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_7706891
_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         'C19 H15 Cl2 N3 Pt'
_chemical_formula_sum            'C19 H15 Cl2 N3 Pt'
_chemical_formula_weight         551.33
_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                 99.3310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.24510(10)
_cell_length_b                   11.86360(10)
_cell_length_c                   20.2553(2)
_cell_measurement_reflns_used    7157
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.7760
_cell_measurement_theta_min      4.3210
_cell_volume                     1717.97(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_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    -44.00 118.00   0.50    0.50    --   37.90  39.00 -52.00  324
  2  \w     28.00 190.00   0.50    0.50    --  109.60  39.00 -52.00  324
  3  \w    -45.00 118.00   0.50    0.50    --   37.90  60.00-150.00  326
  4  \w     28.00 191.00   0.50    0.50    --  109.60  60.00-120.00  326
  5  \w     28.00 191.00   0.50    0.50    --  109.60  60.00  30.00  326
  6  \w     27.00 189.00   0.50    0.50    --  109.60  60.00  90.00  324
  7  \w     28.00 190.00   0.50    0.50    --  109.60  60.00-180.00  324
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0032575000
_diffrn_orient_matrix_UB_12      -0.1282104000
_diffrn_orient_matrix_UB_13      -0.0115422000
_diffrn_orient_matrix_UB_21      -0.0742087000
_diffrn_orient_matrix_UB_22      -0.0195202000
_diffrn_orient_matrix_UB_23      0.0661314000
_diffrn_orient_matrix_UB_31      -0.2025124000
_diffrn_orient_matrix_UB_32      0.0050909000
_diffrn_orient_matrix_UB_33      -0.0378294000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9235
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         4.334
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.980
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0388P)^2^+1.2184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2916
_reflns_number_total             3102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00546d2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7706891--7706895.cif.'
_cod_database_code               7706891
_manchester_internal_coll_name   ldpm9
_manchester_internal_coll_client FO/TC
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 0.5s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   8/7/17
_manchester_internal_process_user FO
_manchester_internal_process_date 8/7/17
_manchester_internal_solution_user FO
_manchester_internal_solution_date 8/7/17
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 18/12/20
_manchester_internal_validation_user FO
_manchester_internal_validation_date 18/12/20
_manchester_internal_archive_date 18/12/20
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19ClN3Pt
_reflns_odcompleteness_completeness 98.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
2.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), C19(H19)
;
_shelx_res_checksum              80880
_shelx_hkl_checksum              76940
_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 4.043
_oxdiff_exptl_absorpt_empirical_full_min 0.538