Carbon-carbon bond formation and cleavage at redox active bis(pyridylimino)isoindole (BPI) germylene compounds.
Nicasio, Antonio I.; Somerville, Rosie J.; Sahagún, Pablo; Soto, Enrique; López-Serrano, Joaquín; Campos, Jesús; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3039–3046; doi:10.1039/d4dt03489a

data_7718252
_publ_section_title
;
 Carbon-carbon bond formation and cleavage at redox active
 bis(pyridylimino)isoindole (BPI) germylene compounds.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3039
_journal_page_last               3046
_journal_paper_doi               10.1039/d4dt03489a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C48 H60 Ag2 Ge2 N12 Si4, 2(C2 F6 N O4 S2), 2(C6 H6)'
_chemical_formula_sum            'C64 H72 Ag2 F12 Ge2 N14 O8 S4 Si4'
_chemical_formula_weight         1994.923
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-11-15 deposited with the CCDC.	2025-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                99.488(4)
_cell_angle_beta                 102.293(4)
_cell_angle_gamma                109.977(4)
_cell_formula_units_Z            2
_cell_length_a                   15.8097(14)
_cell_length_b                   16.6796(15)
_cell_length_c                   17.6314(15)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.45
_cell_volume                     4124.1(7)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9934
_diffrn_measurement_device_type  'Apex3 v2016.9-0 (Bruker, 2016)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.9985
_diffrn_reflns_Laue_measured_fraction_max 0.9934
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20453
_diffrn_reflns_point_group_measured_fraction_full 0.9985
_diffrn_reflns_point_group_measured_fraction_max 0.9934
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.92
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1311 before and 0.0982 after correction.
The Ratio of minimum to maximum transmission is 0.7703.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       block
_exptl_crystal_F_000             2008.379
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.4037
_refine_diff_density_min         -1.9845
_refine_diff_density_rms         0.2755
_refine_ls_d_res_high            0.7487
_refine_ls_d_res_low             10.6082
_refine_ls_goodness_of_fit_ref   1.1917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    121
_refine_ls_number_parameters     992
_refine_ls_number_reflns         20453
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.1906
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0926
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2515
_refine_ls_wR_factor_ref         0.3394
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              21
_reflns_limit_k_min              -22
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                12262
_reflns_number_total             20453
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt03489a3.cif
_cod_data_source_block           jcm05321a
_cod_database_code               7718252
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.743(2)
 0.257(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 C59, C60, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C25(H25), C26(H26), C27(H27), C28(H28), C32(H32),
  C33(H33), C34(H34), C35(H35), C39(H39), C40(H40), C41(H41), C42(H42),
 C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C59(H59),
  C64(H64), C63(H63), C62(H62), C61(H61)
4.b Fitted hexagon refined as free rotating group:
 C60(C59,C64,C63,C62,C61)
4.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C43(H43a,H43b,H43c), C44(H44a,
 H44b,H44c), C45(H45a,H45b,H45c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c),
 C48(H48a,H48b,H48c)
;
_olex2_submission_special_instructions 'No special instructions were received'