Cyclometalated luminescent platinum(II) complexes of dissymmetrical 2,2':4',2''-terpyridine and its self-assembled dimer presenting Pt-Ag dative bonds.
Benda, Lorien; Miton, Louise; Hadj Seyd, Nihal; Chamoreau, Lise-Marie; Jonusauskas, Gediminas; McClenaghan, Nathan D.; Hasenknopf, Bernold; Marvaud, Valérie; Vives, Guillaume; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12477–12485; doi:10.1039/d4dt01153h

data_7716407
_publ_section_title
;
 Cyclometalated luminescent platinum(II) complexes of dissymmetrical
 2,2':4',2''-terpyridine and its self-assembled dimer presenting Pt-Ag
 dative bonds.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12477
_journal_page_last               12485
_journal_paper_doi               10.1039/d4dt01153h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C83 H95 Ag F3 N10 O3 Pt2 S, 2(C F3 O3 S), 2.5(C H Cl3)'
_chemical_formula_sum            'C87.5 H97.5 Ag Cl7.5 F9 N10 O9 Pt2 S3'
_chemical_formula_weight         2464.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.542(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4562(9)
_cell_length_b                   42.508(3)
_cell_length_c                   15.6202(12)
_cell_measurement_reflns_used    4911
_cell_measurement_temperature    200
_cell_measurement_theta_max      45.54
_cell_measurement_theta_min      3.12
_cell_volume                     9887.4(12)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1455
_diffrn_reflns_av_unetI/netI     0.1398
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36015
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        47.263
_diffrn_reflns_theta_max         47.263
_diffrn_reflns_theta_min         3.599
_diffrn_source_current           0.65
_diffrn_source_power             0.02925
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.854
_exptl_absorpt_correction_T_max  0.7493
_exptl_absorpt_correction_T_min  0.4831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.6447.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       needle
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.223
_refine_diff_density_min         -1.793
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8823
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1900
_refine_ls_R_factor_gt           0.1270
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+621.2064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2911
_refine_ls_wR_factor_ref         0.3264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5114
_reflns_number_total             8823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01153h2.cif
_cod_data_source_block           lm010_0m
_cod_depositor_comments
'Adding full bibliography for 7716407--7716408.cif.'
_cod_original_cell_volume        9887.5(12)
_cod_original_formula_sum        'C87.50 H97.50 Ag Cl7.50 F9 N10 O9 Pt2 S3'
_cod_database_code               7716407
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. 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
2. Restrained distances
 Cl8-C63 = Cl7-C63 = Cl4-C63
 1.78 with sigma of 0.02
 C56-C58B
 1.54 with sigma of 0.02
 C88-Cl9
 1.84 with sigma of 0.02
 C88-Cl15
 1.84 with sigma of 0.02
 C8-F7 = C8-F10 = C8-F11
 1.33 with sigma of 0.02
 C8-S6
 1.82 with sigma of 0.02
 S6-O8 = S6-O10 = S6-O11
 1.44 with sigma of 0.02
 C8-O8
 2.58 with sigma of 0.04
 C8-O10
 2.56 with sigma of 0.04
 C8-O11
 2.57 with sigma of 0.04
 Cl9-C88 \\sim Cl10-C88 \\sim Cl12-C88 \\sim Cl14-C88 \\sim Cl13-C88
 with sigma of 0.02
 C8-F7 \\sim C8-F10 \\sim C8-F11
 with sigma of 0.02
 F7-F10 \\sim F10-F11 \\sim F11-F7
 with sigma of 0.04
 S6-F7 \\sim S6-F10 \\sim S6-F11
 with sigma of 0.04
 S6-O8 \\sim S6-O10 \\sim S6-O11
 with sigma of 0.02
 O8-O10 \\sim O10-O11 \\sim O8-O11
 with sigma of 0.04
 C8-O8 \\sim C8-O10 \\sim C8-O11
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl3 \\sim Cl11 \\sim Cl1 \\sim Cl6 \\sim Cl5: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 1.7A
C8 \\sim F7 \\sim F10 \\sim F11 \\sim S6 \\sim O8 \\sim O10 \\sim O11: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uiso(C57) = Uiso(C57A)
Uiso(C62) = Uiso(C62A)
Uiso(C62A) = Uiso(C62)
Uiso(C60) = Uiso(C60A)
Uiso(C59) = Uiso(C59A)
Uiso(C55) = Uiso(C55A)
Uiso(C62A) = Uiso(C62B)
4. Rigid body (RIGU) restrains
 C8, F7, F10, F11, S6, O8, O10, O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C54(0.6) H54A(0.6) H54B(0.6) C55(0.4) H55A(0.4) H55B(0.4) C56(0.4)
 H56(0.4) C58(0.6) H58A(0.6) H58B(0.6) C57(0.4) H57A(0.4) H57B(0.4) C59(0.6)
 H59A(0.6) H59B(0.6) C61(0.6) H61A(0.6) H61B(0.6) C60(0.6) H60(0.6) Cl1(0.5)
 Cl11(0.5) Cl3(0.5) Cl5(0.5) Cl6(0.5) H86A(0.5) H86(0.5) Cl10(0.5) Cl14(0.5)
 Cl9(0.5) H88A(0.5) H88(0.5) C61B(0.4) H61C(0.4) H61D(0.4) C58B(0.4) H58C(0.4)
 H58D(0.4) C54B(0.4) H54C(0.4) H54D(0.4) Cl7(0.5) Cl8(0.5) Cl4(0.5) C63(0.5)
 H63(0.5) C62(0.6) H62(0.6) Cl2(0.5) Cl13(0.5) Cl12(0.5) Cl15(0.5) C57A(0.6)
 H57C(0.6) C55A(0.6) H55C(0.6) C59A(0.4) H59C(0.4) C60A(0.4) H60A(0.4)
 C62A(0.4) H62A(0.4) C62B(0.6) H62B(0.6) H62C(0.6)
6.a Ternary CH refined with riding coordinates:
 C44(H44), C46(H46), C49(H49), C56(H56), C60(H60), C67(H67), C69(H69),
 C72(H72), C78(H78), C80(H80), C83(H83), C86(H86A), C86(H86), C88(H88A),
 C88(H88), C63(H63), C62(H62), C55A(H55C), C59A(H59C), C62A(H62A)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C45(H45A,H45B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,
 H50B), C51(H51A,H51B), C54(H54A,H54B), C55(H55A,H55B), C58(H58A,H58B),
 C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B), C66(H66A,H66B), C68(H68A,H68B),
  C70(H70A,H70B), C71(H71A,H71B), C73(H73A,H73B), C74(H74A,H74B), C77(H77A,
 H77B), C79(H79A,H79B), C81(H81A,H81B), C82(H82A,H82B), C84(H84A,H84B),
 C85(H85A,H85B), C61B(H61C,H61D), C58B(H58C,H58D), C54B(H54C,H54D), C62B(H62B,
 H62C)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C13(H13), C14(H14), C15(H15),
 C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C33(H33), C34(H34),
  C35(H35), C36(H36), C57A(H57C), C60A(H60A)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              58378
_shelx_hkl_checksum              56611
_olex2_submission_special_instructions 'No special instructions were received'