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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/38/1513849.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_1513849
loop_
_publ_author_name
'Tulchinsky, Yuri'
'Kozuch, Sebastian'
'Saha, Prasenjit'
'Botoshansky, Mark'
'Shimon, Linda J. W.'
'Gandelman, Mark'
_publ_section_title
;
 Cation--cation bonding in nitrenium metal complexes
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1305
_journal_paper_doi               10.1039/c3sc53083c
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety
'C34 H36 Cl N3 P2 Pt, 2(C F3 O3 S), 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H40 Cl5 F6 N3 O6 P2 Pt S2'
_chemical_formula_weight         1247.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.7260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.8737(3)
_cell_length_b                   12.5922(2)
_cell_length_c                   16.04680(10)
_cell_measurement_reflns_used    44905
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     4667.93(11)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega 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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44905
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    3.522
_exptl_absorpt_correction_T_max  0.7659
_exptl_absorpt_correction_T_min  0.3720
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Numabs, Hitashi 1999'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.063
_refine_diff_density_min         -1.784
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0299
_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)+(0.0493P)²+7.8971P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                4985
_reflns_number_total             5338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc53083c.txt
_cod_data_source_block           mg13
_cod_original_cell_volume        4667.93(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1513849
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pt1 Pt 0.0000 0.272494(11) 0.2500 0.01216(7) Uani 1 2 d S
Cl1 Cl 0.0000 0.45393(8) 0.2500 0.0173(2) Uani 1 2 d S
P1 P 0.08919(3) 0.28065(6) 0.39287(6) 0.01304(16) Uani 1 1 d .
N1 N 0.02669(10) 0.04529(19) 0.32632(17) 0.0135(5) Uani 1 1 d .
N2 N 0.0000 0.1086(3) 0.2500 0.0126(7) Uani 1 2 d S
C1 C 0.14735(12) 0.3470(3) 0.3876(2) 0.0170(6) Uani 1 1 d .
C2 C 0.15798(14) 0.4546(3) 0.4116(2) 0.0229(7) Uani 1 1 d .
H2 H 0.1342 0.4930 0.4290 0.028 Uiso 1 1 calc R
C3 C 0.20331(14) 0.5055(3) 0.4099(3) 0.0273(7) Uani 1 1 d .
H3 H 0.2103 0.5788 0.4257 0.033 Uiso 1 1 calc R
C4 C 0.23844(14) 0.4497(3) 0.3854(2) 0.0266(7) Uani 1 1 d .
H4 H 0.2700 0.4843 0.3858 0.032 Uiso 1 1 calc R
C5 C 0.22759(14) 0.3438(3) 0.3604(3) 0.0273(7) Uani 1 1 d .
H5 H 0.2514 0.3061 0.3427 0.033 Uiso 1 1 calc R
C6 C 0.18200(15) 0.2916(3) 0.3608(3) 0.0243(7) Uani 1 1 d .
H6 H 0.1746 0.2189 0.3430 0.029 Uiso 1 1 calc R
C7 C 0.08836(13) 0.3400(2) 0.4952(2) 0.0172(6) Uani 1 1 d .
C8 C 0.03748(15) 0.3612(3) 0.4939(2) 0.0247(7) Uani 1 1 d .
H8 H 0.0013 0.3512 0.4359 0.030 Uiso 1 1 calc R
C9 C 0.03919(16) 0.3970(3) 0.5772(3) 0.0301(8) Uani 1 1 d .
H9 H 0.0041 0.4118 0.5758 0.036 Uiso 1 1 calc R
C10 C 0.09173(18) 0.4111(3) 0.6621(3) 0.0304(8) Uani 1 1 d .
H10 H 0.0927 0.4351 0.7191 0.036 Uiso 1 1 calc R
C11 C 0.14237(17) 0.3905(3) 0.6641(3) 0.0319(8) Uani 1 1 d .
H11 H 0.1784 0.4003 0.7225 0.038 Uiso 1 1 calc R
C12 C 0.14129(15) 0.3554(3) 0.5812(2) 0.0249(7) Uani 1 1 d .
H12 H 0.1765 0.3418 0.5828 0.030 Uiso 1 1 calc R
C13 C 0.11345(13) 0.1466(2) 0.4378(2) 0.0183(6) Uani 1 1 d .
H13A H 0.1292 0.1122 0.4007 0.022 Uiso 1 1 calc R
H13B H 0.1443 0.1487 0.5070 0.022 Uiso 1 1 calc R
C14 C 0.06131(13) 0.0842(3) 0.4257(2) 0.0181(6) Uani 1 1 d .
H14A H 0.0748 0.0235 0.4713 0.022 Uiso 1 1 calc R
H14B H 0.0373 0.1306 0.4410 0.022 Uiso 1 1 calc R
C15 C 0.01764(12) -0.0577(2) 0.3000(2) 0.0156(6) Uani 1 1 d .
C16 C 0.04013(14) -0.1539(2) 0.3614(2) 0.0195(6) Uani 1 1 d .
H16A H 0.0194 -0.1656 0.3968 0.023 Uiso 1 1 calc R
H16B H 0.0819 -0.1455 0.4094 0.023 Uiso 1 1 calc R
C17 C 0.03053(17) -0.2486(3) 0.2942(3) 0.0259(8) Uani 1 1 d .
H17A H 0.0590 -0.2453 0.2726 0.031 Uiso 1 1 calc R
H17B H 0.0370 -0.3156 0.3306 0.031 Uiso 1 1 calc R
S1 S 0.38641(3) 0.50717(7) 0.32245(6) 0.02190(17) Uani 1 1 d .
F1 F 0.31097(12) 0.3530(2) 0.2510(2) 0.0576(7) Uani 1 1 d .
F2 F 0.34402(12) 0.4020(3) 0.15983(19) 0.0605(8) Uani 1 1 d .
F3 F 0.28213(10) 0.4983(2) 0.17070(18) 0.0526(7) Uani 1 1 d .
O1 O 0.43062(11) 0.4278(2) 0.37046(19) 0.0372(7) Uani 1 1 d .
O2 O 0.35988(11) 0.5415(2) 0.37594(18) 0.0308(6) Uani 1 1 d .
O3 O 0.40005(11) 0.5901(2) 0.27563(19) 0.0352(6) Uani 1 1 d .
C18 C 0.32780(17) 0.4367(3) 0.2208(3) 0.0341(8) Uani 1 1 d .
Cl3 Cl 0.10749(5) 0.34507(11) 0.05662(10) 0.0577(3) Uani 1 1 d .
Cl2 Cl 0.19678(5) 0.24107(9) 0.03500(9) 0.0400(2) Uani 1 1 d .
C19 C 0.17452(19) 0.2802(3) 0.1171(3) 0.0335(9) Uani 1 1 d .
H19A H 0.1716 0.2168 0.1508 0.040 Uiso 1 1 calc R
H19B H 0.2039 0.3283 0.1666 0.040 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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'
Pt Pt -1.7033 8.3905 '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
_geom_angle_site_symmetry_3
N2 Pt1 Cl1 180.0 . .
N2 Pt1 P1 92.535(18) . .
Cl1 Pt1 P1 87.465(18) . .
N2 Pt1 P1 92.535(18) . 2
Cl1 Pt1 P1 87.465(18) . 2
P1 Pt1 P1 174.93(4) . 2
C1 P1 C7 105.21(14) . .
C1 P1 C13 107.64(14) . .
C7 P1 C13 100.98(14) . .
C1 P1 Pt1 117.00(10) . .
C7 P1 Pt1 115.33(10) . .
C13 P1 Pt1 109.28(10) . .
N2 N1 C15 111.3(2) . .
N2 N1 C14 123.4(2) . .
C15 N1 C14 125.3(2) . .
N1 N2 N1 106.0(3) . 2
N1 N2 Pt1 127.01(17) . .
N1 N2 Pt1 127.01(17) 2 .
C6 C1 C2 119.6(3) . .
C6 C1 P1 120.8(3) . .
C2 C1 P1 119.6(2) . .
C3 C2 C1 120.0(3) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C4 C3 C2 120.2(3) . .
C4 C3 H3 119.9 . .
C2 C3 H3 119.9 . .
C5 C4 C3 119.9(3) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 C6 120.7(3) . .
C4 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C5 C6 C1 119.5(3) . .
C5 C6 H6 120.2 . .
C1 C6 H6 120.2 . .
C8 C7 C12 119.2(3) . .
C8 C7 P1 122.3(2) . .
C12 C7 P1 118.2(2) . .
C7 C8 C9 120.1(3) . .
C7 C8 H8 120.0 . .
C9 C8 H8 120.0 . .
C10 C9 C8 120.3(3) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C11 C10 C9 120.0(3) . .
C11 C10 H10 120.0 . .
C9 C10 H10 120.0 . .
C10 C11 C12 120.3(3) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
C11 C12 C7 120.1(3) . .
C11 C12 H12 119.9 . .
C7 C12 H12 119.9 . .
C14 C13 P1 107.8(2) . .
C14 C13 H13A 110.1 . .
P1 C13 H13A 110.1 . .
C14 C13 H13B 110.1 . .
P1 C13 H13B 110.1 . .
H13A C13 H13B 108.5 . .
N1 C14 C13 110.1(2) . .
N1 C14 H14A 109.7 . .
C13 C14 H14A 109.7 . .
N1 C14 H14B 109.7 . .
C13 C14 H14B 109.7 . .
H14A C14 H14B 108.2 . .
N1 C15 C15 105.67(16) . 2
N1 C15 C16 129.2(3) . .
C15 C15 C16 125.14(17) 2 .
C15 C16 C17 107.6(3) . .
C15 C16 H16A 110.2 . .
C17 C16 H16A 110.2 . .
C15 C16 H16B 110.2 . .
C17 C16 H16B 110.2 . .
H16A C16 H16B 108.5 . .
C17 C17 C16 111.6(3) 2 .
C17 C17 H17A 109.3 2 .
C16 C17 H17A 109.3 . .
C17 C17 H17B 109.3 2 .
C16 C17 H17B 109.3 . .
H17A C17 H17B 108.0 . .
O2 S1 O1 114.59(15) . .
O2 S1 O3 115.51(17) . .
O1 S1 O3 115.00(16) . .
O2 S1 C18 102.50(16) . .
O1 S1 C18 103.98(19) . .
O3 S1 C18 102.76(17) . .
F3 C18 F2 107.2(3) . .
F3 C18 F1 107.7(3) . .
F2 C18 F1 107.9(4) . .
F3 C18 S1 111.6(3) . .
F2 C18 S1 111.1(3) . .
F1 C18 S1 111.1(3) . .
Cl3 C19 Cl2 111.1(2) . .
Cl3 C19 H19A 109.4 . .
Cl2 C19 H19A 109.4 . .
Cl3 C19 H19B 109.4 . .
Cl2 C19 H19B 109.4 . .
H19A C19 H19B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 N2 2.064(4) .
Pt1 Cl1 2.2847(10) .
Pt1 P1 2.3230(8) .
Pt1 P1 2.3230(8) 2
P1 C1 1.812(3) .
P1 C7 1.815(3) .
P1 C13 1.821(3) .
N1 N2 1.323(3) .
N1 C15 1.347(4) .
N1 C14 1.460(4) .
N2 N1 1.323(3) 2
C1 C6 1.395(4) .
C1 C2 1.398(5) .
C2 C3 1.388(5) .
C2 H2 0.9500 .
C3 C4 1.386(5) .
C3 H3 0.9500 .
C4 C5 1.379(6) .
C4 H4 0.9500 .
C5 C6 1.394(5) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.382(5) .
C7 C12 1.400(4) .
C8 C9 1.389(5) .
C8 H8 0.9500 .
C9 C10 1.385(5) .
C9 H9 0.9500 .
C10 C11 1.370(5) .
C10 H10 0.9500 .
C11 C12 1.388(5) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.529(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C15 1.386(6) 2
C15 C16 1.482(4) .
C16 C17 1.539(5) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C17 1.525(8) 2
C17 H17A 0.9900 .
C17 H17B 0.9900 .
S1 O2 1.434(2) .
S1 O1 1.438(3) .
S1 O3 1.439(3) .
S1 C18 1.817(4) .
F1 C18 1.332(5) .
F2 C18 1.332(4) .
F3 C18 1.322(5) .
Cl3 C19 1.751(4) .
Cl2 C19 1.772(4) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
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_4
N2 Pt1 P1 C1 119.68(12) . .
Cl1 Pt1 P1 C1 -60.32(12) . .
N2 Pt1 P1 C7 -115.78(11) . .
Cl1 Pt1 P1 C7 64.22(11) . .
N2 Pt1 P1 C13 -2.89(11) . .
Cl1 Pt1 P1 C13 177.11(11) . .
C15 N1 N2 N1 0.18(15) . 2
C14 N1 N2 N1 -179.8(3) . 2
C15 N1 N2 Pt1 -179.82(15) . .
C14 N1 N2 Pt1 0.2(3) . .
P1 Pt1 N2 N1 26.89(13) . .
P1 Pt1 N2 N1 -153.11(13) 2 .
P1 Pt1 N2 N1 -153.11(13) . 2
P1 Pt1 N2 N1 26.89(13) 2 2
C7 P1 C1 C6 143.8(3) . .
C13 P1 C1 C6 36.7(3) . .
Pt1 P1 C1 C6 -86.7(3) . .
C7 P1 C1 C2 -35.6(3) . .
C13 P1 C1 C2 -142.7(3) . .
Pt1 P1 C1 C2 93.9(3) . .
C6 C1 C2 C3 -0.9(5) . .
P1 C1 C2 C3 178.5(3) . .
C1 C2 C3 C4 -0.6(5) . .
C2 C3 C4 C5 1.5(5) . .
C3 C4 C5 C6 -0.9(5) . .
C4 C5 C6 C1 -0.5(5) . .
C2 C1 C6 C5 1.4(5) . .
P1 C1 C6 C5 -178.0(3) . .
C1 P1 C7 C8 141.7(3) . .
C13 P1 C7 C8 -106.4(3) . .
Pt1 P1 C7 C8 11.2(3) . .
C1 P1 C7 C12 -44.3(3) . .
C13 P1 C7 C12 67.6(3) . .
Pt1 P1 C7 C12 -174.8(2) . .
C12 C7 C8 C9 -0.2(5) . .
P1 C7 C8 C9 173.7(3) . .
C7 C8 C9 C10 -0.4(5) . .
C8 C9 C10 C11 0.5(6) . .
C9 C10 C11 C12 0.0(6) . .
C10 C11 C12 C7 -0.5(6) . .
C8 C7 C12 C11 0.6(5) . .
P1 C7 C12 C11 -173.5(3) . .
C1 P1 C13 C14 -170.2(2) . .
C7 P1 C13 C14 79.8(2) . .
Pt1 P1 C13 C14 -42.2(2) . .
N2 N1 C14 C13 -63.4(3) . .
C15 N1 C14 C13 116.6(3) . .
P1 C13 C14 N1 81.9(3) . .
N2 N1 C15 C15 -0.4(4) . 2
C14 N1 C15 C15 179.6(3) . 2
N2 N1 C15 C16 178.7(3) . .
C14 N1 C15 C16 -1.3(5) . .
N1 C15 C16 C17 -165.0(3) . .
C15 C15 C16 C17 14.0(5) 2 .
C15 C16 C17 C17 -46.6(4) . 2
O2 S1 C18 F3 57.8(3) . .
O1 S1 C18 F3 177.4(3) . .
O3 S1 C18 F3 -62.4(3) . .
O2 S1 C18 F2 177.5(3) . .
O1 S1 C18 F2 -62.9(3) . .
O3 S1 C18 F2 57.3(3) . .
O2 S1 C18 F1 -62.4(3) . .
O1 S1 C18 F1 57.2(3) . .
O3 S1 C18 F1 177.4(3) . .
