Visualizing supramolecular assembly behavior, stimulus response, and solid state emission of higher-order Pt<sup>2+</sup> aggregates.
Li, Jing; Xu, Bao-Sen; Yi, Shao-Zhe; Zhang, Xing-Long; Zhao, Le-Le; Meng, Yu; Wang, Wen-Jin; Li, Bao-Ning; Dalton transactions (Cambridge, England : 2003) 54 (2024) 357–367; doi:10.1039/d4dt02771j

data_7717514
_publ_section_title
;
 Visualizing supramolecular assembly behavior, stimulus response, and
 solid state emission of higher-order Pt<sup>2+</sup> aggregates.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              357
_journal_page_last               367
_journal_paper_doi               10.1039/d4dt02771j
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         '4(C20 H18 N3 Pt), Ag2 N8 O24, 2(C2 H3 N)'
_chemical_formula_sum            'C84 H78 Ag2 N22 O24 Pt4'
_chemical_formula_weight         2775.78
_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     iterative
_audit_creation_date             2020-11-13
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-11-20 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.0790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6693(2)
_cell_length_b                   18.7992(2)
_cell_length_c                   27.1249(3)
_cell_measurement_reflns_used    11569
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      71.8140
_cell_measurement_theta_min      3.8260
_cell_volume                     9004.11(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.959
_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   -110.00 -23.00   1.00    5.00    --  -40.20 -57.00-150.00   87
  2  \w    -82.00  -8.00   1.00    5.00    --  -40.20 125.00 -90.00   74
  3  \w     32.00  94.00   1.00    5.00    --   40.20-125.00-120.00   62
  4  \w     57.00 124.00   1.00   20.00    --  102.03 -45.00-120.00   67
  5  \w    139.00 178.00   1.00   20.00    --  102.03  77.00-120.00   39
  6  \w     80.00 165.00   1.00   20.00    --  102.03  45.00-120.00   85
  7  \w    103.00 178.00   1.00   20.00    --  102.03  77.00 -30.00   75
  8  \w     28.00 135.00   1.00   20.00    --  102.03 -77.00  30.00  107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0870740000
_diffrn_orient_matrix_UB_12      -0.0033113000
_diffrn_orient_matrix_UB_13      -0.0038939000
_diffrn_orient_matrix_UB_21      -0.0029220000
_diffrn_orient_matrix_UB_22      0.0804795000
_diffrn_orient_matrix_UB_23      -0.0106525000
_diffrn_orient_matrix_UB_31      0.0034119000
_diffrn_orient_matrix_UB_32      -0.0151866000
_diffrn_orient_matrix_UB_33      -0.0557139000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31901
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.883
_diffrn_reflns_theta_min         3.434
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.491
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_description       block
_exptl_crystal_F_000             5336
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         9.105
_refine_diff_density_min         -7.407
_refine_diff_density_rms         0.395
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.435
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1101
_refine_ls_number_reflns         16939
_refine_ls_number_restraints     804
_refine_ls_restrained_S_all      1.406
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.1012
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3140
_refine_ls_wR_factor_ref         0.3422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13866
_reflns_number_total             16939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02771j2.cif
_cod_data_source_block           exp_4544
_cod_depositor_comments
'Adding full bibliography for 7717514--7717515.cif.'
_cod_database_code               7717514
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.167
_shelx_estimated_absorpt_t_min   0.107
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
 O23-N7
 1.582 with sigma of 0.02
 C83-C84
 1.45 with sigma of 0.02
 N9-C83
 1.18 with sigma of 0.02
 C20-C19
 1.43 with sigma of 0.02
 C8-C7
 1.5 with sigma of 0.02
 O11-N4 \\sim O12-N4 \\sim O10-N4
 with sigma of 0.02
 O5-N2 \\sim O6-N2 \\sim O4-N2
 with sigma of 0.02
 C11-C10 \\sim C8-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Pt1 \\sim N11 \\sim N12 \\sim N13 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5
\\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13
\\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim Pt2
\\sim N14 \\sim N15 \\sim N16 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim Pt3
\\sim N17 \\sim N18 \\sim N19 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45
\\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53
\\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim Pt4
\\sim N20 \\sim N21 \\sim N22 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim Ag1
\\sim Ag2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim
O8 \\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim
O16 \\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim
O24 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8
\\sim N9 \\sim C83 \\sim C84: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C33) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C13) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C13) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N7) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C83) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O17) = Uanis(O16) = Uanis(O18) = Uanis(O23) = Uanis(O19) = Uanis(O22) =
Uanis(O20) = Uanis(O21) = Uanis(O24) = Uanis(O13) = Uanis(O15) = Uanis(O14) =
Uanis(O12) = Uanis(O10) = Uanis(O11) = Uanis(O8) = Uanis(O7) = Uanis(O9) =
Uanis(O4) = Uanis(O5) = Uanis(O6) = Uanis(O3) = Uanis(O2) = Uanis(O1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C15(H15), C16(H16), C17(H17),
 C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C29(H29), C35(H35), C36(H36),
  C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C49(H49),
 C55(H55), C56(H56), C57(H57), C58(H58), C61(H61), C62(H62), C63(H63), C64(H64),
  C69(H69), C75(H75), C76(H76), C77(H77), C78(H78)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C28(H28A,H28B,
 H28C), C31(H31A,H31B,H31C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C51(H51A,
 H51B,H51C), C60(H60A,H60B,H60C), C68(H68A,H68B,H68C), C71(H71A,H71B,H71C),
 C80(H80A,H80B,H80C), C84(H84A,H84B,H84C), C82(H82A,H82B,H82C)
;
_shelx_res_checksum              5161
_shelx_hkl_checksum              23194
_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 5.098
_oxdiff_exptl_absorpt_empirical_full_min 0.490