0.0280(3) 0.0301(10) Uani 1 1 d .
H15A H 0.2491 0.5661 -0.0129 0.036 Uiso 1 1 calc R
H15B H 0.3031 0.5568 0.0786 0.036 Uiso 1 1 calc R
C16 C 0.4739(2) 0.3384(4) 0.1140(3) 0.0279(9) Uani 1 1 d .
H16A H 0.5055 0.3974 0.0825 0.033 Uiso 1 1 calc R
C17 C 0.4514(3) 0.4221(5) 0.1851(3) 0.0383(11) Uani 1 1 d .
H17A H 0.4990 0.4497 0.2239 0.057 Uiso 1 1 calc R
H17B H 0.4182 0.3680 0.2156 0.057 Uiso 1 1 calc R
H17C H 0.4224 0.5024 0.1616 0.057 Uiso 1 1 calc R
C18 C 0.5261(3) 0.2188(5) 0.1499(3) 0.0453(13) Uani 1 1 d .
H18A H 0.5721 0.2525 0.1891 0.068 Uiso 1 1 calc R
H18B H 0.5435 0.1700 0.1037 0.068 Uiso 1 1 calc R
H18C H 0.4961 0.1577 0.1799 0.068 Uiso 1 1 calc R
C19 C 0.4251(2) 0.1904(4) -0.0425(3) 0.0280(9) Uani 1 1 d .
H19A H 0.4535 0.1100 -0.0145 0.034 Uiso 1 1 calc R
C21 C 0.3588(2) 0.1376(5) -0.1098(3) 0.0339(10) Uani 1 1 d .
H21A H 0.3811 0.0882 -0.1526 0.051 Uiso 1 1 calc R
H21B H 0.3275 0.2136 -0.1364 0.051 Uiso 1 1 calc R
H21C H 0.3253 0.0771 -0.0839 0.051 Uiso 1 1 calc R
C22 C 0.4839(3) 0.2702(5) -0.0830(3) 0.0432(12) Uani 1 1 d .
H22A H 0.5023 0.2142 -0.1256 0.065 Uiso 1 1 calc R
H22B H 0.5287 0.2961 -0.0396 0.065 Uiso 1 1 calc R
H22C H 0.4585 0.3515 -0.1097 0.065 Uiso 1 1 calc R
C23 C 0.1666(2) 0.4499(4) 0.1381(2) 0.0257(9) Uani 1 1 d .
H23A H 0.1262 0.3834 0.1493 0.031 Uiso 1 1 calc R
C24 C 0.2234(3) 0.4679(4) 0.2211(3) 0.0343(10) Uani 1 1 d .
H24A H 0.1958 0.5093 0.2626 0.051 Uiso 1 1 calc R
H24B H 0.2669 0.5263 0.2123 0.051 Uiso 1 1 calc R
H24C H 0.2441 0.3797 0.2417 0.051 Uiso 1 1 calc R
C25 C 0.1221(3) 0.5798(5) 0.1099(3) 0.0407(11) Uani 1 1 d .
H25A H 0.0978 0.6144 0.1560 0.061 Uiso 1 1 calc R
H25B H 0.0813 0.5611 0.0608 0.061 Uiso 1 1 calc R
H25C H 0.1588 0.6471 0.0950 0.061 Uiso 1 1 calc R
C26 C 0.1364(2) 0.3574(4) -0.0354(3) 0.0271(9) Uani 1 1 d .
H26A H 0.1128 0.4490 -0.0474 0.032 Uiso 1 1 calc R
C27 C 0.1666(3) 0.3111(5) -0.1137(3) 0.0393(11) Uani 1 1 d .
H27A H 0.1226 0.3047 -0.1612 0.059 Uiso 1 1 calc R
H27B H 0.1916 0.2225 -0.1032 0.059 Uiso 1 1 calc R
H27C H 0.2051 0.3764 -0.1271 0.059 Uiso 1 1 calc R
C28 C 0.0713(3) 0.2632(5) -0.0177(3) 0.0370(11) Uani 1 1 d .
H28A H 0.0301 0.2571 -0.0680 0.055 Uiso 1 1 calc R
H28B H 0.0489 0.2989 0.0294 0.055 Uiso 1 1 calc R
H28C H 0.0932 0.1733 -0.0032 0.055 Uiso 1 1 calc R
N1 N 0.23821(19) -0.2295(3) 0.3556(2) 0.0253(7) Uani 1 1 d .
S1 S 0.19610(5) 0.10358(9) 0.16532(6) 0.0218(2) Uani 1 1 d .
Pt1 Pt 0.291358(8) 0.182293(13) 0.095783(9) 0.01744(5) Uani 1 1 d .
P1 P 0.38550(6) 0.28414(10) 0.03921(7) 0.0219(2) Uani 1 1 d .
P2 P 0.21581(6) 0.37236(10) 0.05781(6) 0.0208(2) 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'
N N 0.0061 0.0033 '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'
Pt Pt -1.7033 8.3905 '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
C2 C1 C12 121.3(3)
C2 C1 S1 124.4(3)
C12 C1 S1 114.2(3)
C1 C2 C3 128.8(4)
C4 C3 C2 130.4(4)
C3 C4 Pt1 128.8(3)
N1 C5 C6 125.5(4)
C7 C6 C5 117.2(4)
C6 C7 C8 120.6(4)
C7 C8 C9 122.3(4)
C7 C8 C13 117.6(4)
C9 C8 C13 120.1(4)
C10 C9 C8 120.5(4)
C9 C10 C11 119.7(4)
C12 C11 C10 123.1(4)
C11 C12 C13 117.7(3)
C11 C12 C1 119.4(3)
C13 C12 C1 122.8(3)
N1 C13 C8 121.0(4)
N1 C13 C12 120.2(3)
C8 C13 C12 118.8(3)
C15 C14 P1 112.7(3)
C14 C15 P2 111.8(3)
C17 C16 C18 110.4(4)
C17 C16 P1 110.9(3)
C18 C16 P1 112.5(3)
C21 C19 C22 110.3(4)
C21 C19 P1 110.8(3)
C22 C19 P1 114.1(3)
C24 C23 C25 112.0(3)
C24 C23 P2 111.1(3)
C25 C23 P2 114.5(3)
C27 C26 C28 110.3(4)
C27 C26 P2 112.5(3)
C28 C26 P2 111.2(3)
C5 N1 C13 118.0(4)
C1 S1 Pt1 114.00(13)
C4 Pt1 P1 91.31(11)
C4 Pt1 S1 93.46(11)
P1 Pt1 S1 172.17(4)
C4 Pt1 P2 173.96(11)
P1 Pt1 P2 86.74(4)
S1 Pt1 P2 89.12(3)
C19 P1 C14 105.34(19)
C19 P1 C16 104.07(19)
C14 P1 C16 103.13(19)
C19 P1 Pt1 117.05(13)
C14 P1 Pt1 109.70(13)
C16 P1 Pt1 116.16(14)
C15 P2 C23 105.58(19)
C15 P2 C26 104.00(19)
C23 P2 C26 103.58(18)
C15 P2 Pt1 107.80(13)
C23 P2 Pt1 117.72(13)
C26 P2 Pt1 116.83(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.364(5)
C1 C12 1.486(5)
C1 S1 1.736(4)
C2 C3 1.424(5)
C3 C4 1.343(5)
C4 Pt1 2.028(4)
C5 N1 1.307(5)
C5 C6 1.409(6)
C6 C7 1.359(6)
C7 C8 1.409(6)
C8 C9 1.409(6)
C8 C13 1.436(5)
C9 C10 1.359(6)
C10 C11 1.409(5)
C11 C12 1.380(5)
C12 C13 1.438(5)
C13 N1 1.367(5)
C14 C15 1.540(5)
C14 P1 1.844(4)
C15 P2 1.837(4)
C16 C17 1.522(6)
C16 C18 1.540(6)
C16 P1 1.848(4)
C19 C21 1.522(6)
C19 C22 1.525(6)
C19 P1 1.843(4)
C23 C24 1.521(6)
C23 C25 1.525(5)
C23 P2 1.842(4)
C26 C27 1.523(6)
C26 C28 1.528(6)
C26 P2 1.850(4)
S1 Pt1 2.2918(9)
Pt1 P1 2.2458(10)
Pt1 P2 2.3115(10)
