#------------------------------------------------------------------------------
#$Date: 2022-05-03 02:15:34 +0300 (Tue, 03 May 2022) $
#$Revision: 274814 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/01/7710143.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7710143
loop_
_publ_author_name
'Liu, Jingjing'
'Shang, Jianxuan'
'Wei, Jing'
'Gao, Fangfang'
'Hou, Lei'
'Zeng, FanLong'
'Li, Anyang'
'Wang, Wenyuan'
_publ_section_title
;
 An α-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         'C30 H40 Ge N2'
_chemical_formula_sum            'C30 H40 Ge N2'
_chemical_formula_weight         501.23
_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             2021-04-08
_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                101.563(2)
_cell_angle_beta                 90.578(2)
_cell_angle_gamma                98.666(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9419(5)
_cell_length_b                   11.8530(7)
_cell_length_c                   13.4458(7)
_cell_measurement_reflns_used    8096
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      54.79
_cell_measurement_theta_min      3.97
_cell_volume                     1379.04(13)
_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)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21154
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.692
_diffrn_reflns_theta_min         1.547
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5616
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1402 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.7480.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0528P)²+1.3393P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4232
_reflns_number_total             5236
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00981a5.cif
_cod_data_source_block           compound4
_cod_database_code               7710143
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.765
_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.a Ternary CH refined with riding coordinates:
 C16(H16), C13(H13), C25(H25), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C11(H11), C23(H23), C10(H10), C22(H22), C9(H9), C21(H21)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C15(H15A,H15B,
 H15C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C29(H29A,
 H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.04081(4) 0.16291(3) 0.24651(2) 0.03451(13) Uani 1 1 d . . . . .
N1 N 0.0989(3) 0.27214(19) 0.16726(16) 0.0238(5) Uani 1 1 d . . . . .
N2 N 0.1796(3) 0.25627(19) 0.34359(16) 0.0232(5) Uani 1 1 d . . . . .
C19 C 0.2299(3) 0.2266(2) 0.4355(2) 0.0251(6) Uani 1 1 d . . . . .
C2 C 0.2556(3) 0.3571(2) 0.31563(19) 0.0224(6) Uani 1 1 d . . . . .
C7 C 0.0432(3) 0.2632(2) 0.06448(19) 0.0236(6) Uani 1 1 d . . . . .
C1 C 0.2048(3) 0.3688(2) 0.21412(19) 0.0221(6) Uani 1 1 d . . . . .
C8 C -0.0890(3) 0.3085(2) 0.0472(2) 0.0267(6) Uani 1 1 d . . . . .
C12 C 0.1203(3) 0.2062(2) -0.0162(2) 0.0258(6) Uani 1 1 d . . . . .
C24 C 0.3553(3) 0.1662(2) 0.4317(2) 0.0280(6) Uani 1 1 d . . . . .
C16 C -0.1705(4) 0.3737(3) 0.1336(2) 0.0325(7) Uani 1 1 d . . . . .
H16 H -0.1013 0.3930 0.1956 0.039 Uiso 1 1 calc R . . . .
C3 C 0.3667(3) 0.4357(2) 0.3696(2) 0.0285(6) Uani 1 1 d . . . . .
H3 H 0.3945 0.4292 0.4364 0.034 Uiso 1 1 calc R . . . .
C6 C 0.2543(3) 0.4640(3) 0.1777(2) 0.0310(7) Uani 1 1 d . . . . .
H6 H 0.2268 0.4673 0.1100 0.037 Uiso 1 1 calc R . . . .
C11 C 0.0582(4) 0.1892(3) -0.1140(2) 0.0309(7) Uani 1 1 d . . . . .
H11 H 0.1075 0.1490 -0.1694 0.037 Uiso 1 1 calc R . . . .
C23 C 0.4060(4) 0.1415(3) 0.5224(2) 0.0347(7) Uani 1 1 d . . . . .
H23 H 0.4912 0.1024 0.5224 0.042 Uiso 1 1 calc R . . . .
C10 C -0.0752(4) 0.2301(3) -0.1320(2) 0.0325(7) Uani 1 1 d . . . . .
H10 H -0.1173 0.2170 -0.1992 0.039 Uiso 1 1 calc R . . . .
C13 C 0.2678(3) 0.1617(3) 0.0019(2) 0.0303(6) Uani 1 1 d . . . . .
H13 H 0.3083 0.2006 0.0720 0.036 Uiso 1 1 calc R . . . .
C20 C 0.1578(3) 0.2590(3) 0.5263(2) 0.0310(6) Uani 1 1 d . . . . .
C22 C 0.3346(4) 0.1727(3) 0.6120(2) 0.0389(8) Uani 1 1 d . . . . .
H22 H 0.3704 0.1541 0.6726 0.047 Uiso 1 1 calc R . . . .
C9 C -0.1463(3) 0.2894(3) -0.0526(2) 0.0303(6) Uani 1 1 d . . . . .
H9 H -0.2365 0.3180 -0.0660 0.036 Uiso 1 1 calc R . . . .
C21 C 0.2122(4) 0.2306(3) 0.6143(2) 0.0362(7) Uani 1 1 d . . . . .
H21 H 0.1641 0.2514 0.6765 0.043 Uiso 1 1 calc R . . . .
C25 C 0.4261(3) 0.1232(3) 0.3324(2) 0.0317(7) Uani 1 1 d . . . . .
H25 H 0.4064 0.1747 0.2849 0.038 Uiso 1 1 calc R . . . .
C4 C 0.4461(4) 0.5325(3) 0.3251(2) 0.0352(7) Uani 1 1 d . . . . .
H4A H 0.5406 0.5094 0.2955 0.042 Uiso 1 1 calc R . . . .
H4B H 0.4748 0.6018 0.3803 0.042 Uiso 1 1 calc R . . . .
C5 C 0.3536(4) 0.5662(3) 0.2436(2) 0.0373(7) Uani 1 1 d . . . . .
H5A H 0.2891 0.6227 0.2766 0.045 Uiso 1 1 calc R . . . .
H5B H 0.4233 0.6056 0.2000 0.045 Uiso 1 1 calc R . . . .
C26 C 0.3488(4) -0.0014(3) 0.2853(2) 0.0414(8) Uani 1 1 d . . . . .
H26A H 0.3682 -0.0543 0.3298 0.062 Uiso 1 1 calc GR . . . .
H26B H 0.3895 -0.0268 0.2186 0.062 Uiso 1 1 calc GR . . . .
H26C H 0.2394 -0.0025 0.2777 0.062 Uiso 1 1 calc GR . . . .
C17 C -0.2088(4) 0.4880(3) 0.1121(3) 0.0414(8) Uani 1 1 d . . . . .
H17A H -0.1172 0.5344 0.0934 0.062 Uiso 1 1 calc GR . . . .
H17B H -0.2488 0.5319 0.1730 0.062 Uiso 1 1 calc GR . . . .
H17C H -0.2851 0.4712 0.0561 0.062 Uiso 1 1 calc GR . . . .
C28 C 0.0205(4) 0.3207(3) 0.5306(2) 0.0437(8) Uani 1 1 d . . . . .
H28 H 0.0070 0.3428 0.4635 0.052 Uiso 1 1 calc R . . . .
C27 C 0.5963(4) 0.1271(3) 0.3420(3) 0.0434(8) Uani 1 1 d . . . . .
H27A H 0.6448 0.2073 0.3694 0.065 Uiso 1 1 calc GR . . . .
H27B H 0.6349 0.0998 0.2750 0.065 Uiso 1 1 calc GR . . . .
H27C H 0.6190 0.0767 0.3879 0.065 Uiso 1 1 calc GR . . . .
C15 C 0.3878(4) 0.1932(4) -0.0728(3) 0.0611(11) Uani 1 1 d . . . . .
H15A H 0.3510 0.1564 -0.1423 0.092 Uiso 1 1 calc GR . . . .
H15B H 0.4815 0.1652 -0.0576 0.092 Uiso 1 1 calc GR . . . .
H15C H 0.4078 0.2780 -0.0661 0.092 Uiso 1 1 calc GR . . . .
C18 C -0.3128(5) 0.2986(3) 0.1566(3) 0.0667(13) Uani 1 1 d . . . . .
H18A H -0.3860 0.2836 0.0990 0.100 Uiso 1 1 calc GR . . . .
H18B H -0.3567 0.3391 0.2175 0.100 Uiso 1 1 calc GR . . . .
H18C H -0.2879 0.2245 0.1684 0.100 Uiso 1 1 calc GR . . . .
C14 C 0.2406(4) 0.0311(3) -0.0030(3) 0.0510(9) Uani 1 1 d . . . . .
H14A H 0.1665 0.0128 0.0469 0.076 Uiso 1 1 calc GR . . . .
H14B H 0.3360 0.0055 0.0122 0.076 Uiso 1 1 calc GR . . . .
H14C H 0.2017 -0.0094 -0.0713 0.076 Uiso 1 1 calc GR . . . .
C30 C -0.1207(5) 0.2379(5) 0.5469(3) 0.0721(13) Uani 1 1 d . . . . .
H30A H -0.1321 0.1677 0.4930 0.108 Uiso 1 1 calc GR . . . .
H30B H -0.2099 0.2766 0.5452 0.108 Uiso 1 1 calc GR . . . .
H30C H -0.1109 0.2163 0.6131 0.108 Uiso 1 1 calc GR . . . .
C29 C 0.0403(5) 0.4321(3) 0.6128(3) 0.0550(10) Uani 1 1 d . . . . .
H29A H 0.0501 0.4123 0.6796 0.083 Uiso 1 1 calc GR . . . .
H29B H -0.0480 0.4715 0.6103 0.083 Uiso 1 1 calc GR . . . .
H29C H 0.1317 0.4840 0.6010 0.083 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ge1 N2 85.64(9) . . ?
C7 N1 Ge1 124.60(18) . . ?
C1 N1 Ge1 115.36(17) . . ?
C1 N1 C7 120.0(2) . . ?
C19 N2 Ge1 126.08(18) . . ?
C2 N2 Ge1 115.08(16) . . ?
C2 N2 C19 118.2(2) . . ?
C24 C19 N2 118.3(2) . . ?
C20 C19 N2 120.4(2) . . ?
C20 C19 C24 121.3(2) . . ?
N2 C2 C1 112.2(2) . . ?
C3 C2 N2 126.9(2) . . ?
C3 C2 C1 120.8(3) . . ?
C8 C7 N1 119.6(2) . . ?
C12 C7 N1 119.0(2) . . ?
C12 C7 C8 121.4(2) . . ?
N1 C1 C2 111.5(2) . . ?
C6 C1 N1 127.3(2) . . ?
C6 C1 C2 121.2(2) . . ?
C7 C8 C16 121.9(2) . . ?
C9 C8 C7 117.7(3) . . ?
C9 C8 C16 120.4(3) . . ?
C7 C12 C13 121.6(2) . . ?
C11 C12 C7 118.4(3) . . ?
C11 C12 C13 120.0(2) . . ?
C19 C24 C25 121.4(2) . . ?
C23 C24 C19 117.5(3) . . ?
C23 C24 C25 120.9(3) . . ?
C8 C16 C17 112.4(2) . . ?
C18 C16 C8 111.1(3) . . ?
C18 C16 C17 109.9(3) . . ?
C2 C3 C4 120.3(3) . . ?
C1 C6 C5 120.2(3) . . ?
C12 C11 C10 120.8(3) . . ?
C22 C23 C24 121.3(3) . . ?
C9 C10 C11 120.0(3) . . ?
C12 C13 C15 111.9(3) . . ?
C14 C13 C12 111.2(3) . . ?
C14 C13 C15 110.5(3) . . ?
C19 C20 C28 121.8(3) . . ?
C21 C20 C19 118.5(3) . . ?
C21 C20 C28 119.6(3) . . ?
C21 C22 C23 120.5(3) . . ?
C10 C9 C8 121.5(3) . . ?
C22 C21 C20 120.8(3) . . ?
C24 C25 C26 109.6(3) . . ?
C24 C25 C27 113.8(3) . . ?
C27 C25 C26 110.1(3) . . ?
C3 C4 C5 114.3(3) . . ?
C6 C5 C4 113.5(3) . . ?
C20 C28 C30 109.8(3) . . ?
C20 C28 C29 112.1(3) . . ?
C30 C28 C29 110.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.855(2) . ?
Ge1 N2 1.856(2) . ?
N1 C7 1.443(3) . ?
N1 C1 1.406(3) . ?
N2 C19 1.436(3) . ?
N2 C2 1.404(3) . ?
C19 C24 1.415(4) . ?
C19 C20 1.399(4) . ?
C2 C1 1.473(3) . ?
C2 C3 1.348(4) . ?
C7 C8 1.406(4) . ?
C7 C12 1.404(4) . ?
C1 C6 1.336(4) . ?
C8 C16 1.518(4) . ?
C8 C9 1.394(4) . ?
C12 C11 1.387(4) . ?
C12 C13 1.527(4) . ?
C24 C23 1.395(4) . ?
C24 C25 1.512(4) . ?
C16 C17 1.527(4) . ?
C16 C18 1.512(5) . ?
C3 C4 1.490(4) . ?
C6 C5 1.507(4) . ?
C11 C10 1.391(4) . ?
C23 C22 1.380(4) . ?
C10 C9 1.372(4) . ?
C13 C15 1.533(4) . ?
C13 C14 1.519(4) . ?
C20 C21 1.396(4) . ?
C20 C28 1.516(4) . ?
C22 C21 1.373(5) . ?
C25 C26 1.539(4) . ?
C25 C27 1.519(4) . ?
C4 C5 1.517(4) . ?
C28 C30 1.525(6) . ?
C28 C29 1.529(5) . ?
