Silane catecholates: Versatile tools for self-assembled dynamic covalent bond chemistry
Kabe, Yoshio; Kawakami, Yoshiteru; Ogishima, Tsuyoshi; Kawara, Tomoki; Yamauchi, Shota; Okamoto, Kazuhiko; Nikaido, Singo; Souma, Daiki; Jin, Ren-hua; Chemical Communications  (2019) –; doi:10.1039/C9CC02103E

data_7123345
_publ_section_title
;
 Silane catecholates: Versatile tools for self-assembled dynamic covalent
 bond chemistry
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02103E
_journal_year                    2019
_chemical_formula_sum            'C80 H101 N2 O17.5 S7 Si2'
_chemical_formula_weight         1651.23
_chemical_name_systematic
; 
 ? 
;
_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
_audit_update_record
;
2019-01-21 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.14(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.993(7)
_cell_length_b                   21.486(9)
_cell_length_c                   27.205(11)
_cell_measurement_reflns_used    18714
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      3.0085
_cell_volume                     8933(7)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
'Saturn724+ (4x4 bin mode)'
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            128180
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3500
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.784
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         20240
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.785
_refine_ls_R_factor_all          0.2191
_refine_ls_R_factor_gt           0.1894
_refine_ls_shift/su_max          0.287
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4934
_refine_ls_wR_factor_ref         0.5169
_reflns_number_gt                14227
_reflns_number_total             20240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc02103e2.cif
_cod_data_source_block           PhSi4EAT4_bluebox_14DMSO_5H2O
_cod_original_cell_volume        8934(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C80 H101 N2 O17.50 S7 Si2'
_cod_database_code               7123345