Sequential [6+2], [2+2], and [3+2] annulations for rapid assembly of multiple fragments
Velisoju Mahendar; Hideaki Oikawa; Hiroki Oguri; Chem.Commun. 49 (2013) 2299–; doi:10.1039/c2cc38854e

data_7108945
_publ_section_title
;
 Sequential [6+2], [2+2], and [3+2] annulations for rapid assembly of
 multiple fragments
;
_journal_name_full               Chem.Commun.
_journal_page_first              2299
_journal_paper_doi               10.1039/c2cc38854e
_journal_volume                  49
_journal_year                    2013
_chemical_compound_source        'synthesised by authors, see text'
_chemical_formula_moiety         'C35 H38 N2 O5 Si, 0.5(C3 H8 O)'
_chemical_formula_sum            'C36.5 H42 N2 O5.5 Si'
_chemical_formula_weight         624.81
_chemical_name_systematic
;
?
;
_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           SHELXL-97
_cell_angle_alpha                82.6410(10)
_cell_angle_beta                 81.6980(10)
_cell_angle_gamma                64.6870(10)
_cell_formula_units_Z            2
_cell_length_a                   10.06519(18)
_cell_length_b                   11.1789(2)
_cell_length_c                   16.4195(3)
_cell_measurement_reflns_used    17152
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.29
_cell_measurement_theta_min      4.39
_cell_volume                     1648.05(5)
_computing_cell_refinement       'Rigaku RAPID AUTO'
_computing_data_collection       'Rigaku RAPID AUTO'
_computing_data_reduction        'Rigaku RAPID AUTO'
_computing_molecular_graphics    'Crystal Structure and PLATON(Spek, 2003)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'IP area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19565
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         4.39
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.9238
_exptl_absorpt_correction_T_min  0.8802
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Lorentz-polarization
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         5910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+0.6503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                4987
_reflns_number_total             5910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc38854e.txt
_cod_data_source_block           shelxl2
_cod_original_cell_volume        1648.04(5)
_cod_original_formula_sum        'C36.50 H42 N2 O5.50 Si'
_cod_database_code               7108945