Strongly emitting Ge(II) imide complexes.
Kryuchenkova, Alina A.; Ilichev, Vasily A.; Rumyantsev, Roman V.; Zhao, Yanxia; Dodonov, Vladimir A.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16605–16610; doi:10.1039/d5dt02112j

data_7719697
_publ_section_title
;
 Strongly emitting Ge(II) imide complexes.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16605
_journal_page_last               16610
_journal_paper_doi               10.1039/d5dt02112j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C74 H70 Ge2 N2, 2(C7 H8)'
_chemical_formula_sum            'C88 H86 Ge2 N2'
_chemical_formula_weight         1316.76
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2024-11-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-25 deposited with the CCDC.	2025-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                62.520(4)
_cell_angle_beta                 80.734(4)
_cell_angle_gamma                70.827(4)
_cell_formula_units_Z            1
_cell_length_a                   11.6472(5)
_cell_length_b                   13.1169(8)
_cell_length_c                   14.0288(9)
_cell_measurement_reflns_used    9743
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      51.33
_cell_measurement_theta_min      5.62
_cell_volume                     1795.85(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_number            5737
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        51.276
_diffrn_reflns_theta_max         51.276
_diffrn_reflns_theta_min         4.135
_diffrn_source_current           2.86
_diffrn_source_power             0.1997996
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5737
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0891P)^2^+1.5129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5493
_reflns_number_total             5737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02112j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7719697--7719698.cif.'
_cod_database_code               7719697
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.843
_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
 C38-C39
 1.51 with sigma of 0.02
 C39-C40 = C39-C44 = C41-C42
 1.39 with sigma of 0.02
 C40-C41 = C42-C43 = C43-C44
 1.38 with sigma of 0.02
 C45-C46
 1.51 with sigma of 0.02
 C46-C47 = C46-C51 = C48-C49
 1.39 with sigma of 0.02
 C47-C48 = C49-C50 = C50-C51
 1.38 with sigma of 0.02
 C38-C40 = C38-C44
 2.52 with sigma of 0.04
 C39-C41
 2.42 with sigma of 0.04
 C39-C43
 2.41 with sigma of 0.04
 C40-C42
 2.39 with sigma of 0.04
 C41-C43 = C42-C44
 2.4 with sigma of 0.04
 C45-C47 = C45-C51
 2.52 with sigma of 0.04
 C46-C48
 2.42 with sigma of 0.04
 C46-C50
 2.41 with sigma of 0.04
 C47-C49
 2.39 with sigma of 0.04
 C48-C50 = C49-C51
 2.4 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C38) = Uanis(C39) = Uanis(C40) = Uanis(C41) = Uanis(C42) = Uanis(C43) =
Uanis(C44)
Uanis(C51) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48) = Uanis(C50) =
Uanis(C49)
4. Others
 Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Fixed Sof: C38(0.5) H38C(0.5) H38B(0.5) H38A(0.5) C39(0.5) C40(0.5) H40(0.5)
 C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5)
 C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C46(0.5) C51(0.5) H51(0.5) C50(0.5)
 H50(0.5) C49(0.5) H49(0.5) C48(0.5) H48(0.5) C47(0.5) H47(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C23(H23)
5.b Me refined with riding coordinates:
 C38(H38C,H38B,H38A), C45(H45A,H45B,H45C)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C3(H3), C16(H16), C5(H5), C20(H20), C29(H29), C26(H26), C9(H9),
 C13(H13), C33(H33), C19(H19), C32(H32), C10(H10), C28(H28), C36(H36), C17(H17),
  C12(H12), C35(H35), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
 C51(H51), C50(H50), C49(H49), C48(H48), C47(H47)
5.d Fitted hexagon refined as free rotating group:
 C39(C40,C41,C42,C43,C44), C46(C51,C50,C49,C48,C47)
5.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C37(H37A,H37B,H37C), C30(H30A,H30B,H30C), C30(H30D,H30E,
 H30F), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              95682
_shelx_hkl_checksum              10312
_olex2_submission_special_instructions 'No special instructions were received'