Rh(i)-catalyzed stereoselective desymmetrization of prochiral cyclohexadienones <i>via</i> highly <i>exo</i>-selective Huisgen-type [3 + 2] cycloaddition.
Gollapelli, Krishna Kumar; Patil, Vaibhav B.; Vinaykumar, Allam; Chegondi, Rambabu; Chemical science 12 (2020) 1544–1550; doi:10.1039/d0sc05543c

data_1559655
_publ_section_title
;
 Rh(i)-catalyzed stereoselective desymmetrization of prochiral
 cyclohexadienones <i>via</i> highly <i>exo</i>-selective Huisgen-type [3
 + 2] cycloaddition.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              1544
_journal_page_last               1550
_journal_paper_doi               10.1039/d0sc05543c
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C17 H14 O4'
_chemical_formula_sum            'C17 H14 O4'
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_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
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_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-06-07 deposited with the CCDC.	2020-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_length_c                   14.430(9)
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_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.031
_cell_measurement_theta_min      2.265
_cell_volume                     1336.3(15)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2016)'
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_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_min         2.264
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
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'Re-crystallisation from solvent: Dichloromethane/Hexane'
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_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0484
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.5717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2331
_reflns_number_total             3063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05543c2.cif
_cod_data_source_block           KA579_0m
_cod_depositor_comments
;Adding full bibliography for 1559655.cif.

 Adding full bibliography for 1559655.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1559655
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              59883