Formation of a silicon-containing macrocycle with a pyridoxalimine Schiff base ligand
Böhme, Uwe; Günther, Betty; Schwarzer, Anke; Acta Crystallographica Section C 64 (2008) o630–o632; doi:10.1107/S0108270108036238

data_2016864
_publ_section_title
;
 Formation of a silicon-containing macrocycle with a pyridoxalimine
 Schiff base ligand
;
_journal_coeditor_code           GA3110
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o630
_journal_page_last               o632
_journal_paper_doi               10.1107/S0108270108036238
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C52 H44 N4 O6 Si2 , 4C H Cl3'
_chemical_formula_moiety         'C52 H44 N4 O6 Si2 , 4(C H Cl3)'
_chemical_formula_sum            'C56 H48 Cl12 N4 O6 Si2'
_chemical_formula_weight         1354.56
_chemical_name_common
;
<i>cyclo</i>-bis{5-(oxymethyl)-4-{(<i>E</i>)-[(2-oxyphenyl)imino]methyl}-
2-methylpyridin-3-ol}diphenylsilane} chloroform tetrasolvate
;
_chemical_name_systematic
;
9,27-dimethyl-3,3,21,21-tetraphenyl-2,4,20,22-tetraoxa-8,13,26,31-tetraaza-
3,21-disilapentacyclo[30.4.0.0^6,11^.0^14,19^.0^24,29^]hexatrideca-
1(32),6,8,10,12,14,16,18,24,26,28,30,33,35-tetradecaene-10,28-diol
chloroform tetrasolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                102.853(2)
_cell_angle_beta                 101.8990(10)
_cell_angle_gamma                98.7330(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8831(3)
_cell_length_b                   11.2094(3)
_cell_length_c                   14.7584(4)
_cell_measurement_reflns_used    8116
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.15
_cell_volume                     1525.91(8)
_computing_cell_refinement       'SMART (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14146
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.8728
_exptl_absorpt_correction_T_min  0.8176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6493
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.349
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0480P)^2^+1.0265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                5116
_reflns_number_total             6493
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3110.cif
_cod_data_source_block           III
_cod_database_code               2016864
_cod_database_fobs_code          2016864