Luminescent ionic heterobimetallic diphosphine-β-diketiminate complexes.
Kebernik, Steven; Krätschmer, Frederic; Sun, Xiaofei; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13192–13199; doi:10.1039/d5dt00977d

data_7719274
_publ_section_title
;
 Luminescent ionic heterobimetallic diphosphine-&#x3b2;-diketiminate
 complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13192
_journal_page_last               13199
_journal_paper_doi               10.1039/d5dt00977d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'F6 Sb, C45 H43 Ag Cl N2 O P2 Zn, 3[C4H8O]'
_chemical_formula_sum            'C57 H67 Ag Cl F6 N2 O4 P2 Sb Zn'
_chemical_formula_weight         1350.50
_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             2025-04-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-24 deposited with the CCDC.	2025-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                91.087(5)
_cell_angle_beta                 94.890(5)
_cell_angle_gamma                100.860(5)
_cell_formula_units_Z            2
_cell_length_a                   12.3341(7)
_cell_length_b                   14.1447(9)
_cell_length_c                   18.6109(13)
_cell_measurement_reflns_used    28544
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      1.69
_cell_volume                     3175.1(4)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
 739 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.0911
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29778
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.688
_exptl_absorpt_coefficient_mu    1.254
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.0585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.976
_refine_diff_density_min         -1.974
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         12392
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0918
_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^)+(0.1766P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2485
_refine_ls_wR_factor_ref         0.2746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7467
_reflns_number_total             12392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00977d2.cif
_cod_data_source_block           stk021
_cod_depositor_comments
'Adding full bibliography for 7719271--7719275.cif.'
_cod_database_code               7719274
_shelx_shelxl_version_number     2019/2
_audit_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_audit_contact_letter
;
;
_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
 P2-C36A \\sim P2-C36
 with sigma of 0.02
 C36A-C37 \\sim C36-C37A
 with sigma of 0.02
 C36A-C41A \\sim C36-C41
 with sigma of 0.02
 C39-C38 \\sim C39A-C38A
 with sigma of 0.02
 C37-C38 \\sim C37A-C38A
 with sigma of 0.02
 P2-C37 \\sim P2-C37A
 with sigma of 0.04
 C40-C41A \\sim C40A-C41
 with sigma of 0.02
 C40-C39 \\sim C40A-C39A
 with sigma of 0.02
 C36A-C38 \\sim C36-C38A
 with sigma of 0.04
 C40-C38 \\sim C40A-C38A
 with sigma of 0.04
 C41A-C37 \\sim C41-C37A
 with sigma of 0.04
 P2-C41A \\sim P2-C41
 with sigma of 0.04
 C39-C37 \\sim C39A-C37A
 with sigma of 0.04
 C36A-C40 \\sim C36-C40A
 with sigma of 0.04
 C41A-C39 \\sim C41-C39A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
H35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41A \\sim C36A
\\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39A)=Sof(H39A)=Sof(C40A)=
 Sof(H40A)=Sof(C41)=Sof(H41)=1-FVAR(1)
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41A)=Sof(H41A)=Sof(C36A)=Sof(C37A)=
 Sof(H37A)=Sof(C38A)=Sof(H38A)=FVAR(1)
 Fixed Sof: Sb1(0.5) F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
  C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41A(H41A), C37A(H37A),
 C38A(H38A), C39A(H39A), C40A(H40A), C41(H41)
5.c Fitted hexagon refined as free rotating group:
 C36(C37,C38,C39,C40,C41A), C36A(C37A,C38A,C39A,C40A,C41)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74641
_shelx_hkl_checksum              47531
_shelx_fab_checksum              61684
_olex2_submission_special_instructions 'No special instructions were received'