Synthesis and Biological Activities of Luminescent 5,6-Membered Bis(Metallacyclic) Platinum(II) Complexes
Jing, Jing; Yu, Miao; Pan, Lei; Zhao, Yang; Xu, Guo; Zhang, Hua-Hong; Li, Chen; Zhang, Xiao-Peng; Molecules 28 (2023) 6369–; doi:10.3390/molecules28176369

data_1569819
_publ_section_title
;
 Synthesis and Biological Activities of Luminescent 5,6-Membered
 Bis(Metallacyclic) Platinum(II) Complexes
;
_journal_issue                   17
_journal_name_full               Molecules
_journal_page_first              6369
_journal_paper_doi               10.3390/molecules28176369
_journal_volume                  28
_journal_year                    2023
_chemical_absolute_configuration rm
_chemical_formula_moiety         '2(C38 H35 N4 Pt), C F3 O3 S'
_chemical_formula_sum            'C77 H70 F3 N8 O3 Pt2 S'
_chemical_formula_weight         1634.65
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-25
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_cell_angle_alpha                70.891(2)
_cell_angle_beta                 86.709(2)
_cell_angle_gamma                84.755(2)
_cell_formula_units_Z            1
_cell_length_a                   7.2605(2)
_cell_length_b                   14.3218(3)
_cell_length_c                   18.0040(3)
_cell_measurement_reflns_used    22952
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      35.8280
_cell_measurement_theta_min      2.2070
_cell_volume                     1760.80(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25177
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.059
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             811
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.185(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         11281
_refine_ls_number_restraints     4899
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0138P)^2^+11.9285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.814
_reflns_Friedel_fraction_max     0.814
_reflns_number_gt                10450
_reflns_number_total             11281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            (-)-2.cif
_cod_data_source_block           1
_cod_database_code               1569819
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.563
_shelx_estimated_absorpt_t_min   0.497
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.815(12)
 0.185(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C31-F1 = C31-F3 = C31-F2
 1.33 with sigma of 0.02
 H77B_$1-H37A_$1
 2.1 with sigma of 0.01
 C2-C17
 1.55 with sigma of 0.01
 H17B-H33A
 2.1 with sigma of 0.01
 C33-C65
 1.55 with sigma of 0.01
 C31-S1
 1.82 with sigma of 0.02
 C33-C68
 1.55 with sigma of 0.01
 S1-O1 = S1-O3 = S1-O2
 1.44 with sigma of 0.02
 C75-C71
 1.55 with sigma of 0.01
 C2-C69
 1.55 with sigma of 0.01
 C2-C65
 1.55 with sigma of 0.01
 C67-C65
 1.55 with sigma of 0.01
 C67-C63
 1.55 with sigma of 0.01
 C63-C47
 1.55 with sigma of 0.01
 C2-C63
 1.55 with sigma of 0.01
 C73-C19
 1.5 with sigma of 0.01
 C75-C35
 1.5 with sigma of 0.01
 C73-C71
 1.5 with sigma of 0.01
 C71-C75
 1.5 with sigma of 0.01
 C15-C77
 1.5 with sigma of 0.01
 C71-C70
 1.5 with sigma of 0.01
 C73-C37
 1.5 with sigma of 0.01
 C73-C35
 1.5 with sigma of 0.01
 C35-C77
 1.5 with sigma of 0.01
 C31-O2
 2.57 with sigma of 0.04
 C31-O1
 2.58 with sigma of 0.04
 C31-O3
 2.56 with sigma of 0.04
 C31-O1 \\sim C31-O3 \\sim C31-O2
 with sigma of 0.04
 C31-F1 \\sim C31-F3 \\sim C31-F2
 with sigma of 0.02
 F1-F3 \\sim F3-F2 \\sim F2-F1
 with sigma of 0.04
 S1-F1 \\sim S1-F3 \\sim S1-F2
 with sigma of 0.04
 S1-O1 \\sim S1-O3 \\sim S1-O2
 with sigma of 0.02
 O1-O3 \\sim O3-O2 \\sim O1-O2
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim N3 \\sim N5 \\sim N4 \\sim N6 \\sim N7 \\sim N8 \\sim C1
\\sim C2 \\sim C17 \\sim C20 \\sim C22 \\sim C24 \\sim C26 \\sim C28 \\sim C30
\\sim C25 \\sim C29 \\sim C33 \\sim C40 \\sim C42 \\sim C44 \\sim C46 \\sim C48
\\sim C50 \\sim C52 \\sim C47 \\sim C51 \\sim C13 \\sim C53 \\sim C27 \\sim C55
\\sim C7 \\sim C56 \\sim C57 \\sim C58 \\sim C60 \\sim C61 \\sim C62 \\sim C63
\\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C3 \\sim C4 \\sim C5
\\sim C41 \\sim C21 \\sim C43 \\sim C11 \\sim C45 \\sim C6 \\sim C8 \\sim C10
\\sim C12 \\sim C14 \\sim C16 \\sim C9 \\sim C15 \\sim C18 \\sim C19 \\sim C23
\\sim C32 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C49
\\sim C54 \\sim C59 \\sim C64 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74
\\sim C75 \\sim C76 \\sim C77 \\sim C31: within 5A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 5A
S1 \\sim F1 \\sim F2 \\sim F3 \\sim O1 \\sim O2 \\sim O3 \\sim C31: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 S1, F1, F2, F3, O1, O2, O3, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 C17(H17A,H17B,H17C), C33(H33A,H33B), C77(H77A,H77B)
6.b Ternary CH refined with riding coordinates:
 C63(H63), C65(H65), C35(H35), C71(H71)
6.c Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C75(H75A,H75B)
6.d Aromatic/amide H refined with riding coordinates:
 C24(H24), C26(H26), C28(H28), C30(H30), C40(H40), C42(H42), C44(H44),
 C46(H46), C48(H48), C50(H50), C53(H53), C27(H27), C55(H55), C57(H57), C58(H58),
  C60(H60), C62(H62), C3(H3), C41(H41), C21(H21), C43(H43), C11(H11), C45(H45),
 C6(H6), C8(H8), C10(H10), C12(H12), C9(H9), C23(H23), C38(H38), C39(H39),
 C54(H54), C64(H64), C72(H72)
6.e Fitted hexagon refined as free rotating group:
 C20(C22,C24,C26,C28,C30), C42(C44,C46,C48,C50,C52), C51(C13,C53,C27,C55,C7),
 C5(C41,C21,C43,C11,C45), C6(C8,C10,C12,C14,C16)
6.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C61(H61A,H61B,H61C), C69(H69A,H69B,H69C), C4(H4A,H4B,
 H4C), C19(H19A,H19B,H19C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              379
_shelx_hkl_checksum              22160
_shelx_fab_checksum              16924
_olex2_submission_special_instructions 'No special instructions were received'