Ruthenium(0) Catalyzed Endiyne-α-Ketol [4 + 2] Cycloaddition: Convergent Assembly of Type II Polyketide Substructures via C-C Bond Forming Transfer Hydrogenation.
Saxena, Aakarsh; Perez, Felix; Krische, Michael J.; Journal of the American Chemical Society 137 (2015) 5883–5886; doi:10.1021/jacs.5b02755

data_4123779
_publ_section_title
;
 Ruthenium(0) Catalyzed Endiyne-\a-Ketol [4 + 2] Cycloaddition: Convergent
 Assembly of Type II Polyketide Substructures via C-C Bond Forming
 Transfer Hydrogenation.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5883
_journal_page_last               5886
_journal_paper_doi               10.1021/jacs.5b02755
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C32 H34 O6'
_chemical_formula_weight         514.59
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.484(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.6828(17)
_cell_length_b                   10.5143(7)
_cell_length_c                   23.5935(18)
_cell_measurement_temperature    100(2)
_cell_volume                     5514.3(7)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28711
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.832
_exptl_absorpt_coefficient_mu    0.085
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6320
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.122
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+3.9550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5021
_reflns_number_total             6320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b02755_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4123779
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.983
_shelxl_version_number           2013-4
_shelx_res_checksum              63235
_shelx_hkl_checksum              49029