Rhodium-catalyzed cycloisomerization of ester-tethered 1,6-diynes with cyclopropanol moiety leading to tetralone/exocyclic diene hybrid molecules.
Yasui, Takeshi; Kikuchi, Tomohiro; Yamamoto, Yoshihiko; Chemical communications (Cambridge, England) 56 (2020) 12865–12868; doi:10.1039/d0cc05429a

data_7127273
_publ_section_title
;
 Rhodium-catalyzed cycloisomerization of ester-tethered 1,6-diynes with
 cyclopropanol moiety leading to tetralone/exocyclic diene hybrid
 molecules.
;
_journal_issue                   84
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12865
_journal_page_last               12868
_journal_paper_doi               10.1039/d0cc05429a
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C21 H16 O3'
_chemical_formula_sum            'C21 H16 O3'
_chemical_formula_weight         316.36
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-06-03 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
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_cell_angle_gamma                90.0000
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_cell_length_b                   8.1201(3)
_cell_length_c                   10.9799(4)
_cell_measurement_reflns_used    7311
_cell_measurement_temperature    123
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      4.50
_cell_volume                     767.22(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
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_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
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_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
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_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8943
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.214
_diffrn_reflns_theta_min         4.497
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
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_exptl_crystal_size_mid          0.200
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_refine_ls_abs_structure_details
;
 Flack x determined using 1098 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_coef       0.0050(11)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2701
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.1740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                2602
_reflns_number_total             2701
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d0cc05429a3.cif
_cod_data_source_block           KIK-0575-pro
_cod_depositor_comments
'Adding full bibliography for 7127270--7127274.cif.'
_cod_original_cell_volume        767.22(4)
_cod_database_code               7127273
_shelx_res_checksum              47088
_shelx_hkl_checksum              94324