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_7710144
_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'
_chemical_formula_sum            'C60 H82 Ge2 N4'
_chemical_formula_weight         1004.47
_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             2021-07-24
_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                93.181(3)
_cell_angle_beta                 92.200(3)
_cell_angle_gamma                114.758(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3724(9)
_cell_length_b                   14.6460(9)
_cell_length_c                   15.5895(11)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.982
_cell_measurement_theta_min      2.900
_cell_volume                     2761.9(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      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61048
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.006
_diffrn_reflns_theta_min         2.475
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0864 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.8737.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         10496
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+1.0829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9222
_reflns_number_total             10496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00981a5.cif
_cod_data_source_block           compound6a
_cod_database_code               7710144
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.809
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H6A(0.5) H6B(0.5) H3AA(0.5) H3AB(0.5) H3BC(0.5) H3BD(0.5) H33(0.7)
 H33A(0.3) H36A(0.7) H36B(0.7) H36C(0.3) H36D(0.3) C5(0.5) H5A(0.5) H5B(0.5)
 C34A(0.7) H34A(0.7) H34B(0.7) C35A(0.7) H35A(0.7) H35B(0.7) C4(0.5) H4A(0.5)
 H4B(0.5) C35(0.3) H35C(0.3) H35D(0.3) C34(0.3) H34C(0.3) H34D(0.3) C4A(0.5)
 H4AA(0.5) H4AB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5)
4.a Ternary CH refined with riding coordinates:
 C6(H6A), C6(H6B), C13(H13), C25(H25), C16(H16), C55(H55), C33(H33), C33(H33A),
  C58(H58), C43(H43), C28(H28), C46(H46)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C36(H36A,H36B), C36(H36C,H36D), C5(H5A,H5B),
 C34A(H34A,H34B), C35A(H35A,H35B), C4(H4A,H4B), C35(H35C,H35D), C34(H34C,H34D),
 C4A(H4AA,H4AB), C5A(H5AA,H5AB)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C23(H23), C9(H9), C21(H21), C10(H10), C22(H22), C51(H51), C41(H41),
 C53(H53), C39(H39), C40(H40), C52(H52)
4.d Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C26(H26A,H26B,H26C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C57(H57A,H57B,H57C), C44(H44A,
 H44B,H44C), C60(H60A,H60B,H60C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C),
 C45(H45A,H45B,H45C), C59(H59A,H59B,H59C), C30(H30A,H30B,H30C), C48(H48A,H48B,
 H48C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              85775
_olex2_submission_special_instructions 'No special instructions were received'