An α-diiminato germylene family: syntheses, structures, and reactivity towards C-C coupled digermylene and digermylene oxide
Liu, Jingjing; Shang, Jianxuan; Wei, Jing; Gao, Fangfang; Hou, Lei; Zeng, FanLong; Li, Anyang; Wang, Wenyuan; Dalton Transactions  (2022) –; doi:10.1039/D2DT00981A

data_7710146
_publ_section_title
;
 An \a-diiminato germylene family: syntheses, structures, and reactivity
 towards C-C coupled digermylene and digermylene oxide
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00981A
_journal_year                    2022
_chemical_formula_moiety         'C60 H82 Ge2 N4 O, C6 H14'
_chemical_formula_sum            'C66 H96 Ge2 N4 O'
_chemical_formula_weight         1106.64
_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     iterative
_audit_creation_date             2021-09-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-30 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                73.279(18)
_cell_angle_beta                 85.825(19)
_cell_angle_gamma                71.002(18)
_cell_formula_units_Z            2
_cell_length_a                   12.930(5)
_cell_length_b                   15.925(8)
_cell_length_c                   17.049(8)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      53.860
_cell_measurement_theta_min      2.662
_cell_volume                     3178(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      153.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            62124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.940
_diffrn_reflns_theta_min         2.355
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1437 before and 0.0737 after correction. The Ratio of minimum to maximum transmission is 0.8634. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         11632
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0544P)^2^+1.4381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8487
_reflns_number_total             11632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00981a5.cif
_cod_data_source_block           compound7a
_cod_database_code               7710146
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.825
_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
 C64-C65
 1.52 with sigma of 0.01
 H65B-H66C
 2.8 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C46(H46), C25(H25), C55(H55), C58(H58), C43(H43), C13(H13), C16(H16), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C6(H6A,H6B), C34(H34A,H34B), C5(H5A,H5B), C4(H4A,H4B),
 C35(H35A,H35B), C63(H63A,H63B), C64(H64A,H64B), C62(H62A,H62B), C65(H65A,H65B)
3.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C53(H53), C3(H3), C51(H51), C52(H52), C23(H23), C22(H22), C39(H39),
 C11(H11), C41(H41), C9(H9), C40(H40), C21(H21), C10(H10)
3.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C56(H56A,H56B,H56C), C27(H27A,H27B,H27C), C48(H48A,H48B,
 H48C), C57(H57A,H57B,H57C), C26(H26A,H26B,H26C), C60(H60A,H60B,H60C), C59(H59A,
 H59B,H59C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C29(H29A,H29B,H29C), C18(H18A,H18B,
 H18C), C30(H30A,H30B,H30C), C66(H66A,H66B,H66C), C61(H61A,H61B,H61C)
;
_shelx_res_checksum              10483
_olex2_submission_special_instructions 'No special instructions were received'