An approach for rapid increase in molecular complexity: atom economic routes to fused polycyclic ring systems.
Trost, Barry M.; Ehmke, Veronika; Organic letters 16 (2014) 2708–2711; doi:10.1021/ol5009872

data_1515947
_publ_section_title
;
 An approach for rapid increase in molecular complexity: atom economic
 routes to fused polycyclic ring systems.
;
_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              2708
_journal_page_last               2711
_journal_paper_doi               10.1021/ol5009872
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C28 H37 N O5 Si'
_chemical_formula_sum            'C28 H37 N O5 Si'
_chemical_formula_weight         495.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3680(3)
_cell_length_b                   55.5740(13)
_cell_length_c                   6.2795(2)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      70.35
_cell_measurement_theta_min      3.18
_cell_volume                     5363.1(2)
_computing_cell_refinement       'Bruker SAINT v8.27B'
_computing_data_collection       'Bruker APEX-II v2013-2.0'
_computing_data_reduction        'Bruker SAINT v8.27B'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXT-2012/2 (Sheldrick, 2012)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            75015
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.523
_diffrn_reflns_theta_min         2.983
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.9365
_exptl_absorpt_correction_T_min  0.8470
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;

 Flack x determined using 3170 quotients [(I+)-(I-)]/[(I+)+(I-)]

 (Parsons and Flack (2004), Acta Cryst. A60, s61).

;
_refine_ls_abs_structure_Flack   0.017(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10408
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

 w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+5.3800P]

 where P=(Fo^2^+2Fc^2^)/3

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1765
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                8635
_reflns_number_total             10408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5009872_si_002.cif
_cod_data_source_block           su1302
_cod_depositor_comments
;
          Adding full bibliography for 1515947.cif.

2019-08-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C28 H37 N O5 Si)'
_cod_original_formula_sum        'C56 H74 N2 O10 Si2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     991.35
_cod_database_code               1515947
_shelx_estimated_absorpt_t_min   0.863
_shelx_estimated_absorpt_t_max   0.898
_diffrn_source_monochromator     'MONTEL Multi-layer'
_shelxl_version_number           2012-9