Syntheses, structural, photophysical and theoretical studies of heteroleptic cycloplatinated guanidinate(1−) complexes bearing acetylacetonate and picolinate ancillary ligands
Thakur, Vasudha; Thomas, Jisha Mary; Adnan, Mohammad; Sivasankar, Chinnappan; Vijaya Prakash, G.; Thirupathi, Natesan; RSC Advances 14 (2024) 13291–13305; doi:10.1039/D4RA00828F

data_7248521
_publ_section_title
;
 Syntheses, structural, photophysical and theoretical studies of
 heteroleptic cycloplatinated guanidinate(1&#x2212;) complexes bearing
 acetylacetonate and picolinate ancillary ligands
;
_journal_issue                   19
_journal_name_full               'RSC Advances'
_journal_page_first              13291
_journal_page_last               13305
_journal_paper_doi               10.1039/D4RA00828F
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         '2(C30 H35 N3 O2 Pt), C3.25 H4'
_chemical_formula_sum            'C63.25 H74 N6 O4 Pt2'
_chemical_formula_weight         1372.46
_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   mixed
_audit_creation_date             2024-04-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-04 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                93.304(3)
_cell_angle_beta                 98.761(3)
_cell_angle_gamma                104.327(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4667(5)
_cell_length_b                   13.3851(7)
_cell_length_c                   18.9089(6)
_cell_measurement_reflns_used    7070
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.3110
_cell_measurement_theta_min      3.1730
_cell_volume                     3006.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.1309
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40424
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.003
_exptl_absorpt_coefficient_mu    4.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84266
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1367
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12285
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0237P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6413
_reflns_number_total             12285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra00828f3.cif
_cod_data_source_block           Complex-13
_cod_database_code               7248521
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.912
_olex2_refinement_description
;
1. Restrained distances
 C25-C26
 1.51 with sigma of 0.02
 C26-C27 = C26-C31 = C28-C29
 1.39 with sigma of 0.02
 C27-C28 = C29-C30 = C30-C31
 1.38 with sigma of 0.02
 C25-C27 = C25-C31
 2.52 with sigma of 0.04
 C26-C28
 2.42 with sigma of 0.04
 C26-C30
 2.41 with sigma of 0.04
 C27-C29
 2.39 with sigma of 0.04
 C28-C30 = C29-C31
 2.4 with sigma of 0.04
 C26-C27 \\sim C27-C28 \\sim C28-C29 \\sim C29-C30 \\sim C30-C31 \\sim C31-C26
 with sigma of 0.02
 C26-C30 \\sim C26-C28 \\sim C31-C29 \\sim C27-C31 \\sim C28-C30 \\sim C27-C29
 with sigma of 0.04
 C25-C31 \\sim C25-C27
 with sigma of 0.04
2. Restrained planarity
 C25, C26, C27, C28, C29, C30, C31
 with sigma of 0.1
3. Rigid bond restraints
 C7B, C7"
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13B, C13"
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C7B \\sim C7": within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C13B \\sim C13": within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C25, C26, C27, C28, C29, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C26(0.25) C27(0.5) H27(0.5)
 C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5)
7.a Riding coordinates:
 N2A(H2A)
7.b Aromatic/amide H refined with riding coordinates:
 N3A(H3A), C3A(H3AA), C4A(H4A), C6A(H6A), C9A(H9A), C10A(H10A), C12A(H12A),
 C16A(H16A), C18A(H18A), C22A(H22A), N2B(H2B), N3B(H3B), C3B(H3BA), C4B(H4B),
 C6B(H6B), C9B(H9B), C10B(H10B), C12B(H12B), C16B(H16B), C18B(H18B), C22B(H22B),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31)
7.c Idealised Me refined as rotating group:
 C5'(H5'A,H5'B,H5'C), C7'(H7'A,H7'B,H7'C), C11'(H11A,H11B,H11C), C13'(H13A,
 H13B,H13C), C17'(H17A,H17B,H17C), C19'(H19A,H19B,H19C), C20A(H20A,H20B,H20C),
 C24A(H24A,H24B,H24C), C5"(H5"A,H5"B,H5"C), C7"(H7"A,H7"B,H7"C), C11"(H11D,H11E,
 H11F), C13"(H13D,H13E,H13F), C17"(H17D,H17E,H17F), C19"(H19D,H19E,H19F),
 C20B(H20D,H20E,H20F), C24B(H24D,H24E,H24F), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              11846
_olex2_submission_special_instructions 'No special instructions were received'