#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:30:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180265 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/51/7115118.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_7115118
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Nixon, John F.'
'Sakarya, Nurgün'
_publ_section_title
;
 Syntheses of the novel cage compounds P3Se3C3But3 and P3Se4C3But3 and an
 unusual insertion reaction of [PtCl2(PMe3)] into the Se--Se bond of the
 latter to give the six-coordinate Pt(iv) complex [PtCl2(PMe3)P3Se4C3But3]
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1745
_journal_paper_doi               10.1039/b005123n
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C15 H27 P3 Se3'
_chemical_formula_structural     'C15 H27 P3 Se3'
_chemical_formula_sum            'C15 H27 P3 Se3'
_chemical_formula_weight         537.16
_chemical_name_common            '[(CtBu)3P3Se3]'
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-09-07T12:21:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.264(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7751(3)
_cell_length_b                   16.2798(7)
_cell_length_c                   11.6992(3)
_cell_measurement_reflns_used    9479
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      4.076
_cell_measurement_wavelength     0.71073
_cell_volume                     2005.40(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor  1997)''
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor  1997)''
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia,  1997)''
_computing_publication_material
'WinGX publication routines (Farrugia,  1999)''
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16312
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         4.84
_exptl_absorpt_coefficient_mu    5.734
_exptl_absorpt_correction_T_max  0.5386
_exptl_absorpt_correction_T_min  0.3897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         5787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0344P)²+1.1175P] where  P=(Fo²+2Fc²)/3''
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                4569
_reflns_number_total             5787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005123n.txt
_cod_data_source_block           JFN-4
_cod_original_cell_volume        2005.40(11)
_cod_original_sg_symbol_H-M      P2(1)/N
_cod_database_code               7115118
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
Se1 Se 0.06806(3) 0.146682(19) 0.90146(2) 0.03500(9) Uani 1 1 d .
Se2 Se -0.05525(3) 0.136789(19) 0.49306(2) 0.03535(9) Uani 1 1 d .
Se3 Se -0.25352(3) 0.26005(2) 0.65996(3) 0.04375(10) Uani 1 1 d .
P1 P 0.09391(7) 0.09089(4) 0.65119(6) 0.02940(15) Uani 1 1 d .
P2 P -0.07921(6) 0.20573(4) 0.65571(6) 0.02643(14) Uani 1 1 d .
P3 P 0.18405(6) 0.23767(5) 0.82563(6) 0.03042(15) Uani 1 1 d .
C1 C 0.0767(2) 0.26274(16) 0.6837(2) 0.0266(5) Uani 1 1 d .
C2 C 0.1778(2) 0.19336(16) 0.6782(2) 0.0266(5) Uani 1 1 d .
C3 C -0.0259(2) 0.11374(17) 0.7438(2) 0.0272(5) Uani 1 1 d .
C4 C 0.0654(3) 0.35522(17) 0.6434(3) 0.0373(6) Uani 1 1 d .
C5 C -0.0111(4) 0.3633(2) 0.5177(3) 0.0541(9) Uani 1 1 d .
H5A H -0.0918 0.3365 0.5109 0.081 Uiso 1 1 calc R
H5B H 0.0348 0.338 0.4651 0.081 Uiso 1 1 calc R
H5C H -0.0244 0.4203 0.4982 0.081 Uiso 1 1 calc R
C6 C 0.0010(4) 0.4023(2) 0.7295(4) 0.0582(9) Uani 1 1 d .
H6A H -0.0804 0.3783 0.7292 0.087 Uiso 1 1 calc R
H6B H -0.01 0.4588 0.7059 0.087 Uiso 1 1 calc R
H6C H 0.0532 0.3992 0.8068 0.087 Uiso 1 1 calc R
C7 C 0.1933(3) 0.3980(2) 0.6505(3) 0.0500(8) Uani 1 1 d .
H7A H 0.2433 0.3936 0.7286 0.075 Uiso 1 1 calc R
H7B H 0.1793 0.455 0.6303 0.075 Uiso 1 1 calc R
H7C H 0.2376 0.3724 0.5969 0.075 Uiso 1 1 calc R
C8 C 0.3015(3) 0.19341(19) 0.6266(2) 0.0348(6) Uani 1 1 d .
C9 C 0.2699(3) 0.2115(3) 0.4950(3) 0.0517(9) Uani 1 1 d .
H9A H 0.2311 0.2647 0.4817 0.078 Uiso 1 1 calc R
H9B H 0.2123 0.1706 0.4555 0.078 Uiso 1 1 calc R
H9C H 0.3465 0.2106 0.4655 0.078 Uiso 1 1 calc R
C10 C 0.4060(3) 0.2525(2) 0.6898(3) 0.0512(9) Uani 1 1 d .
H10A H 0.3746 0.3078 0.6822 0.077 Uiso 1 1 calc R
H10B H 0.4791 0.2482 0.6555 0.077 Uiso 1 1 calc R
H10C H 0.4292 0.2381 0.7712 0.077 Uiso 1 1 calc R
C11 C 0.3638(3) 0.1082(2) 0.6455(4) 0.0554(9) Uani 1 1 d .
H11A H 0.3045 0.0673 0.6086 0.083 Uiso 1 1 calc R
H11B H 0.3881 0.097 0.7278 0.083 Uiso 1 1 calc R
H11C H 0.4377 0.1071 0.612 0.083 Uiso 1 1 calc R
C12 C -0.1205(3) 0.04254(19) 0.7576(3) 0.0372(6) Uani 1 1 d .
C13 C -0.2014(3) 0.0676(2) 0.8453(3) 0.0493(8) Uani 1 1 d .
H13A H -0.2506 0.1153 0.8169 0.074 Uiso 1 1 calc R
H13B H -0.1468 0.0797 0.9195 0.074 Uiso 1 1 calc R
H13C H -0.2573 0.0233 0.8544 0.074 Uiso 1 1 calc R
C14 C -0.2116(3) 0.0184(2) 0.6434(3) 0.0520(9) Uani 1 1 d .
H14A H -0.2621 0.0652 0.6124 0.078 Uiso 1 1 calc R
H14B H -0.2662 -0.025 0.6584 0.078 Uiso 1 1 calc R
H14C H -0.1637 0.0001 0.5878 0.078 Uiso 1 1 calc R
C15 C -0.0430(4) -0.0341(2) 0.8036(3) 0.0547(9) Uani 1 1 d .
H15A H 0.0075 -0.0503 0.749 0.082 Uiso 1 1 calc R
H15B H -0.0996 -0.078 0.8128 0.082 Uiso 1 1 calc R
H15C H 0.0116 -0.022 0.8778 0.082 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 0 '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'
Se Se -0.0929 2.2259 '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
C3 Se1 P3 91.61(8)
P2 Se2 P1 70.81(2)
C3 P1 C2 95.24(12)
C3 P1 Se2 87.22(8)
C2 P1 Se2 94.31(8)
C3 P1 P2 43.96(8)
C2 P1 P2 71.83(8)
Se2 P1 P2 54.04(2)
C3 P2 C1 98.22(11)
C3 P2 Se3 120.49(9)
C1 P2 Se3 124.10(9)
C3 P2 Se2 89.40(8)
C1 P2 Se2 97.63(8)
Se3 P2 Se2 119.52(3)
C3 P2 P1 45.51(8)
C1 P2 P1 75.27(8)
Se3 P2 P1 160.20(4)
Se2 P2 P1 55.15(2)
C1 P3 C2 50.35(11)
C1 P3 Se1 101.89(9)
C2 P3 Se1 101.42(8)
C4 C1 C2 133.0(2)
C4 C1 P3 118.15(18)
C2 C1 P3 64.88(13)
C4 C1 P2 114.16(18)
C2 C1 P2 103.75(17)
P3 C1 P2 114.17(13)
C8 C2 C1 131.4(2)
C8 C2 P3 119.27(18)
C1 C2 P3 64.77(13)
C8 C2 P1 110.48(18)
C1 C2 P1 109.14(16)
P3 C2 P1 114.76(13)
C12 C3 P2 121.67(19)
C12 C3 P1 116.72(19)
P2 C3 P1 90.53(12)
C12 C3 Se1 108.54(17)
P2 C3 Se1 109.78(13)
P1 C3 Se1 108.11(12)
C7 C4 C5 107.9(3)
C7 C4 C6 105.3(3)
C5 C4 C6 111.0(3)
C7 C4 C1 114.1(2)
C5 C4 C1 111.1(2)
C6 C4 C1 107.3(3)
C9 C8 C11 108.4(3)
C9 C8 C10 110.2(3)
C11 C8 C10 104.0(3)
C9 C8 C2 111.1(2)
C11 C8 C2 108.9(2)
C10 C8 C2 114.0(2)
C14 C12 C15 107.3(3)
C14 C12 C13 107.5(3)
C15 C12 C13 109.0(3)
C14 C12 C3 114.1(2)
C15 C12 C3 108.6(2)
C13 C12 C3 110.2(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Se1 C3 1.980(2)
Se1 P3 2.2392(8)
Se2 P2 2.2707(7)
Se2 P1 2.3023(7)
Se3 P2 2.0862(7)
P1 C3 1.890(3)
P1 C2 1.892(3)
P1 P2 2.6494(10)
P2 C3 1.839(3)
P2 C1 1.886(3)
P3 C1 1.857(2)
P3 C2 1.858(3)
C1 C4 1.574(4)
C1 C2 1.580(4)
C2 C8 1.575(4)
C3 C12 1.574(4)
C4 C7 1.531(4)
C4 C5 1.532(5)
C4 C6 1.543(5)
C8 C9 1.533(4)
C8 C11 1.536(5)
C8 C10 1.545(4)
C12 C14 1.532(4)
C12 C15 1.534(5)
C12 C13 1.536(4)
