Synthesis and characterization of new Pd(ii) and Pt(ii) complexes with 3-substituted 1-(2-pyridyl)imidazo[1,5-a]pyridine ligands.
Pischedda, Sara; Stoccoro, Sergio; Zucca, Antonio; Sciortino, Giuseppe; Ortu, Fabrizio; Clarkson, Guy J.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4859–4873; doi:10.1039/d1dt00546d

data_7706893
_publ_section_title
;
 Synthesis and characterization of new Pd(ii) and Pt(ii) complexes with
 3-substituted 1-(2-pyridyl)imidazo[1,5-a]pyridine ligands.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4859
_journal_page_last               4873
_journal_paper_doi               10.1039/d1dt00546d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C22 H22 Cl N3 Pd'
_chemical_formula_sum            'C22 H22 Cl N3 Pd'
_chemical_formula_weight         470.27
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-02-06 deposited with the CCDC.	2021-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                73.015(8)
_cell_angle_beta                 80.802(7)
_cell_angle_gamma                85.043(7)
_cell_formula_units_Z            2
_cell_length_a                   8.6794(7)
_cell_length_b                   10.7831(9)
_cell_length_c                   10.8932(9)
_cell_measurement_reflns_used    2329
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.8480
_cell_measurement_theta_min      1.9690
_cell_volume                     961.65(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.750
_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    -15.00  27.00   1.00    3.00    --   -7.80 -66.00 173.00   42
  2  \w    -80.00 -27.00   1.00    3.00    --   -7.80 -66.00 173.00   53
  3  \w    -28.00  65.00   1.00    3.00    --    5.00  57.00-120.00   93
  4  \w    -31.00  72.00   1.00    3.00    --   -7.80  57.00  30.00  103
  5  \w    -21.00  38.00   1.00    3.00    --   -7.80  66.00 -52.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0286118000
_diffrn_orient_matrix_UB_12      0.0521957000
_diffrn_orient_matrix_UB_13      0.0257686000
_diffrn_orient_matrix_UB_21      -0.0554449000
_diffrn_orient_matrix_UB_22      -0.0408643000
_diffrn_orient_matrix_UB_23      0.0453259000
_diffrn_orient_matrix_UB_31      0.0545258000
_diffrn_orient_matrix_UB_32      -0.0185650000
_diffrn_orient_matrix_UB_33      0.0448476000
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0803
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.750
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10385
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.654
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.40a (Rigaku Oxford Diffraction, 2019)
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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       plate
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4473
_refine_ls_number_restraints     247
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0364P)^2^+0.0958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3359
_reflns_number_total             4473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00546d2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7706891--7706895.cif.'
_cod_database_code               7706893
_manchester_internal_coll_name   rtc1
_manchester_internal_coll_client FO/SS
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 3s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method \w
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   18/07/2018
_manchester_internal_process_user FO
_manchester_internal_process_date 30/04/2019
_manchester_internal_solution_user FO
_manchester_internal_solution_date 30/04/2019
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 18/12/2020
_manchester_internal_validation_user FO
_manchester_internal_validation_date 18/12/2020
_manchester_internal_archive_date 18/12/2020
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'PtC30 Cl'
_reflns_odcompleteness_completeness 98.37
_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. Restrained distances
 Pd1-Cl1A \\sim Pd1-Cl1
 with sigma of 0.02
 Pd1-C22A \\sim Pd1-C22
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1A) = Uanis(C22) = Uanis(Cl1) = Uanis(C22A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1A)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(Cl1)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
6.a Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C22A(H22D,H22E,H22F)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15),
 C17(H17)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              63185
_shelx_hkl_checksum              49001
_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 1.555
_oxdiff_exptl_absorpt_empirical_full_min 0.788