Synthesis of Mono-, Di- and Tripalladated 1,3,5-Benzenetristyryl Complexes. CO Insertion to give a Dipalladated Indenone
Shenoy, Rashmi V.; Jones, P. G.; Soler, José Vicente; Martinez-Viviente, Eloisa; Dalton Transactions  (2023) –; doi:10.1039/D3DT00091E

data_7712408
_publ_section_title
;
 Synthesis of Mono-, Di- and Tripalladated 1,3,5-Benzenetristyryl
 Complexes. CO Insertion to give a Dipalladated Indenone
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00091E
_journal_year                    2023
_chemical_formula_moiety         'C69 H57 Br3 P2 Pd, C H Cl3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C72 H63 Br3 Cl3 O0.5 P2 Pd'
_chemical_formula_weight         1449.63
_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     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-08-10 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                72.181(5)
_cell_angle_beta                 85.818(5)
_cell_angle_gamma                76.627(4)
_cell_formula_units_Z            2
_cell_length_a                   13.4054(5)
_cell_length_b                   14.5302(7)
_cell_length_c                   18.0084(7)
_cell_measurement_reflns_used    19239
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8142
_cell_measurement_theta_min      2.1771
_cell_volume                     3248.9(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.40 (release 27-04-2009 CrysAlis171 .NET)
(compiled Apr 27 2009,10:20:11)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.40 (release 27-04-2009 CrysAlis171 .NET)
(compiled Apr 27 2009,10:20:11)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.40 (release 27-04-2009 CrysAlis171 .NET)
(compiled Apr 27 2009,10:20:11)
;
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54851
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.181
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.40 (release 27-04-2009 CrysAlis171 .NET)
(compiled Apr 27 2009,10:20:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         13267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0188P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9113
_reflns_number_total             13267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00091e2.cif
_cod_data_source_block           frash
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7712408
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.494
_shelx_estimated_absorpt_t_max   0.720
_smtbx_masks_special_details
;
A solvent mask was calculated using Olex2, and 174 electrons were
found in a volume of 676\%A^3^ in 1 void per unit cell.
This is consistent with the presence of 1[CHCl3], 0.5[C4H10O] per asymmetric
unit, which accounts for 158 electrons per unit cell. However, the assignment
of solvent content should be regarded as tentative.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              18762
_shelx_hkl_checksum              99830
_shelx_fab_checksum              44409