Pd-catalyzed intermolecular consecutive double Heck reaction "on water" under air: facile synthesis of substituted indenes.
Wei, Dong; Lu, Han-Yu; Miao, Han-Zhe; Feng, Chen-Guo; Lin, Guo-Qiang; Liu, Yingbin; RSC advances 13 (2023) 19312–19316; doi:10.1039/d3ra03510g

data_7246945
_publ_section_title
;
 Pd-catalyzed intermolecular consecutive double Heck reaction "on water"
 under air: facile synthesis of substituted indenes.
;
_journal_issue                   28
_journal_name_full               'RSC advances'
_journal_page_first              19312
_journal_page_last               19316
_journal_paper_doi               10.1039/d3ra03510g
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C30 H21 F3'
_chemical_formula_sum            'C30 H21 F3'
_chemical_formula_weight         438.47
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-04 deposited with the CCDC.	2023-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                73.3310(10)
_cell_angle_beta                 86.7220(10)
_cell_angle_gamma                83.7240(10)
_cell_formula_units_Z            2
_cell_length_a                   9.26090(10)
_cell_length_b                   10.8518(2)
_cell_length_c                   11.3998(2)
_cell_measurement_reflns_used    7553
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.92
_cell_measurement_theta_min      5.32
_cell_volume                     1090.53(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      170.01
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11640
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.916
_diffrn_reflns_theta_min         3.717
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0709 before and 0.0435 after correction. The Ratio of minimum to maximum transmission is 0.8440. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.5468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3592
_reflns_number_total             4096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra03510g2.cif
_cod_data_source_block           mjl18402_0m
_cod_database_code               7246945
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30)
2.b X=CH2 refined with riding coordinates:
 C24(H24A,H24B)
;
_shelx_res_checksum              61277
_olex2_submission_special_instructions 'No special instructions were received'