Formation of a macrocycle from dichlorodimethylsilane and a pyridoxalimine Schiff base ligand
Böhme, Uwe; Schwarzer, Anke; Günther, Betty; Acta Crystallographica Section E 77 (2021) –; doi:10.1107/S2056989021010185

data_2243936
_publ_section_title
;
 Formation of a macrocycle from dichlorodimethylsilane and a
 pyridoxalimine Schiff base ligand
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021010185
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C24 H36 N4 O6 Si2'
_chemical_formula_moiety         'C24 H36 N4 O6 Si2'
_chemical_formula_sum            'C24 H36 N4 O6 Si2'
_chemical_formula_weight         532.75
_chemical_name_systematic
(8<i>E</i>,22<i>E</i>)-4,4,12,18,18,26-Hexamethyl-3,5,17,19-tetraoxa-8,13,22,27-tetraaza-4,18-disilatricyclo[22.4.0.0^10,15^]octacosa-1(24),8,10,12,14,22,25,27-octaene-11,25-diol
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 101.198(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9641(8)
_cell_length_b                   16.8966(7)
_cell_length_c                   13.1085(8)
_cell_measurement_reflns_used    19293
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      3.15
_cell_volume                     2816.7(3)
_computing_cell_refinement
;
X-AREA (Stoe, 2009)
;
_computing_data_collection
;
X-AREA (Stoe, 2009)
;
_computing_data_reduction
;
X-RED (Stoe, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
<i>SHELXL2017/1</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
<i>SHELXL2017/1</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      153
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19293
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.990
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_voltage           0
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.9933
_exptl_absorpt_correction_T_min  0.9067
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED; Stoe, 2009)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0343P)^2^+2.1897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                2833
_reflns_number_total             3242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq2266sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'I 2/c'
_cod_database_code               2243936
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.975
_shelx_hkl_checksum              87176
_shelx_res_checksum              72364
_cod_database_fobs_code 2243936