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_7706894
_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         'C20 H18 Cl N3 Pd'
_chemical_formula_sum            'C20 H18 Cl N3 Pd'
_chemical_formula_weight         442.22
_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
_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                90
_cell_angle_beta                 101.194(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7186(5)
_cell_length_b                   18.0115(11)
_cell_length_c                   14.8207(10)
_cell_measurement_reflns_used    1714
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      24.8310
_cell_measurement_theta_min      2.6500
_cell_volume                     1759.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.840
_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    -18.00  63.00   1.00    6.00    --   20.02 -99.00-150.00   81
  2  \w    -24.00  90.00   1.00    6.00    --   20.02  19.00-180.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0389876000
_diffrn_orient_matrix_UB_12      -0.0363914000
_diffrn_orient_matrix_UB_13      0.0089788000
_diffrn_orient_matrix_UB_21      0.0674314000
_diffrn_orient_matrix_UB_22      0.0131255000
_diffrn_orient_matrix_UB_23      0.0396578000
_diffrn_orient_matrix_UB_31      -0.0743551000
_diffrn_orient_matrix_UB_32      -0.0072024000
_diffrn_orient_matrix_UB_33      0.0269699000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6580
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.828
_diffrn_reflns_theta_min         1.800
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3859
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0229P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2802
_reflns_number_total             3859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00546d2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7706891--7706895.cif.'
_cod_database_code               7706894
_manchester_internal_coll_name   atc12
_manchester_internal_coll_client FO/SS
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 6s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method \w
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   09/07/2018
_manchester_internal_process_user FO
_manchester_internal_process_date 10/07/2018
_manchester_internal_solution_user FO
_manchester_internal_solution_date 10/07/2018
_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         C22ClN3Pd
_chemical_oxdiff_usercomment     'for TC/SS from UNISS'
_reflns_odcompleteness_completeness 98.63
_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-Cl1 \\sim Pd1-Cl1A
 with sigma of 0.02
 Pd1-C20 \\sim Pd1-C20A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(C20A) = Uanis(Cl1A) = Uanis(C20)
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(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(Cl1)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
6.a Me refined with riding coordinates:
 C20A(H20D,H20E,H20F)
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),
 C16(H16), C17(H17), C18(H18)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              83070
_shelx_hkl_checksum              93315
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.646
_oxdiff_exptl_absorpt_empirical_full_min 0.723