Rh-Catalyzed cascade C-H activation/C-C cleavage/cyclization of carboxylic acids with cyclopropanols.
Wang, Siqi; Miao, Erfei; Wang, Hao; Song, Bichao; Huang, Wei; Yang, Weibo; Chemical communications (Cambridge, England) 57 (2021) 5929–5932; doi:10.1039/d1cc01778k

data_7128276
_publ_section_title
;
 Rh-Catalyzed cascade C-H activation/C-C cleavage/cyclization of
 carboxylic acids with cyclopropanols.
;
_journal_issue                   48
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5929
_journal_page_last               5932
_journal_paper_doi               10.1039/d1cc01778k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C17 H14 O3'
_chemical_formula_sum            'C17 H14 O3'
_chemical_formula_weight         266.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-25 deposited with the CCDC.	2021-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.15(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.843(11)
_cell_length_b                   5.480(2)
_cell_length_c                   15.129(6)
_cell_measurement_reflns_used    1101
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.581
_cell_measurement_theta_min      2.593
_cell_volume                     1302.3(11)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'bruker d8 venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0836
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6128
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.262
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1058 before and 0.0596 after correction. The Ratio of minimum to maximum transmission is 0.8739. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       needle
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+5.0625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2488
_refine_ls_wR_factor_ref         0.2709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1573
_reflns_number_total             2261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01778k2.cif
_cod_data_source_block           sq255-4
_cod_depositor_comments          'Adding full bibliography for 7128276.cif.'
_cod_original_cell_volume        1302.2(11)
_cod_database_code               7128276
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.989
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H17(0.029) H9(0.031) H16(0.034) H7(0.036) H6(0.039) H14(0.037)
 H13(0.029) H4A(0.059) H4B(0.059) H4C(0.059) H5(0.042) H10A(0.028) H10B(0.028)
 H15(0.035)
 Fixed X: H17(0.497047) H9(0.231) H16(0.638702) H7(0.219207) H6(0.133804)
 H14(0.643977) H13(0.500872) H4A(-0.000498) H4B(0.032905) H4C(0.086352)
 H5(0.060969) H10A(0.358804) H10B(0.361263) H15(0.711022)
 Fixed Y: H17(-0.296582) H9(-0.015001) H16(-0.234438) H7(0.282958)
 H6(0.611001) H14(0.404662) H13(0.353295) H4A(0.733497) H4B(0.975645)
 H4C(0.858807) H5(0.852221) H10A(0.192262) H10B(0.343282) H15(0.115463)
 Fixed Z: H17(0.689927) H9(0.43888) H16(0.790329) H7(0.271786) H6(0.190559)
 H14(0.658109) H13(0.561856) H4A(0.434493) H4B(0.400015) H4C(0.500981)
 H5(0.263369) H10A(0.434311) H10B(0.525859) H15(0.774659)
;
_olex2_submission_special_instructions 'No special instructions were received'