Piano-Stool Rhodium Enalcarbenoids: Application to Catalyst-Controlled Metal-Templated Annulations of Diazoenals and 1,3-Dicarbonyls
Lad, Bapurao Sudam; Katukojvala, Sreenivas; ACS Catalysis 8 (2018) 11807–; doi:10.1021/acscatal.8b03865

data_4515778
_publ_section_title
;
 Piano-Stool Rhodium Enalcarbenoids: Application to Catalyst-Controlled
 Metal-Templated Annulations of Diazoenals and 1,3-Dicarbonyls
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              11807
_journal_paper_doi               10.1021/acscatal.8b03865
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C26 H18 O3'
_chemical_formula_sum            'C26 H18 O3'
_chemical_formula_weight         378.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 100.161(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   5.8589(6)
_cell_length_c                   26.361(3)
_cell_measurement_reflns_used    6876
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.48
_cell_volume                     3784.9(7)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            18674
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.145
_diffrn_reflns_theta_min         2.480
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       needle
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0346P)^2^+4.4542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2760
_reflns_number_total             4081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b03865_si_002.cif
_cod_data_source_block           BL_04-404
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4515778
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              63125
_shelx_hkl_checksum              21972