Versatile Access to Martin's Spirosilanes and Their Hypervalent Derivatives.
Lenormand, Hugo; Corcé, Vincent; Sorin, Geoffroy; Chhun, Christine; Chamoreau, Lise-Marie; Krim, Lahouari; Zins, Emilie-Laure; Goddard, Jean-Philippe; Fensterbank, Louis; The Journal of organic chemistry 80 (2015) 3280–3288; doi:10.1021/jo5028497

data_4030766
_publ_section_title
;
 Versatile Access to Martin's Spirosilanes and Their Hypervalent
 Derivatives.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3280
_journal_page_last               3288
_journal_paper_doi               10.1021/jo5028497
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C46 H40 F26 Na2 O12 Si2'
_chemical_formula_sum            'C46 H40 F26 Na2 O12 Si2'
_chemical_formula_weight         1380.94
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                76.5950(10)
_cell_angle_beta                 87.1180(10)
_cell_angle_gamma                78.9230(10)
_cell_formula_units_Z            1
_cell_length_a                   9.7682(2)
_cell_length_b                   12.0747(2)
_cell_length_c                   12.4636(3)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.50
_cell_volume                     1403.34(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(1)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0140
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30730
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.538
_diffrn_reflns_theta_min         1.680
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0733P)^2^+0.4173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                7747
_reflns_number_total             8555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5028497_si_001.cif
_cod_data_source_block           jp1908
_cod_depositor_comments
;
Adding full bibliography for 4030763--4030766.cif.

2024-02-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C23 H20 F13 Na O6 Si'
_cod_original_formula_weight         690.47
_cod_original_formula_moiety         'C20 H12 F13 O4 Si, C3 H6 O, H2 O, Na'
_cod_original_formula_units_Z            2
_cod_database_code               4030766