Novel photolabile protecting group for carbonyl compounds.
Wang, Pengfei; Hu, Huayou; Wang, Yun; Organic letters 9 (2007) 1533–1535; doi:10.1021/ol070346f

data_1505352
_publ_section_title
;
 Novel photolabile protecting group for carbonyl compounds.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              1533
_journal_page_last               1535
_journal_paper_doi               10.1021/ol070346f
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C32 H30 O3'
_chemical_formula_weight         462.56
_chemical_name_common            3f(I)
_chemical_name_systematic        spiro[1,3-benzodioxine-2,1'-cyclohexane]
_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                90.28(3)
_cell_angle_beta                 92.84(3)
_cell_angle_gamma                110.76(3)
_cell_formula_units_Z            4
_cell_length_a                   10.355(2)
_cell_length_b                   13.627(3)
_cell_length_c                   18.942(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2495.5(10)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.1003
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7500
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             984
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0094(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         6502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0871P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1808
_reflns_number_gt                3753
_reflns_number_total             6502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol070346fsi20070212_020911.cif
_cod_data_source_block           hyii147a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2495.7(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1505352