Rh-Catalyzed intramolecular decarbonylative cyclization of ortho-formyl group tethered alkylidenecyclopropanes (ACPs) for the construction of 2-methylindenes
Fan, Xing; Liu, Ruixing; Wei, Yin; Shi, Min; Organic Chemistry Frontiers 6 (2019) 2667–; doi:10.1039/C9QO00614A

data_1554970
_publ_section_title
;
 Rh-Catalyzed intramolecular decarbonylative cyclization of ortho-formyl
 group tethered alkylidenecyclopropanes (ACPs) for the construction of
 2-methylindenes
;
_journal_issue                   15
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              2667
_journal_paper_doi               10.1039/C9QO00614A
_journal_volume                  6
_journal_year                    2019
_chemical_formula_sum            'C17 H14 Cl'
_chemical_formula_weight         253.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-01-04 deposited with the CCDC.	2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                111.893(15)
_cell_angle_beta                 107.027(17)
_cell_angle_gamma                93.776(19)
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_cell_length_b                   12.073(6)
_cell_length_c                   12.827(6)
_cell_measurement_reflns_used    4558
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.542
_cell_measurement_theta_min      5.123
_cell_volume                     1348.7(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0614
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         25.998
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_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.502
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_refine_diff_density_rms         0.047
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+0.6719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3172
_reflns_number_total             5294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo00614a2.cif
_cod_data_source_block           mo_d8v19013_0m
_cod_database_code               1554970
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.979
_shelxl_version_number           2013-4
_shelx_res_checksum              36090
_shelx_hkl_checksum              70061