Control of Selectivity in the Generation and Reactions of Oxonium Ylides
Deana M. Jaber; Ryan N. Burgin; Matthew Hepler; Peter Zavalij; Zavalij, Peter; Michael P. Doyle; Chem. Commun. 47 (2011) 7623–; doi:10.1039/c1cc12443a

data_7106617
_publ_section_title
;
 Control of Selectivity in the Generation and Reactions of Oxonium Ylides
;
_journal_name_full               'Chem. Commun.'
_journal_page_first              7623
_journal_paper_doi               10.1039/c1cc12443a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C16 H16 O5'
_chemical_formula_sum            'C16 H16 O5'
_chemical_formula_weight         288.29
_chemical_name_common            'Diazo Decomp-Major product'
_chemical_name_systematic
;
Diazo Decomp-Major product
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                89.6028(14)
_cell_angle_beta                 67.7337(13)
_cell_angle_gamma                80.3302(14)
_cell_formula_units_Z            4
_cell_length_a                   10.3115(11)
_cell_length_b                   11.0094(12)
_cell_length_c                   13.2743(14)
_cell_measurement_reflns_used    8296
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.2
_cell_volume                     1372.1(3)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 16.667
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      610,610,610
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.1060969
_diffrn_orient_matrix_UB_12      -0.0236176
_diffrn_orient_matrix_UB_13      -0.0339294
_diffrn_orient_matrix_UB_21      0.0012428
_diffrn_orient_matrix_UB_22      -0.0279975
_diffrn_orient_matrix_UB_23      0.0715073
_diffrn_orient_matrix_UB_31      -0.0092487
_diffrn_orient_matrix_UB_32      -0.0847421
_diffrn_orient_matrix_UB_33      -0.0196926
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6300
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.88
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_id
'Doyle/DeanaJaber Diazo Decomp-Major product @ 120K'
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0359
_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^)+(0.02P)^2^+0.562P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                5367
_reflns_number_total             6300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12443a.txt
_cod_data_source_block           1906
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106617
_diffrn_measurement_frame_width-ccd -0.3
_diffrn_measurement_total_frames-ccd 1830
_diffrn_measurement_frame_time-ccd 60
_diffrn_measurement_total_time-ccd 33.5
_diffrn_detector_distance-ccd    5.0000
_diffrn_measurement_frame_size-ccd 1024