Palladium hydrazonato complexes and their role in the Pd-catalyzed cross-coupling reactions of hydrazones as carbene precursors
Villalba, Francisco; Albéniz, Ana C.; Dalton Transactions  (2022) –; doi:10.1039/D2DT03251A

data_7711726
_publ_section_title
;
 Palladium hydrazonato complexes and their role in the Pd-catalyzed
 cross-coupling reactions of hydrazones as carbene precursors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03251A
_journal_year                    2022
_chemical_formula_moiety         'C46 H33 F5 Fe O2 P2 Pd S'
_chemical_formula_sum            'C46 H33 F5 Fe O2 P2 Pd S'
_chemical_formula_weight         968.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-07 deposited with the CCDC.	2022-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.506(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9070(6)
_cell_length_b                   10.8331(5)
_cell_length_c                   31.6024(13)
_cell_measurement_reflns_used    5282
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.8370
_cell_measurement_theta_min      3.6960
_cell_volume                     4344.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_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      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.820
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  52.00   1.00   55.16    --   12.51 -99.00-150.00   72
  2  \w     -8.00  83.00   1.00   55.16    --   12.51  37.00 -30.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0463713000
_diffrn_orient_matrix_UB_12      0.0243259000
_diffrn_orient_matrix_UB_13      -0.0127536000
_diffrn_orient_matrix_UB_21      -0.0300646000
_diffrn_orient_matrix_UB_22      -0.0224369000
_diffrn_orient_matrix_UB_23      0.0150569000
_diffrn_orient_matrix_UB_31      0.0080370000
_diffrn_orient_matrix_UB_32      0.0565738000
_diffrn_orient_matrix_UB_33      0.0114570000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19107
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.784
_diffrn_reflns_theta_min         3.377
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
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_colour_primary    yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       prism
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+0.8065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7008
_reflns_number_total             10169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03251a2.cif
_cod_data_source_block           fv1328c
_cod_database_code               7711726
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C46 H33 F5 Fe O2 P2 S Pd'
_chemical_oxdiff_usercomment     yellow
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.709
_reflns_odcompleteness_completeness 98.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00H(H00H), C00I(H00I), C00M(H00M), C00N(H00N), C00O(H00O),
 C00P(H00P), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C010(H010), C012(H012), C014(H014), C015(H015),
 C016(H016), C017(H017), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C),
 C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01M(H01M),
 C01N(H01N), C01O(H01O), C01P(H01P)
;
_shelx_res_checksum              14053
_shelx_hkl_checksum              27895
_shelx_fab_checksum              78185
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.242
_oxdiff_exptl_absorpt_empirical_full_min 0.789