Homoleptic low-valent polyazides of group 14 elements
Benjamin Peerless; Theo Keane; Anthony J. H. M. Meijer; Peter Portius; Chem.Commun. 51 (2015) 7435–; doi:10.1039/C5cc00259A

data_7117027
_publ_section_title
;
 Homoleptic low-valent polyazides of group 14 elements
;
_journal_name_full               Chem.Commun.
_journal_page_first              7435
_journal_paper_doi               10.1039/C5cc00259A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C24 H20 P, N9 Sn'
_chemical_formula_sum            'C24 H20 N9 P Sn'
_chemical_formula_weight         584.15
_chemical_name_common            (PPh4)[Sn(N3)3]
_chemical_name_systematic        'Tetraphenylphosphonium triazidostannate(II)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-01-26 deposited with the CCDC.
2015-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                91.668(4)
_cell_angle_beta                 108.414(4)
_cell_angle_gamma                116.545(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7560(6)
_cell_length_b                   11.0605(6)
_cell_length_c                   12.3540(7)
_cell_measurement_reflns_used    6545
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.9402
_cell_measurement_theta_min      2.2761
_cell_volume                     1222.10(13)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  'ORTEP-3 for Windows'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-2014
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22380
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.202
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       needle
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.295
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5407
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.3033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4484
_reflns_number_total             5407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc00259a2.cif
_cod_data_source_block           ch1ppx203_0m
_cod_original_cell_volume        1222.11(12)
_cod_database_code               7117027
_shelx_estimated_absorpt_t_min   0.748
_shelx_estimated_absorpt_t_max   0.856
_shelxl_version_number           2014-3
_shelx_res_checksum              61334