Nitron-derivative-based palladium carbene complexes: structural characterization, theoretical calculations, and catalytic applications in the Mizoroki–Heck coupling reaction
Lee, Ming-Yi; Liao, Chih-Hsiang; Hung, Hsiu-Yu; Lee, Jhen-Yi; Lee, Hon Man; RSC Advances 13 (2023) 27434–27445; doi:10.1039/D3RA05016E

data_7247391
_publ_section_title
;
 Nitron-derivative-based palladium carbene complexes: structural
 characterization, theoretical calculations, and catalytic applications in
 the Mizoroki--Heck coupling reaction
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              27434
_journal_page_last               27445
_journal_paper_doi               10.1039/D3RA05016E
_journal_volume                  13
_journal_year                    2023
_chemical_formula_sum            'C38 H54 Cl0 N8 O3 Pd'
_chemical_formula_weight         777.29
_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
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2023-06-29 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.4930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.7355(2)
_cell_length_b                   26.5299(3)
_cell_length_c                   18.7343(2)
_cell_measurement_reflns_used    27593
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.372
_cell_measurement_theta_min      3.3190
_cell_volume                     7604.98(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.33a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.33a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.33a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52932
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.332
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    4.307
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.33a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         12.106
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         13586
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0882
_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^)+(0.1602P)^2^+25.8075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12244
_reflns_number_total             13586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra05016e2.cif
_cod_data_source_block           1c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7247391
_shelx_estimated_absorpt_t_min   0.604
_shelx_estimated_absorpt_t_max   0.782
_shelxl_version_number           2014-3
_shelx_res_checksum              93812