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_7710147
_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_sum            'C120 H164 Ge4 N8 O2'
_chemical_formula_weight         2040.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4853(5)
_cell_length_b                   24.7376(13)
_cell_length_c                   34.1042(18)
_cell_measurement_reflns_used    9021
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.84
_cell_measurement_theta_min      3.64
_cell_volume                     11377.0(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_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  0.0814
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            142714
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.911
_diffrn_reflns_theta_min         1.919
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       block
_exptl_crystal_F_000             4336
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 7976 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1270
_refine_ls_number_reflns         21579
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0468P)^2^+3.3558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                19183
_reflns_number_total             21579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00981a5.cif
_cod_data_source_block           compound7
_cod_database_code               7710147
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.854
_shelx_estimated_absorpt_t_max   0.899
_shelx_res_checksum              24572