Precious metal complexes of bis(pyridyl)allenes: synthesis and catalytic and medicinal applications
Maliszewska, Hanna K.; Arnau del Valle, Carla; Xia, Ying; Marín, María J.; Waller, Zoë A. E.; Muñoz, María Paz; Dalton Transactions  (2021) –; doi:10.1039/D1DT02929K

data_7708794
_publ_section_title
;
 Precious metal complexes of bis(pyridyl)allenes: synthesis and catalytic
 and medicinal applications
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02929K
_journal_year                    2021
_chemical_formula_moiety         'C25 H26 Cl2 N2 Pd'
_chemical_formula_sum            'C25 H26 Cl2 N2 Pd'
_chemical_formula_weight         531.78
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-07-06 deposited with the CCDC.	2021-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.017(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3560(3)
_cell_length_b                   14.1423(4)
_cell_length_c                   17.5530(5)
_cell_measurement_reflns_used    21971
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1750
_cell_measurement_theta_min      2.2200
_cell_volume                     2262.85(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.799
_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    -77.00  11.00   0.50   11.71    --   -4.50 -58.00 -44.00  176
  2  \w      0.00  26.00   0.50   11.71    --   -4.50 -99.00   0.00   52
  3  \w    -21.00   5.00   0.50   11.71    --   -4.50 -77.00  60.00   52
  4  \w      2.00  28.00   0.50   11.71    --   -4.50 -99.00 120.00   52
  5  \w    -20.00  68.00   0.50   11.71    --   -4.50  58.00  97.00  176
  6  \w    -10.00  47.00   0.50   11.71    --    4.11  57.00 120.00  114
  7  \w      2.00  28.00   0.50   11.71    --    4.11 -99.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0258246000
_diffrn_orient_matrix_UB_12      -0.0309322000
_diffrn_orient_matrix_UB_13      -0.0257671000
_diffrn_orient_matrix_UB_21      -0.0728686000
_diffrn_orient_matrix_UB_22      -0.0154838000
_diffrn_orient_matrix_UB_23      -0.0156604000
_diffrn_orient_matrix_UB_31      -0.0089089000
_diffrn_orient_matrix_UB_32      0.0363229000
_diffrn_orient_matrix_UB_33      -0.0284765000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26885
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.997
_diffrn_reflns_theta_min         2.234
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method
'vapour diffusion of dichloromethane/MeOH solution and n-Hex at 4 \%C'
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0210P)^2^+2.4440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5379
_reflns_number_total             5767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02929k2.cif
_cod_data_source_block           hm_233b_2
_cod_database_code               7708794
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H104 Cl8 N8 Pd4 '
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.718
_diffrn_oxdiff_digest_frames
;
019446f0bfe512f9b8df72e988ff815421000258f1f
;
_diffrn_oxdiff_digest_hkl
;
019fc68e755b3772f4203a70db6594ba45e637
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00D(H00D), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00N(H00N), C00P(H00P), C00R(H00S), C00T(H00W)
2.b Idealised Me refined as rotating group:
 C00M(H00A,H00C,H00E), C00O(H00F,H00L,H00M), C00Q(H00O,H00Q,H00R), C00S(H00T,
 H00U,H00V), C00U(H00X,H00Y,H)
;
_shelx_res_checksum              8041
_shelx_hkl_checksum              67897
_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 1.640
_oxdiff_exptl_absorpt_empirical_full_min 0.515