Bis(triphenyl-λ(5)-phosphanylidene)ammonium fluoride: a reactive fluoride source to access the hypervalent silicates [MenSiF5-n](-) (n = 0-3).
Bolli, Christoph; Gellhaar, Jorit; Jenne, Carsten; Keßler, Mathias; Scherer, Harald; Seeger, Helene; Uzun, Rabiya; Dalton transactions (Cambridge, England : 2003) 43 (2014) 4326–4334; doi:10.1039/c3dt52617h

data_7028926
_publ_section_title
;
 Bis(triphenyl-\l(5)-phosphanylidene)ammonium fluoride: a reactive
 fluoride source to access the hypervalent silicates [MenSiF5-n](-) (n =
 0-3).
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4326
_journal_page_last               4334
_journal_paper_doi               10.1039/c3dt52617h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         '2(C36 H30 N P2), F6 Si, 6(C H4 O)'
_chemical_formula_sum            'C78 H84 F6 N2 O6 P4 Si'
_chemical_formula_weight         1411.44
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 91.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.131(2)
_cell_length_b                   12.139(2)
_cell_length_c                   26.696(5)
_cell_measurement_reflns_used    3183
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.83
_cell_volume                     3605.5(11)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS Spider'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            28032
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.9574
_exptl_absorpt_correction_T_min  0.9275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
March 2001 T Higashi
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         8259
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0375P)^2^+2.4597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                7019
_reflns_number_total             8259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52617h.txt
_cod_data_source_block           ck-ru-08
_cod_original_cell_volume        3605.4(12)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7028926