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_7719275
_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         'C45 H43 Au Cl N2 O P2 Zn, F6 Sb, 0.5(C4 H8 O)'
_chemical_formula_sum            'C47 H47 Au Cl F6 N2 O1.5 P2 Sb Zn'
_chemical_formula_weight         1259.34
_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                108.618(5)
_cell_angle_beta                 94.390(6)
_cell_angle_gamma                109.761(5)
_cell_formula_units_Z            2
_cell_length_a                   12.6670(10)
_cell_length_b                   14.0572(10)
_cell_length_c                   15.3543(11)
_cell_measurement_reflns_used    28445
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      1.75
_cell_volume                     2385.6(3)
_computing_cell_refinement
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.192.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.3, Darmstadt 2023
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
 457 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24428
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.890
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    4.313
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5955
_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    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.971
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9301
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7455
_reflns_number_total             9301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00977d2.cif
_cod_data_source_block           stk020
_cod_depositor_comments
'Adding full bibliography for 7719271--7719275.cif.'
_cod_original_formula_sum        'C47 H47 Au Cl F6 N2 O1.50 P2 Sb Zn'
_cod_database_code               7719275
_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
;
;
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.626
_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
 O2-C46 = O2-C49
 1.44 with sigma of 0.02
 C46-C47 = C48-C49
 1.53 with sigma of 0.02
 C47-C48
 1.54 with sigma of 0.02
 O2-C47 = O2-C48 = C46-C48 = C47-C49
 2.38 with sigma of 0.04
 C46-C47 \\sim C47-C48 \\sim C48-C49
 with sigma of 0.02
 O2-C46 \\sim O2-C49
 with sigma of 0.02
 O2-C47 \\sim O2-C48
 with sigma of 0.04
 C47-C49 \\sim C46-C48
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2 \\sim C46 \\sim C47 \\sim C48 \\sim C49: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O2 \\sim O2 \\sim C46 \\sim C46 \\sim C47 \\sim C47 \\sim C48 \\sim C48 \\sim
C49 \\sim C49: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
4. Rigid body (RIGU) restrains
 O2, C46, C47, C48, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O2(0.5) C46(0.5) H46A(0.5) H46B(0.5) C47(0.5) H47A(0.5) H47B(0.5)
 C48(0.5) H48A(0.5) H48B(0.5) C49(0.5) H49A(0.5) H49B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B)
6.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), C25(H25),
  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)
6.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              89826
_shelx_hkl_checksum              47225
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   12.0
_stoe_evaluation_integration_b   -0.1
_stoe_evaluation_integration_ems 0.014
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 6
_stoe_evaluation_lana_bos_l_odd_max 3
_stoe_evaluation_lana_completeness 81.4
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 60.2
_stoe_evaluation_lana_max_2theta_desired 60.2
_stoe_evaluation_lana_mean_redundancy 2.4
_stoe_evaluation_lana_number_refls_after_or 27143
_stoe_evaluation_lana_number_refls_outliers 4158
_stoe_evaluation_lana_number_refls_total 31301
_stoe_evaluation_lana_number_refls_unique 11439
_stoe_evaluation_lana_number_refls_written 27143
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta           6.3   12.7   19.1   25.5   31.9   38.3   44.7   51.1   57.5
<Resolution>    5.52   3.05   2.09   1.59   1.29   1.08   0.94   0.83   0.76
N(total)         179    753   2168   3718   5790   6568   6084   4847   1194
<Redundancy>     2.4    2.5    3.3    3.4    3.5    2.9    2.2    1.6    1.1
Complet. [%%]    96.6   97.8  100.0  100.0  100.0   99.9   99.6   93.6   30.9
<I/sigma>       92.3   58.7   38.0   27.0   17.7   13.0    8.2    4.6    2.8
R(int)         0.044  0.024  0.020  0.022  0.028  0.034  0.056  0.096  0.102
;
_stoe_measurement_identifier     STK020
_stoe_measurement_max_exposure_per_frame '5.0 s'
_stoe_measurement_mean_exposure_per_frame '5.0 s'
_stoe_measurement_min_exposure_per_frame '5.0 s'
_stoe_measurement_total_exposure_time '38 min'
_stoe_measurement_total_frame_number 457
_stoe_measurement_total_run_number 9
_stoe_measurement_tube_power     '49.8 W'