Controllable Rh(III)-Catalyzed Annulation between Salicylaldehydes and Diazo Compounds: Divergent Synthesis of Chromones and Benzofurans.
Sun, Peng; Gao, Shang; Yang, Chi; Guo, Songjin; Lin, Aijun; Yao, Hequan; Organic letters 18 (2016) 6464–6467; doi:10.1021/acs.orglett.6b03355

data_1555983
_publ_section_title
;
 Controllable Rh(III)-Catalyzed Annulation between Salicylaldehydes and
 Diazo Compounds: Divergent Synthesis of Chromones and Benzofurans.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              6464
_journal_page_last               6467
_journal_paper_doi               10.1021/acs.orglett.6b03355
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C13 H14 O3'
_chemical_formula_weight         218.24
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 95.022(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   19.607(6)
_cell_length_c                   7.492(2)
_cell_measurement_reflns_used    3895
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.3565
_cell_measurement_theta_min      2.5345
_cell_volume                     1173.6(6)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
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_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.495
_diffrn_reflns_theta_min         2.077
_exptl_absorpt_coefficient_mu    0.087
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.140
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.029(4)
_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   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2176
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0719P)^2^+0.1756P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1342
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_reflns_number_gt                1808
_reflns_number_total             2176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b03355_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        1173.7(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1555983
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2013-2
_shelx_res_checksum              55725
_shelx_hkl_checksum              16524