Metal phosphine aldehyde complexes and their application in Cu-free Sonogashira and Suzuki-Miyaura cross-coupling reactions
Baweja, Saral; Gabler, Tom; Lönnecke, Peter; Hey-Hawkins, Evamarie; Dalton Transactions  (2023) –; doi:10.1039/D3DT00507K

data_7712775
_publ_section_title
;
 Metal phosphine aldehyde complexes and their application in Cu-free
 Sonogashira and Suzuki-Miyaura cross-coupling reactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00507K
_journal_year                    2023
_chemical_formula_moiety         'C30 H30 Cl2 O2 P2 Pd'
_chemical_formula_sum            'C30 H30 Cl2 O2 P2 Pd'
_chemical_formula_weight         661.78
_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   difmap
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_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2023-01-02 deposited with the CCDC.	2023-04-17 downloaded from the CCDC.
;
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_cell_angle_gamma                96.825(2)
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_cell_length_b                   10.1292(2)
_cell_length_c                   10.4543(3)
_cell_measurement_reflns_used    10349
_cell_measurement_temperature    130(2)
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_cell_measurement_theta_min      2.4910
_cell_volume                     715.62(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics
;
 ORTEP3 for Windows
 L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
 or
 DIAMOND Version 4.5.3
 K. Brandenburg, Crystal Impact GbR, Bonn, Germany
;
_computing_publication_material
;
 WINGX
 L.J. Farrugia,
 J. Appl. Cryst., 2012, 45, 849-854.
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
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_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
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_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17006
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        33.140
_diffrn_reflns_theta_max         34.755
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       prism
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         5761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0229P)^2^+0.3720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5328
_reflns_number_total             5761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00507k2.cif
_cod_data_source_block           comp2_x3373fin
_cod_database_code               7712775
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              23600
_shelx_hkl_checksum              97556