#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/40/2004010.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2004010
loop_
_publ_author_name
'Halfpenny, J.'
_publ_section_title
;
 Bis(tetraphenylphosphonium) Tetraazidodimethylstannate(IV)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2044
_journal_page_last               2046
_journal_paper_doi               10.1107/S0108270195005269
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         '2[(C6 H5)4 P] +,C2 H6 N12 Sn1 2-'
_chemical_formula_sum            'C50 H46 N12 P2 Sn'
_chemical_formula_weight         995.59
_chemical_name_systematic
;
bis(tetraphenylphosphonium) tetraazidodimethylstannate(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                123.2(1)
_cell_angle_beta                 77.9(1)
_cell_angle_gamma                100.0(1)
_cell_formula_units_Z            1
_cell_length_a                   12.38(1)
_cell_length_b                   10.11(1)
_cell_length_c                   11.44(1)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    286
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     1168(2)
_computing_data_collection       'Stoe  STADI-2'
_computing_data_reduction        'DATR (Small, 1977)'
_computing_molecular_graphics    'SNOOPI (Davies, 1983)'
_computing_structure_refinement  SHELX76
_computing_structure_solution    'SHELX76 (Sheldrick, 1976) (Patterson)'
_diffrn_ambient_temperature      288
_diffrn_measurement_device       'Stoe STADI-2 two-circle diffractometer'
_diffrn_measurement_method       "variable ω scans, 2θ' fixed"
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4059
_diffrn_reflns_reduction_process 'SHELX76 (Sheldrick, 1976)'
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        '5% maximum, corrected by interpolation'
_diffrn_standards_interval_count 20
_diffrn_standards_number         '1 per layer'
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.8572
_exptl_absorpt_correction_T_min  0.7484
_exptl_absorpt_correction_type   'integration (SHELX76; Sheldrick, 1976)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       'oblique bipyramid'
_exptl_crystal_F_000             510.0
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.427
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     '326 (2 blocks)'
_refine_ls_number_reflns         3451
_refine_ls_R_factor_obs          0.038
_refine_ls_shift/esd_max         .003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.038
_reflns_number_observed          3451
_reflns_number_total             3833
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            jz1036.cif
_cod_data_source_block           a
_cod_original_cell_volume        1168.6(10)
_cod_database_code               2004010
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_refinement_flags
P 0.3226(1) 0.6102(1) 0.4064(1) 0.042(1) Uani ? ? ?
Sn 0.0000 0.0000 0.0000 0.045(1) Uani ? ? S
N1 0.1633(3) 0.1346(4) 0.0804(4) 0.059(4) Uani ? ? ?
N2 0.2212(3) 0.0745(4) 0.1063(4) 0.056(3) Uani ? ? ?
N3 0.2790(3) 0.0206(5) 0.1315(5) 0.088(5) Uani ? ? ?
N4 0.0572(3) 0.0088(4) -0.1958(4) 0.060(3) Uani ? ? ?
N5 0.1080(3) 0.1213(5) -0.1909(4) 0.062(4) Uani ? ? ?
N6 0.1584(4) 0.2288(6) -0.1898(6) 0.099(6) Uani ? ? ?
C1 0.2757(3) 0.4892(5) 0.5717(5) 0.057(4) Uani ? ? ?
C2 0.2148(4) 0.3987(5) 0.6214(5) 0.064(5) Uani ? ? ?
C3 0.1186(3) 0.3138(5) 0.5694(5) 0.061(4) Uani ? ? ?
C4 0.0821(3) 0.3174(5) 0.4687(5) 0.065(4) Uani ? ? ?
C5 0.1422(3) 0.4092(5) 0.4187(4) 0.055(4) Uani ? ? ?
C6 0.2397(3) 0.4950(4) 0.4707(4) 0.043(3) Uani ? ? ?
C7 0.4511(3) 0.3502(4) 0.2405(4) 0.048(3) Uani ? ? ?
C8 0.5409(3) 0.2729(5) 0.1420(5) 0.060(4) Uani ? ? ?
C9 0.6101(3) 0.3429(5) 0.0781(4) 0.060(4) Uani ? ? ?
C10 0.5901(3) 0.4891(6) 0.1095(5) 0.065(4) Uani ? ? ?
C11 0.4999(3) 0.5661(5) 0.2053(5) 0.059(4) Uani ? ? ?
C12 0.4308(3) 0.4974(4) 0.2725(4) 0.044(3) Uani ? ? ?
C13 0.2092(3) 0.5514(5) 0.2039(4) 0.055(4) Uani ? ? ?
C14 0.1494(3) 0.5923(6) 0.1429(5) 0.066(5) Uani ? ? ?
C15 0.1245(3) 0.7480(7) 0.2083(6) 0.070(5) Uani ? ? ?
C16 0.1562(3) 0.8620(6) 0.3352(6) 0.070(5) Uani ? ? ?
C17 0.2144(3) 0.8239(5) 0.4004(5) 0.058(4) Uani ? ? ?
C18 0.2419(3) 0.6676(4) 0.3335(4) 0.046(4) Uani ? ? ?
C19 0.5002(3) 0.8102(5) 0.5415(5) 0.060(4) Uani ? ? ?
C20 0.5451(4) 0.9383(6) 0.6555(6) 0.076(6) Uani ? ? ?
C21 0.4769(5) 1.0373(6) 0.7727(6) 0.082(6) Uani ? ? ?
C22 0.3629(5) 1.0098(5) 0.7813(5) 0.072(5) Uani ? ? ?
C23 0.3164(3) 0.8801(5) 0.6694(4) 0.060(4) Uani ? ? ?
C24 0.3854(3) 0.7804(4) 0.5482(4) 0.046(3) Uani ? ? ?
C25 -.0663(4) 0.2255(5) 0.1089(6) 0.061(5) Uani ? ? ?
H1 0.351(1) 0.555(1) 0.613(1) 0.08(1) Uiso calc C1 ?
H2 0.243(1) 0.394(1) 0.702(1) 0.08(1) Uiso calc C2 ?
H3 0.072(1) 0.243(1) 0.610(1) 0.08(1) Uiso calc C3 ?
H4 0.007(1) 0.250(1) 0.428(1) 0.10(2) Uiso calc C4 ?
H5 0.113(1) 0.414(1) 0.339(1) 0.06(1) Uiso calc C5 ?
H6 0.397(1) 0.295(1) 0.292(1) 0.06(1) Uiso calc C7 ?
H7 0.556(1) 0.157(1) 0.116(1) 0.07(1) Uiso calc C8 ?
H8 0.681(1) 0.283(1) 0.003(1) 0.05(1) Uiso calc C9 ?
H9 0.645(1) 0.544(1) 0.059(1) 0.09(2) Uiso calc C10 ?
H10 0.483(1) 0.680(1) 0.228(1) 0.08(1) Uiso calc C11 ?
H11 0.231(1) 0.431(1) 0.152(1) 0.06(1) Uiso calc C13 ?
H12 0.121(1) 0.503(1) 0.043(1) 0.11(2) Uiso calc C14 ?
H13 0.079(1) 0.779(1) 0.157(1) 0.11(2) Uiso calc C15 ?
H14 0.135(1) 0.983(1) 0.385(1) 0.10(2) Uiso calc C16 ?
H15 0.239(1) 0.913(1) 0.502(1) 0.06(1) Uiso calc C17 ?
H16 0.553(1) 0.733(1) 0.447(1) 0.07(1) Uiso calc C19 ?
H17 0.634(1) 0.960(1) 0.652(1) 0.12(2) Uiso calc C20 ?
H18 0.513(1) 1.139(1) 0.861(1) 0.10(2) Uiso calc C21 ?
H19 0.311(1) 1.090(1) 0.875(1) 0.10(2) Uiso calc C22 ?
H20 0.228(1) 0.856(1) 0.676(1) 0.09(2) Uiso calc C23 ?
H21 -.025(4) 0.288(6) 0.081(6) 0.10(2) Uiso d ? ?
H22 -.134(5) 0.220(7) 0.102(6) 0.12(2) Uiso d ? ?
H23 -.060(4) 0.281(7) 0.204(6) 0.10(2) Uiso d ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C ? 'SHELX76 (Sheldrick, 1976)' ? ?
H ? 'SHELX76 (Sheldrick, 1976)' ? ?
N ? 'SHELX76 (Sheldrick, 1976)' ? ?
P ? 'SHELX76 (Sheldrick, 1976)' ? ?
Sn ? 'SHELX76 (Sheldrick, 1976)' ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C6 P C12 110.0(2) yes
C6 P C18 110.6(2) yes
C6 P C24 108.9(2) yes
C12 P C18 108.6(2) yes
C12 P C24 108.1(2) yes
C18 P C24 110.7(2) yes
N1 Sn N4 88.80(10) yes
N1 Sn C25 86.8(2) yes
N4 Sn C25 91.6(2) yes
Sn N1 N2 118.3(3) yes
Sn N4 N5 121.3(3) yes
N1 N2 N3 177.9(4) yes
N4 N5 N6 178.2(5) yes
C6 C1 C2 119.2(4) ?
C1 C2 C3 120.7(6) ?
C2 C3 C4 120.8(5) ?
C3 C4 C5 118.9(4) ?
C4 C5 C6 120.6(5) ?
C5 C6 C1 119.7(5) ?
C5 C6 P 122.5(4) ?
C1 C6 P 117.8(3) ?
C12 C7 C8 119.9(4) ?
C7 C8 C9 120.3(5) ?
C8 C9 C10 119.9(4) ?
C9 C10 C11 120.5(5) ?
C10 C11 C12 119.99(5) ?
C11 C12 C7 119.5(3) ?
C11 C12 P 117.8(3) ?
C7 C12 P 122.6(3) ?
C18 C13 C14 118.6(4) ?
C13 C14 C15 120.1(3) ?
C14 C15 C16 121.4(7) ?
C15 C16 C17 119.8(5) ?
C16 C17 C18 119.0(4) ?
C17 C18 C13 121.0(5) ?
C17 C18 P 122.0(3) ?
C13 C18 P 117.0(4) ?
C24 C19 C20 119.6(4) ?
C19 C20 C21 119.7(5) ?
C20 C21 C22 121.5(4) ?
C21 C22 C23 119.6(4) ?
C22 C23 C24 119.2(4) ?
C23 C24 C19 120.3(3) ?
C23 C24 P 118.1(3) ?
C19 C24 P 121.5(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C6 P 1.777(5) yes
C12 P 1.789(3) yes
C18 P 1.764(6) yes
C24 P 1.789(3) yes
N1 Sn 2.288(3) yes
N4 Sn 2.250(5) yes
C25 Sn 2.130(5) yes
N2 N1 1.187(7) yes
N3 N2 1.134(8) yes
N5 N4 1.179(6) yes
N6 N5 1.150(8) yes
C2 C1 1.371(8) ?
C6 C1 1.355(8) ?
C3 C2 1.376(6) ?
C4 C3 1.342(9) ?
C5 C4 1.380(8) ?
C6 C5 1.390(5) ?
C8 C7 1.389(5) ?
C12 C7 1.381(6) ?
C9 C8 1.365(8) ?
C10 C9 1.373(8) ?
C11 C10 1.382(5) ?
C12 C11 1.382(7) ?
C14 C13 1.358(9) ?
C18 C13 1.386(5) ?
C15 C14 1.384(8) ?
C16 C15 1.356(7) ?
C17 C16 1.363(10) ?
C18 C17 1.397(6) ?
C20 C19 1.375(6) ?
C24 C19 1.396(5) ?
C21 C20 1.365(7) ?
C22 C21 1.385(8) ?
C23 C22 1.377(6) ?
C24 C23 1.393(5) ?
H21 C25 0.90(7) ?
H22 C25 0.85(7) ?
H23 C25 0.92(6) ?
