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_7117028
_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, Ge N9'
_chemical_formula_sum            'C24 H20 Ge N9 P'
_chemical_formula_weight         538.07
_chemical_name_common            (PPh4)[Ge(N3)3]
_chemical_name_systematic        (PPh4)[Ge(N3)3]
_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
;
2014-10-18 deposited with the CCDC.
2015-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                93.278(2)
_cell_angle_beta                 99.357(2)
_cell_angle_gamma                100.865(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7712(2)
_cell_length_b                   11.4711(4)
_cell_length_c                   14.2003(4)
_cell_measurement_reflns_used    4545
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.4081
_cell_measurement_theta_min      2.4303
_cell_volume                     1221.59(6)
_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-97
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0598
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24413
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         1.815
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_T_max  0.9233
_exptl_absorpt_correction_T_min  0.7117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       needle
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4124
_reflns_number_total             5613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc00259a2.cif
_cod_data_source_block           ch1ppx202_0m
_cod_database_code               7117028
_shelx_estimated_absorpt_t_min   0.712
_shelx_estimated_absorpt_t_max   0.923
_shelxl_version_number           2014-3
_shelx_res_checksum              42559