#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:11:22 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180127 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/25/7102514.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_7102514
loop_
_publ_author_name
'Ortega, Esteban'
'Pirio, Nadine'
'Meunier, Philippe'
'Donnadieu, Bruno'
_publ_section_title
;
 Isolation, dynamic NMR study and X-ray characterisation of a bis
 sulfonium zirconocene-ate dimer.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              678
_journal_page_last               679
_journal_paper_doi               10.1039/b312954c
_journal_year                    2004
_chemical_formula_sum            'C31 H27 P S Zr'
_chemical_formula_weight         553.78
_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                90.0
_cell_angle_beta                 98.21(1)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   15.724(2)
_cell_length_b                   10.3050(6)
_cell_length_c                   15.826(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.3
_cell_volume                     2538.0(17)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       φ
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19651
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  3
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0332
_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)+(0.0519P)²+0.3535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                4014
_reflns_number_total             4985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b312954c.txt
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      ' P 21/c'
_cod_database_code               7102514
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
Zr1 Zr 0.572833(14) 0.15605(2) 0.085682(15) 0.02805(9) Uani 1 1 d .
S1 S 0.57758(4) -0.03402(7) -0.01903(6) 0.0477(2) Uani 1 1 d .
P1 P 0.80680(4) 0.21146(7) 0.13027(4) 0.03643(16) Uani 1 1 d .
C1 C 0.71988(16) 0.1100(3) 0.07247(16) 0.0343(5) Uani 1 1 d .
C2 C 0.74451(18) 0.0018(3) 0.03515(18) 0.0415(6) Uani 1 1 d .
C3 C 0.68619(18) -0.0976(3) -0.0128(2) 0.0426(6) Uani 1 1 d .
C4 C 0.70900(16) -0.1218(3) -0.1008(2) 0.0432(7) Uani 1 1 d .
C5 C 0.7264(2) -0.2458(4) -0.1263(3) 0.0599(9) Uani 1 1 d .
H5 H 0.7241 -0.3152 -0.0891 0.072 Uiso 1 1 calc R
C6 C 0.7477(2) -0.2674(5) -0.2083(3) 0.0847(16) Uani 1 1 d .
H6 H 0.7589 -0.3509 -0.2260 0.102 Uiso 1 1 calc R
C7 C 0.7517(3) -0.1621(5) -0.2628(3) 0.0782(14) Uani 1 1 d .
H7 H 0.7652 -0.1754 -0.3175 0.094 Uiso 1 1 calc R
C8 C 0.7359(2) -0.0401(5) -0.2363(2) 0.0627(10) Uani 1 1 d .
H8 H 0.7394 0.0299 -0.2727 0.075 Uiso 1 1 calc R
C9 C 0.71488(18) -0.0197(3) -0.1561(2) 0.0475(7) Uani 1 1 d .
H9 H 0.7044 0.0643 -0.1387 0.057 Uiso 1 1 calc R
C10 C 0.64914(19) 0.0953(4) 0.23196(17) 0.0473(7) Uani 1 1 d .
H10 H 0.7087 0.0875 0.2387 0.057 Uiso 1 1 calc R
C11 C 0.6005(4) 0.2099(4) 0.24111(19) 0.0809(15) Uani 1 1 d .
H11 H 0.6220 0.2922 0.2558 0.097 Uiso 1 1 calc R
C12 C 0.5141(3) 0.1738(6) 0.2235(3) 0.0882(18) Uani 1 1 d .
H12 H 0.4673 0.2292 0.2229 0.106 Uiso 1 1 calc R
C13 C 0.5099(2) 0.0499(6) 0.2080(3) 0.0843(17) Uani 1 1 d .
H13 H 0.4591 0.0030 0.1964 0.101 Uiso 1 1 calc R
C14 C 0.5894(2) -0.0018(3) 0.2111(2) 0.0514(8) Uani 1 1 d .
H14 H 0.6017 -0.0882 0.2009 0.062 Uiso 1 1 calc R
C15 C 0.60270(19) 0.3224(3) -0.02448(18) 0.0421(6) Uani 1 1 d .
H15 H 0.6416 0.3020 -0.0615 0.051 Uiso 1 1 calc R
C16 C 0.62233(18) 0.3818(3) 0.05515(19) 0.0402(6) Uani 1 1 d .
H16 H 0.6768 0.4062 0.0811 0.048 Uiso 1 1 calc R
C17 C 0.5457(2) 0.3982(3) 0.08902(18) 0.0425(6) Uani 1 1 d .
H17 H 0.5398 0.4383 0.1405 0.051 Uiso 1 1 calc R
C18 C 0.47981(18) 0.3439(3) 0.0319(2) 0.0433(7) Uani 1 1 d .
H18 H 0.4223 0.3381 0.0392 0.052 Uiso 1 1 calc R
C19 C 0.5158(2) 0.2996(3) -0.03857(18) 0.0442(7) Uani 1 1 d .
H19 H 0.4859 0.2609 -0.0870 0.053 Uiso 1 1 calc R
C111 C 0.90321(17) 0.1068(3) 0.14186(17) 0.0392(6) Uani 1 1 d .
C112 C 0.9042(2) -0.0015(4) 0.1936(2) 0.0552(8) Uani 1 1 d .
H112 H 0.8560 -0.0194 0.2196 0.066 Uiso 1 1 calc R
C113 C 0.9739(2) -0.0841(4) 0.2083(2) 0.0608(9) Uani 1 1 d .
H113 H 0.9719 -0.1574 0.2422 0.073 Uiso 1 1 calc R
C114 C 1.0465(2) -0.0566(4) 0.1722(2) 0.0585(9) Uani 1 1 d .
H114 H 1.0942 -0.1108 0.1815 0.070 Uiso 1 1 calc R
C115 C 1.0475(2) 0.0516(4) 0.1224(2) 0.0642(10) Uani 1 1 d .
H115 H 1.0967 0.0710 0.0985 0.077 Uiso 1 1 calc R
C116 C 0.97695(18) 0.1330(3) 0.1067(2) 0.0500(7) Uani 1 1 d .
H116 H 0.9792 0.2057 0.0722 0.060 Uiso 1 1 calc R
C121 C 0.83432(17) 0.3265(3) 0.04985(19) 0.0405(6) Uani 1 1 d .
C122 C 0.83202(19) 0.2952(3) -0.0362(2) 0.0480(7) Uani 1 1 d .
H122 H 0.8129 0.2136 -0.0556 0.058 Uiso 1 1 calc R
C123 C 0.8578(2) 0.3838(4) -0.0932(2) 0.0588(9) Uani 1 1 d .
H123 H 0.8563 0.3617 -0.1503 0.071 Uiso 1 1 calc R
C124 C 0.8858(2) 0.5052(4) -0.0646(3) 0.0645(10) Uani 1 1 d .
H124 H 0.9030 0.5650 -0.1028 0.077 Uiso 1 1 calc R
C125 C 0.8885(2) 0.5383(4) 0.0197(3) 0.0615(9) Uani 1 1 d .
H125 H 0.9074 0.6204 0.0383 0.074 Uiso 1 1 calc R
C126 C 0.86315(19) 0.4496(3) 0.0772(2) 0.0511(7) Uani 1 1 d .
H126 H 0.8654 0.4724 0.1343 0.061 Uiso 1 1 calc R
H2 H 0.806(2) -0.018(3) 0.033(2) 0.048(8) Uiso 1 1 d .
H3 H 0.685(2) -0.183(4) 0.019(2) 0.050(9) Uiso 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'
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'
Zr Zr -2.9673 0.5597 '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_3
C1 Zr1 C12 124.94(13) .
C1 Zr1 C11 95.44(15) .
C12 Zr1 C11 32.55(16) .
C1 Zr1 C18 130.36(9) .
C12 Zr1 C18 88.26(12) .
C11 Zr1 C18 100.07(13) .
C1 Zr1 C19 106.74(10) .
C12 Zr1 C19 120.29(12) .
C11 Zr1 C19 129.07(12) .
C18 Zr1 C19 32.30(10) .
C1 Zr1 C16 80.68(9) .
C12 Zr1 C16 105.25(18) .
C11 Zr1 C16 88.19(11) .
C18 Zr1 C16 53.30(9) .
C19 Zr1 C16 52.73(9) .
C1 Zr1 C10 72.15(9) .
C12 Zr1 C10 53.44(12) .
C11 Zr1 C10 32.94(13) .
C18 Zr1 C10 132.95(11) .
C19 Zr1 C10 158.22(11) .
C16 Zr1 C10 106.54(10) .
C1 Zr1 C17 111.35(10) .
C12 Zr1 C17 79.93(15) .
C11 Zr1 C17 76.52(11) .
C18 Zr1 C17 32.09(10) .
C19 Zr1 C17 52.86(10) .
C16 Zr1 C17 32.09(10) .
C10 Zr1 C17 106.51(11) .
C1 Zr1 C15 78.38(9) .
C12 Zr1 C15 132.82(16) .
C11 Zr1 C15 120.21(12) .
C18 Zr1 C15 53.09(9) .
C19 Zr1 C15 31.49(10) .
C16 Zr1 C15 32.03(10) .
C10 Zr1 C15 133.34(10) .
C17 Zr1 C15 52.89(9) .
C1 Zr1 C13 117.75(11) .
C12 Zr1 C13 29.88(17) .
C11 Zr1 C13 51.55(16) .
C18 Zr1 C13 108.66(13) .
C19 Zr1 C13 135.44(12) .
C16 Zr1 C13 134.96(17) .
C10 Zr1 C13 51.83(11) .
C17 Zr1 C13 108.83(16) .
C15 Zr1 C13 160.75(15) .
C1 Zr1 C14 87.06(10) .
C12 Zr1 C14 51.37(14) .
C11 Zr1 C14 52.52(12) .
C18 Zr1 C14 138.46(11) .
C19 Zr1 C14 165.18(10) .
C16 Zr1 C14 137.50(10) .
C10 Zr1 C14 31.50(10) .
C17 Zr1 C14 127.65(10) .
C15 Zr1 C14 163.24(10) .
C13 Zr1 C14 30.81(12) .
C1 Zr1 S1 71.12(7) .
C12 Zr1 S1 131.86(17) .
C11 Zr1 S1 141.81(9) .
C18 Zr1 S1 116.03(8) .
C19 Zr1 S1 89.08(8) .
C16 Zr1 S1 122.73(8) .
C10 Zr1 S1 110.32(9) .
C17 Zr1 S1 141.58(7) .
C15 Zr1 S1 92.68(8) .
C13 Zr1 S1 102.30(16) .
C14 Zr1 S1 90.38(9) .
C3 S1 Zr1 110.63(10) .
C3 S1 Zr1 127.25(10) 3_655
Zr1 S1 Zr1 119.49(3) 3_655
C121 P1 C111 100.04(13) .
C121 P1 C1 104.60(13) .
C111 P1 C1 104.86(13) .
C2 C1 P1 116.5(2) .
C2 C1 Zr1 123.0(2) .
P1 C1 Zr1 119.81(13) .
C1 C2 C3 126.3(3) .
C1 C2 H2 122.2(19) .
C3 C2 H2 111.3(19) .
C2 C3 C4 111.7(2) .
C2 C3 S1 106.39(19) .
C4 C3 S1 110.8(2) .
C2 C3 H3 113.1(19) .
C4 C3 H3 109.6(19) .
S1 C3 H3 105.1(18) .
C5 C4 C9 119.2(3) .
C5 C4 C3 120.4(3) .
C9 C4 C3 120.4(3) .
C4 C5 C6 120.1(4) .
C4 C5 H5 120.0 .
C6 C5 H5 120.0 .
C7 C6 C5 119.2(4) .
C7 C6 H6 120.4 .
C5 C6 H6 120.4 .
C8 C7 C6 120.2(4) .
C8 C7 H7 119.9 .
C6 C7 H7 119.9 .
C7 C8 C9 120.4(4) .
C7 C8 H8 119.8 .
C9 C8 H8 119.8 .
C8 C9 C4 121.1(3) .
C8 C9 H9 119.5 .
C4 C9 H9 119.5 .
C14 C10 C11 105.6(3) .
C14 C10 Zr1 75.09(17) .
C11 C10 Zr1 72.33(18) .
C14 C10 H10 127.2 .
C11 C10 H10 127.2 .
Zr1 C10 H10 117.6 .
C12 C11 C10 106.2(4) .
C12 C11 Zr1 73.5(2) .
C10 C11 Zr1 74.73(17) .
C12 C11 H11 126.9 .
C10 C11 H11 126.9 .
Zr1 C11 H11 117.1 .
C13 C12 C11 108.7(4) .
C13 C12 Zr1 77.2(2) .
C11 C12 Zr1 73.92(19) .
C13 C12 H12 125.7 .
C11 C12 H12 125.7 .
Zr1 C12 H12 115.3 .
C12 C13 C14 111.0(4) .
C12 C13 Zr1 72.9(2) .
C14 C13 Zr1 74.87(19) .
C12 C13 H13 124.5 .
C14 C13 H13 124.5 .
Zr1 C13 H13 119.3 .
C13 C14 C10 108.5(4) .
C13 C14 Zr1 74.31(19) .
C10 C14 Zr1 73.41(17) .
C13 C14 H14 125.8 .
C10 C14 H14 125.8 .
Zr1 C14 H14 118.4 .
C19 C15 C16 108.0(2) .
C19 C15 Zr1 73.62(16) .
C16 C15 Zr1 73.41(16) .
C19 C15 H15 126.0 .
C16 C15 H15 126.0 .
Zr1 C15 H15 118.9 .
C15 C16 C17 107.9(3) .
C15 C16 Zr1 74.56(16) .
C17 C16 Zr1 74.43(16) .
C15 C16 H16 126.0 .
C17 C16 H16 126.0 .
Zr1 C16 H16 117.0 .
C18 C17 C16 107.7(3) .
C18 C17 Zr1 72.66(16) .
C16 C17 Zr1 73.48(15) .
C18 C17 H17 126.1 .
C16 C17 H17 126.1 .
Zr1 C17 H17 119.6 .
C17 C18 C19 107.5(3) .
C17 C18 Zr1 75.25(16) .
C19 C18 Zr1 74.62(16) .
C17 C18 H18 126.2 .
C19 C18 H18 126.2 .
Zr1 C18 H18 116.1 .
C15 C19 C18 108.8(3) .
C15 C19 Zr1 74.88(16) .
C18 C19 Zr1 73.08(16) .
C15 C19 H19 125.6 .
C18 C19 H19 125.6 .
Zr1 C19 H19 118.3 .
C116 C111 C112 117.2(3) .
C116 C111 P1 124.7(2) .
C112 C111 P1 118.0(2) .
C113 C112 C111 122.5(3) .
C113 C112 H112 118.7 .
C111 C112 H112 118.7 .
C114 C113 C112 119.3(3) .
C114 C113 H113 120.4 .
C112 C113 H113 120.4 .
C115 C114 C113 119.1(3) .
C115 C114 H114 120.5 .
C113 C114 H114 120.5 .
C114 C115 C116 121.5(3) .
C114 C115 H115 119.2 .
C116 C115 H115 119.2 .
C111 C116 C115 120.4(3) .
C111 C116 H116 119.8 .
C115 C116 H116 119.8 .
C122 C121 C126 118.3(3) .
C122 C121 P1 123.5(2) .
C126 C121 P1 118.1(2) .
C123 C122 C121 121.0(3) .
C123 C122 H122 119.5 .
C121 C122 H122 119.5 .
C124 C123 C122 119.6(3) .
C124 C123 H123 120.2 .
C122 C123 H123 120.2 .
C125 C124 C123 120.5(3) .
C125 C124 H124 119.7 .
C123 C124 H124 119.7 .
C124 C125 C126 120.1(4) .
C124 C125 H125 119.9 .
C126 C125 H125 119.9 .
C125 C126 C121 120.5(3) .
C125 C126 H126 119.8 .
C121 C126 H126 119.8 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 C1 2.399(3) .
Zr1 C12 2.494(3) .
Zr1 C11 2.498(3) .
Zr1 C18 2.501(3) .
Zr1 C19 2.521(3) .
Zr1 C16 2.522(3) .
Zr1 C10 2.530(3) .
Zr1 C17 2.534(3) .
Zr1 C15 2.536(3) .
Zr1 C13 2.544(3) .
Zr1 C14 2.551(3) .
Zr1 S1 2.5735(11) .
S1 C3 1.818(3) .
S1 Zr1 2.7524(10) 3_655
P1 C121 1.835(3) .
P1 C111 1.848(3) .
P1 C1 1.855(3) .
C1 C2 1.344(4) .
C2 C3 1.506(4) .
C2 H2 1.00(3) .
C3 C4 1.509(4) .
C3 H3 1.01(4) .
C4 C5 1.379(4) .
C4 C9 1.379(5) .
C5 C6 1.402(6) .
C5 H5 0.9300 .
C6 C7 1.394(7) .
C6 H6 0.9300 .
C7 C8 1.359(6) .
C7 H7 0.9300 .
C8 C9 1.373(5) .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 C14 1.379(5) .
C10 C11 1.426(6) .
C10 H10 0.9300 .
C11 C12 1.399(7) .
C11 H11 0.9300 .
C12 C13 1.299(7) .
C12 H12 0.9300 .
C13 C14 1.353(5) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C15 C19 1.372(4) .
C15 C16 1.395(4) .
C15 H15 0.9300 .
C16 C17 1.397(4) .
C16 H16 0.9300 .
C17 C18 1.392(4) .
C17 H17 0.9300 .
C18 C19 1.397(4) .
C18 H18 0.9300 .
C19 H19 0.9300 .
C111 C116 1.382(4) .
C111 C112 1.384(5) .
C112 C113 1.381(5) .
C112 H112 0.9300 .
C113 C114 1.377(5) .
C113 H113 0.9300 .
C114 C115 1.366(5) .
C114 H114 0.9300 .
C115 C116 1.385(5) .
C115 H115 0.9300 .
C116 H116 0.9300 .
C121 C122 1.395(4) .
C121 C126 1.396(4) .
C122 C123 1.384(5) .
C122 H122 0.9300 .
C123 C124 1.381(6) .
C123 H123 0.9300 .
C124 C125 1.372(6) .
C124 H124 0.9300 .
C125 C126 1.388(5) .
C125 H125 0.9300 .
C126 H126 0.9300 .
