#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:29:40 +0100 (vie 25 de mar de 2016) $
#$Revision: 179847 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/43/7014382.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_7014382
loop_
_publ_author_name
'Meinholz, Margret M.'
'Pandey, Sushil K.'
'Deuerlein, Stephan M.'
'Stalke, Dietmar'
_publ_section_title
;
 Access to new Janus head ligands: linking sulfur diimides and
 phosphanes for hemilabile tripodal scorpionates.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1662
_journal_page_last               1671
_journal_paper_doi               10.1039/c0dt00665c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C19 H31 N2 P S Si2'
_chemical_formula_weight         406.67
_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                 99.8430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9937(7)
_cell_length_b                   9.9367(6)
_cell_length_c                   18.1145(10)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.949
_cell_measurement_theta_min      2.595
_cell_volume                     2304.4(2)
_computing_cell_refinement       'SAINT v46A'
_computing_data_collection       'APEX2 v2.2-0'
_computing_data_reduction        'SAINT v46A'
_computing_molecular_graphics    'XSHELL v4.01'
_computing_publication_material  'XSHELL v4.01'
_computing_structure_refinement  'SHELXL in SHELXTL v2008/4'
_computing_structure_solution    'SHELXS in SHELXTL v2008/4'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker TXS Mo rotating anode'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_av_sigmaI/netI    0.0083
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43786
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.8590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5491
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0278
_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)+(0.0380P)²+1.0873P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                5259
_reflns_number_total             5491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00665C.TXT
_cod_data_source_block           p21n
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7014382
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.18064(9) 0.23395(12) -0.15557(7) 0.0245(2) Uani 1 1 d . . .
C2 C 0.24069(10) 0.12721(13) -0.17411(7) 0.0282(3) Uani 1 1 d . . .
H2 H 0.3031 0.1033 -0.1414 0.034 Uiso 1 1 calc R . .
C3 C 0.21013(11) 0.05492(15) -0.24034(8) 0.0342(3) Uani 1 1 d . . .
H3 H 0.2523 -0.0169 -0.2528 0.041 Uiso 1 1 calc R . .
C4 C 0.11859(12) 0.08754(17) -0.28789(8) 0.0381(3) Uani 1 1 d . . .
H4 H 0.0972 0.0374 -0.3325 0.046 Uiso 1 1 calc R . .
C5 C 0.05814(12) 0.19382(17) -0.27012(8) 0.0374(3) Uani 1 1 d . . .
H5 H -0.0050 0.2161 -0.3025 0.045 Uiso 1 1 calc R . .
C6 C 0.08939(10) 0.26754(14) -0.20537(7) 0.0311(3) Uani 1 1 d . . .
H6 H 0.0485 0.3419 -0.1945 0.037 Uiso 1 1 calc R . .
C7 C 0.31581(9) 0.23499(13) -0.01330(7) 0.0256(2) Uani 1 1 d . . .
C8 C 0.41939(10) 0.27605(16) -0.00750(8) 0.0344(3) Uani 1 1 d . . .
H8 H 0.4357 0.3541 -0.0335 0.041 Uiso 1 1 calc R . .
C9 C 0.49921(11) 0.20344(19) 0.03617(9) 0.0450(4) Uani 1 1 d . . .
H9 H 0.5697 0.2317 0.0392 0.054 Uiso 1 1 calc R . .
C10 C 0.47693(13) 0.09175(19) 0.07473(9) 0.0455(4) Uani 1 1 d . . .
H10 H 0.5318 0.0432 0.1047 0.055 Uiso 1 1 calc R . .
C11 C 0.37517(13) 0.04968(18) 0.07016(9) 0.0441(4) Uani 1 1 d . . .
H11 H 0.3596 -0.0277 0.0970 0.053 Uiso 1 1 calc R . .
C12 C 0.29491(11) 0.12096(15) 0.02603(8) 0.0354(3) Uani 1 1 d . . .
H12 H 0.2248 0.0911 0.0228 0.043 Uiso 1 1 calc R . .
C13 C 0.09890(8) 0.30418(12) -0.03031(7) 0.0219(2) Uani 1 1 d . . .
H13A H 0.0380 0.3470 -0.0620 0.026 Uiso 1 1 calc R . .
H13B H 0.0865 0.2059 -0.0310 0.026 Uiso 1 1 calc R . .
C14 C -0.00610(10) 0.06696(13) 0.11966(8) 0.0316(3) Uani 1 1 d . . .
H14A H -0.0296 0.0371 0.0680 0.047 Uiso 1 1 calc R . .
H14B H -0.0299 0.0028 0.1542 0.047 Uiso 1 1 calc R . .
H14C H 0.0704 0.0718 0.1298 0.047 Uiso 1 1 calc R . .
C15 C -0.02014(11) 0.29300(15) 0.23134(7) 0.0321(3) Uani 1 1 d . . .
H15A H 0.0563 0.2951 0.2433 0.048 Uiso 1 1 calc R . .
H15B H -0.0472 0.2305 0.2653 0.048 Uiso 1 1 calc R . .
H15C H -0.0478 0.3834 0.2373 0.048 Uiso 1 1 calc R . .
C16 C -0.20572(9) 0.23779(13) 0.10572(7) 0.0254(2) Uani 1 1 d . . .
H16A H -0.2300 0.3308 0.0974 0.038 Uiso 1 1 calc R . .
H16B H -0.2375 0.1975 0.1458 0.038 Uiso 1 1 calc R . .
H16C H -0.2259 0.1859 0.0595 0.038 Uiso 1 1 calc R . .
C17 C 0.35759(11) 0.5869(2) 0.09588(11) 0.0491(4) Uani 1 1 d . . .
H17A H 0.3856 0.4960 0.1064 0.074 Uiso 1 1 calc R . .
H17B H 0.4045 0.6525 0.1247 0.074 Uiso 1 1 calc R . .
H17C H 0.3520 0.6060 0.0423 0.074 Uiso 1 1 calc R . .
C18 C 0.23047(18) 0.5345(2) 0.21939(9) 0.0695(7) Uani 1 1 d . . .
H18A H 0.1610 0.5417 0.2333 0.104 Uiso 1 1 calc R . .
H18B H 0.2804 0.5879 0.2542 0.104 Uiso 1 1 calc R . .
H18C H 0.2525 0.4401 0.2217 0.104 Uiso 1 1 calc R . .
C19 C 0.18521(13) 0.77830(15) 0.11963(9) 0.0417(3) Uani 1 1 d . . .
H19A H 0.1787 0.8116 0.0681 0.063 Uiso 1 1 calc R . .
H19B H 0.2378 0.8314 0.1524 0.063 Uiso 1 1 calc R . .
H19C H 0.1178 0.7866 0.1366 0.063 Uiso 1 1 calc R . .
N1 N -0.01665(7) 0.34967(10) 0.07235(5) 0.01986(18) Uani 1 1 d D . .
H1 H -0.0571(11) 0.3869(15) 0.0362(8) 0.024 Uiso 1 1 d D . .
N2 N 0.13491(7) 0.51754(10) 0.05796(5) 0.02069(19) Uani 1 1 d . . .
P1 P 0.21729(2) 0.33885(3) -0.071450(18) 0.02381(8) Uani 1 1 d . . .
S1 S 0.10774(2) 0.36460(3) 0.064784(15) 0.01901(7) Uani 1 1 d . . .
Si1 Si -0.06140(2) 0.23621(3) 0.133005(17) 0.01848(8) Uani 1 1 d . . .
Si2 Si 0.22564(2) 0.59867(4) 0.122995(18) 0.02355(8) 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'
Si Si 0.0817 0.0704 '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'
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
_geom_angle_publ_flag
C2 C1 C6 118.27(12) . . ?
C2 C1 P1 123.72(10) . . ?
C6 C1 P1 117.94(10) . . ?
C1 C2 C3 120.71(12) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C4 C3 C2 120.17(14) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.68(14) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 120.28(13) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 120.85(13) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C12 C7 C8 118.10(12) . . ?
C12 C7 P1 125.15(10) . . ?
C8 C7 P1 116.73(11) . . ?
C7 C8 C9 120.46(15) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C10 C9 C8 120.52(14) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.05(14) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 C12 119.82(16) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C7 C12 C11 121.04(14) . . ?
C7 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
S1 C13 P1 113.54(6) . . ?
S1 C13 H13A 108.9 . . ?
P1 C13 H13A 108.9 . . ?
S1 C13 H13B 108.9 . . ?
P1 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
S1 N1 Si1 123.18(6) . . ?
S1 N1 H1 112.4(10) . . ?
Si1 N1 H1 122.6(10) . . ?
S1 N2 Si2 122.50(6) . . ?
C7 P1 C1 102.33(6) . . ?
C7 P1 C13 102.17(6) . . ?
C1 P1 C13 96.47(5) . . ?
N2 S1 N1 109.26(5) . . ?
N2 S1 C13 102.99(5) . . ?
N1 S1 C13 98.36(5) . . ?
N1 Si1 C16 104.92(5) . . ?
N1 Si1 C15 109.59(6) . . ?
C16 Si1 C15 111.45(6) . . ?
N1 Si1 C14 108.97(5) . . ?
C16 Si1 C14 111.60(6) . . ?
C15 Si1 C14 110.15(7) . . ?
N2 Si2 C18 113.21(7) . . ?
N2 Si2 C19 105.73(6) . . ?
C18 Si2 C19 109.00(10) . . ?
N2 Si2 C17 110.10(6) . . ?
C18 Si2 C17 110.02(10) . . ?
C19 Si2 C17 108.60(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3915(18) . ?
C1 C6 1.4018(18) . ?
C1 P1 1.8404(13) . ?
C2 C3 1.3964(19) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.3898(19) . ?
C7 C8 1.3930(17) . ?
C7 P1 1.8310(13) . ?
C8 C9 1.393(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.368(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.376(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 S1 1.8092(12) . ?
C13 P1 1.8526(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 Si1 1.8607(13) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 Si1 1.8581(13) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 Si1 1.8559(12) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 Si2 1.8661(16) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 Si2 1.8498(16) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 Si2 1.8587(16) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
N1 S1 1.6520(9) . ?
N1 Si1 1.7421(10) . ?
N1 H1 0.850(13) . ?
N2 S1 1.5698(10) . ?
N2 Si2 1.7184(10) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.54(18) . . . . ?
P1 C1 C2 C3 -177.57(10) . . . . ?
C1 C2 C3 C4 -1.0(2) . . . . ?
C2 C3 C4 C5 1.1(2) . . . . ?
C3 C4 C5 C6 0.4(2) . . . . ?
C4 C5 C6 C1 -1.9(2) . . . . ?
C2 C1 C6 C5 1.98(18) . . . . ?
P1 C1 C6 C5 179.19(10) . . . . ?
C12 C7 C8 C9 0.5(2) . . . . ?
P1 C7 C8 C9 179.43(11) . . . . ?
C7 C8 C9 C10 -0.8(2) . . . . ?
C8 C9 C10 C11 0.5(2) . . . . ?
C9 C10 C11 C12 0.1(2) . . . . ?
C8 C7 C12 C11 0.1(2) . . . . ?
P1 C7 C12 C11 -178.70(11) . . . . ?
C10 C11 C12 C7 -0.4(2) . . . . ?
C12 C7 P1 C1 -75.07(12) . . . . ?
C8 C7 P1 C1 106.11(10) . . . . ?
C12 C7 P1 C13 24.43(13) . . . . ?
C8 C7 P1 C13 -154.39(10) . . . . ?
C2 C1 P1 C7 -17.45(11) . . . . ?
C6 C1 P1 C7 165.51(9) . . . . ?
C2 C1 P1 C13 -121.45(11) . . . . ?
C6 C1 P1 C13 61.51(10) . . . . ?
S1 C13 P1 C7 65.67(7) . . . . ?
S1 C13 P1 C1 169.81(7) . . . . ?
Si2 N2 S1 N1 118.05(7) . . . . ?
Si2 N2 S1 C13 -138.14(7) . . . . ?
Si1 N1 S1 N2 -139.35(7) . . . . ?
Si1 N1 S1 C13 113.67(7) . . . . ?
P1 C13 S1 N2 54.81(7) . . . . ?
P1 C13 S1 N1 166.90(6) . . . . ?
S1 N1 Si1 C16 -169.28(7) . . . . ?
S1 N1 Si1 C15 70.96(9) . . . . ?
S1 N1 Si1 C14 -49.64(9) . . . . ?
S1 N2 Si2 C18 -33.31(13) . . . . ?
S1 N2 Si2 C19 -152.57(8) . . . . ?
S1 N2 Si2 C17 90.31(10) . . . . ?
