Carbazolylpyridine (<i>cp</i>)-based tetradentate platinum(II) complexes containing fused 6/5/6 metallocycles.
Zhang, Chengyao; Dou, Lijie; Wang, Xia; Xu, Kewei; Chen, Jianqiang; Zhan, Feng; Li, Guijie; Yang, Yun-Fang; She, Yuanbin; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3256–3265; doi:10.1039/d4dt02743d

data_7717845
_publ_section_title
;
 Carbazolylpyridine (<i>cp</i>)-based tetradentate platinum(II) complexes
 containing fused 6/5/6 metallocycles.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3256
_journal_page_last               3265
_journal_paper_doi               10.1039/d4dt02743d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C45 H42 N4 Pt'
_chemical_formula_sum            'C45 H42 N4 Pt'
_chemical_formula_weight         833.91
_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
_audit_creation_date             2024-09-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-09-02 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                80.219(2)
_cell_angle_beta                 87.400(2)
_cell_angle_gamma                74.135(2)
_cell_formula_units_Z            4
_cell_length_a                   12.2751(6)
_cell_length_b                   16.9466(7)
_cell_length_c                   19.2822(8)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      60.663
_cell_measurement_theta_min      2.390
_cell_volume                     3802.2(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III M28'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'ZJU Bruker D8 VENTURE Metaljet PHOTON III'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.1460
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48123
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.902
_diffrn_reflns_theta_min         2.023
_diffrn_source                   'liquid Metal X-ray source'
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000001
_diffrn_source_type              'Bruker Excillum Metaljet D2+'
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    4.917
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0766 before and 0.0605 after correction.
The Ratio of minimum to maximum transmission is 0.8419.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.651
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.799
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         13879
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      0.796
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0425
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10481
_reflns_number_total             13879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02743d2.cif
_cod_data_source_block           240830_pt_cp_2
_cod_depositor_comments
'Adding full bibliography for 7717844--7717845.cif.'
_cod_database_code               7717845
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.791
_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
 C87-C90 \\sim C87-C90A
 with sigma of 0.02
 C42-C44 \\sim C42-C44A
 with sigma of 0.02
 C87-C89 \\sim C87-C89A
 with sigma of 0.02
 C87-C88 \\sim C87-C88A
 with sigma of 0.02
 C42-C43 \\sim C42-C43A
 with sigma of 0.02
 C42-C45 \\sim C42-C45A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C42 \\sim C43 \\sim C43A \\sim C44 \\sim C44A \\sim C45 \\sim C45A: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C87 \\sim C88 \\sim C88A \\sim C89 \\sim C89A \\sim C90 \\sim C90A: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(C88A) \\sim Ueq, Uanis(C90A) \\sim Ueq, Uanis(C90) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C45A) \\sim Ueq, Uanis(C44A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C88) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C88A)=Sof(H88D)=Sof(H88E)=Sof(H88F)=Sof(C89A)=Sof(H89D)=Sof(H89E)=
 Sof(H89F)=Sof(C90A)=Sof(H90D)=Sof(H90E)=Sof(H90F)=1-FVAR(1)
 Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=
 Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(1)
 Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(2)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C27(H27), C29(H29), C34(H34),
  C36(H36), C37(H37), C46(H46), C47(H47), C48(H48), C56(H56), C57(H57),
 C58(H58), C59(H59), C61(H61), C62(H62), C63(H63), C67(H67), C68(H68), C69(H69),
  C72(H72), C74(H74), C79(H79), C81(H81), C82(H82)
5.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C43A(H43D,H43E,H43F),
 C44(H44A,H44B,H44C), C44A(H44D,H44E,H44F), C45(H45A,H45B,H45C), C45A(H45D,H45E,
 H45F), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C84(H84A,H84B,H84C), C85(H85A,
 H85B,H85C), C86(H86A,H86B,H86C), C88(H88A,H88B,H88C), C88A(H88D,H88E,H88F),
 C89(H89A,H89B,H89C), C89A(H89D,H89E,H89F), C90(H90A,H90B,H90C), C90A(H90D,H90E,
 H90F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'