Hypersilylated cyclodiphosphadiazanes and cyclodiphosphadiazenium salts
Kuzora, René; Schulz, Axel; Villinger, Alexander; Wustrack, Ronald; Dalton Transactions  (2009) 9304–; doi:10.1039/b911326f

data_7002655
_publ_section_title
;
 Hypersilylated cyclodiphosphadiazanes and cyclodiphosphadiazenium
 salts
;
_journal_issue                   42
_journal_name_full               'Dalton Transactions'
_journal_page_first              9304
_journal_paper_doi               10.1039/b911326f
_journal_year                    2009
_chemical_formula_moiety         'C18 H54 Cl N2 P2 Si8 +, Ga Cl4 -, C H2 Cl2'
_chemical_formula_sum            'C19 H56 Cl7 Ga N2 P2 Si8'
_chemical_formula_weight         917.19
_chemical_name_common
;
1-chloro-2,4-bis(tris(trimethylsilyl)silyl)-cyclo-1,3-
diphospha-2,4-diazenium tetrachlorogallate dichloromethane solvate
;
_chemical_name_systematic
;
1-chloro-2,4-bis[tris(trimethylsilyl)silyl]-cyclo-1,3-diphospha-2,4-diazenium
tetrachlorogallate dichloromethane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.00
_cell_angle_beta                 101.975(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5675(16)
_cell_length_b                   12.0572(16)
_cell_length_c                   27.204(4)
_cell_measurement_reflns_used    9247
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      51.155
_cell_measurement_theta_min      4.559
_cell_volume                     4674.2(11)
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_collection       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37008
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.77
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  0.8514
_exptl_absorpt_correction_T_min  0.7160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.513
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         8045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0861
_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/[\s^2^(Fo^2^)+(0.0972P)^2^+66.2502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2351
_refine_ls_wR_factor_ref         0.2467
_reflns_number_gt                6624
_reflns_number_total             8045
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b911326f.txt
_cod_data_source_block           hyp2n2p2cl_gacl4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7002655