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_7123344
_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            'C128 H172 N4 O24 Si4'
_chemical_formula_weight         2263.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 114.772(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   43.04(5)
_cell_length_b                   9.038(9)
_cell_length_c                   20.98(2)
_cell_measurement_reflns_used    7383
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      3.0493
_cell_volume                     7410(13)
_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 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.1466
_diffrn_reflns_av_sigmaI/netI    0.1950
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21709
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.8(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.345
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         11432
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.348
_refine_ls_R_factor_all          0.2062
_refine_ls_R_factor_gt           0.1748
_refine_ls_shift/su_max          2.229
_refine_ls_shift/su_mean         0.096
_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          0.4365
_refine_ls_wR_factor_ref         0.4671
_reflns_number_gt                5777
_reflns_number_total             11432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc02103e2.cif
_cod_data_source_block           PhSi4EAT4_8MeOH
_cod_original_cell_volume        7409(14)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7123344