DMAP Promoted Tandem Addition Reactions Forming Substituted Tetrahydroxanthones.
Castillo-Contreras, Emmanuel B; Dake, Gregory R.; Organic letters 16 (2014) 1642–1645; doi:10.1021/ol5002945

data_1513928
_publ_section_title
;
 DMAP Promoted Tandem Addition Reactions Forming Substituted
 Tetrahydroxanthones.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1642
_journal_page_last               1645
_journal_paper_doi               10.1021/ol5002945
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C30 H22 N2 O10'
_chemical_formula_sum            'C30 H22 N2 O10'
_chemical_formula_weight         570.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 92.298(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
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_cell_length_b                   14.767(5)
_cell_length_c                   20.845(5)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      1.7
_cell_volume                     2582.1(19)
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker x8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.690
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  .989
_exptl_absorpt_correction_T_min  .907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker - SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          .26
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .10
_exptl_transmission_factor_max   .989
_exptl_transmission_factor_min   .907
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+1.6617P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4676
_reflns_number_total             5920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5002945_si_001.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               1513928
_shelx_estimated_absorpt_t_min   .907
_shelx_estimated_absorpt_t_max   .989
_shelxl_version_number           2012-9
_shelx_res_checksum              20129
_shelx_hkl_checksum              7304