#------------------------------------------------------------------------------
#$Date: 2022-05-03 02:15:34 +0300 (Tue, 03 May 2022) $
#$Revision: 274814 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/01/7710141.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_7710141
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         'C60 H82 Ge2 N4'
_chemical_formula_sum            'C60 H82 Ge2 N4'
_chemical_formula_weight         1004.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-05-17
_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                90
_cell_angle_beta                 104.017(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8471(7)
_cell_length_b                   12.1217(7)
_cell_length_c                   18.1718(9)
_cell_measurement_reflns_used    6490
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      54.69
_cell_measurement_theta_min      3.32
_cell_volume                     2745.6(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)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.1508
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35478
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.766
_diffrn_reflns_theta_min         1.758
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5352
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1625 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.7128.
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    1.215
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0549
_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/[σ²(Fo²)+(0.0663P)²+1.9602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3341
_reflns_number_total             5223
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00981a5.cif
_cod_data_source_block           compound6
_cod_database_code               7710141
_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   0.805
_shelx_estimated_absorpt_t_min   0.727
_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:
 C13(H13), C28(H28), C16(H16), C6(H6), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C22(H22), C23(H23), C21(H21), C9(H9)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C18(H18A,H18B,
 H18C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.86133(4) 0.70724(4) 0.11233(3) 0.03928(17) Uani 1 1 d . . . . .
N1 N 0.9566(2) 0.7777(3) 0.06383(16) 0.0240(7) Uani 1 1 d . . . . .
N2 N 0.7778(2) 0.8329(3) 0.08385(16) 0.0260(7) Uani 1 1 d . . . . .
C12 C 1.0791(3) 0.6912(3) -0.0050(2) 0.0269(8) Uani 1 1 d . . . . .
C1 C 0.9188(3) 0.8788(3) 0.03007(18) 0.0217(8) Uani 1 1 d . . . . .
C5 C 0.8818(3) 0.9793(3) -0.09006(19) 0.0280(9) Uani 1 1 d . . . . .
H5A H 0.8605 0.9122 -0.1211 0.034 Uiso 1 1 calc R . . . .
H5B H 0.9113 1.0324 -0.1211 0.034 Uiso 1 1 calc R . . . .
C2 C 0.8215(3) 0.9073(3) 0.04138(19) 0.0247(8) Uani 1 1 d . . . . .
C20 C 0.5839(3) 0.8222(3) 0.0715(2) 0.0295(9) Uani 1 1 d . . . . .
C13 C 0.9938(3) 0.6899(3) -0.0795(2) 0.0315(9) Uani 1 1 d . . . . .
H13 H 0.9316 0.7349 -0.0726 0.038 Uiso 1 1 calc R . . . .
C7 C 1.0603(3) 0.7309(3) 0.0632(2) 0.0252(8) Uani 1 1 d . . . . .
C8 C 1.1377(3) 0.7194(3) 0.1325(2) 0.0302(9) Uani 1 1 d . . . . .
C28 C 0.5676(3) 0.7614(4) -0.0038(2) 0.0367(10) Uani 1 1 d . . . . .
H28 H 0.6322 0.7759 -0.0239 0.044 Uiso 1 1 calc R . . . .
C16 C 1.1212(3) 0.7567(4) 0.2095(2) 0.0358(10) Uani 1 1 d . . . . .
H16 H 1.0539 0.8015 0.2000 0.043 Uiso 1 1 calc R . . . .
C19 C 0.6845(3) 0.8610(3) 0.11067(19) 0.0265(9) Uani 1 1 d . . . . .
C10 C 1.2558(3) 0.6334(4) 0.0641(3) 0.0422(11) Uani 1 1 d . . . . .
H10 H 1.3232 0.6012 0.0641 0.051 Uiso 1 1 calc R . . . .
C4 C 0.7806(3) 1.0302(4) -0.0723(2) 0.0394(11) Uani 1 1 d . . . . .
H4A H 0.7843 1.1113 -0.0781 0.047 Uiso 1 1 calc R . . . .
H4B H 0.7173 1.0038 -0.1110 0.047 Uiso 1 1 calc R . . . .
C11 C 1.1798(3) 0.6440(4) -0.0024(2) 0.0375(10) Uani 1 1 d . . . . .
H11 H 1.1954 0.6189 -0.0480 0.045 Uiso 1 1 calc R . . . .
C22 C 0.5088(3) 0.9008(4) 0.1697(2) 0.0367(10) Uani 1 1 d . . . . .
H22 H 0.4491 0.9129 0.1909 0.044 Uiso 1 1 calc R . . . .
C6 C 0.9707(3) 0.9485(3) -0.02015(18) 0.0234(8) Uani 1 1 d . . . . .
H6 H 1.0244 0.9018 -0.0374 0.028 Uiso 1 1 calc R . . . .
C3 C 0.7620(3) 1.0064(4) 0.0048(2) 0.0389(11) Uani 1 1 d . . . . .
H3A H 0.7846 1.0713 0.0380 0.047 Uiso 1 1 calc R . . . .
H3B H 0.6843 0.9951 -0.0002 0.047 Uiso 1 1 calc R . . . .
C23 C 0.6077(3) 0.9420(4) 0.2054(2) 0.0331(10) Uani 1 1 d . . . . .
H23 H 0.6147 0.9835 0.2507 0.040 Uiso 1 1 calc R . . . .
C24 C 0.6981(3) 0.9250(3) 0.1773(2) 0.0303(9) Uani 1 1 d . . . . .
C21 C 0.4959(3) 0.8422(4) 0.1033(2) 0.0352(10) Uani 1 1 d . . . . .
H21 H 0.4269 0.8149 0.0787 0.042 Uiso 1 1 calc R . . . .
C9 C 1.2358(3) 0.6687(4) 0.1312(2) 0.0375(10) Uani 1 1 d . . . . .
H9 H 1.2889 0.6589 0.1772 0.045 Uiso 1 1 calc R . . . .
C26 C 0.8066(3) 0.9707(4) 0.2183(2) 0.0384(10) Uani 1 1 d . . . . .
H26 H 0.8555 0.9632 0.1834 0.046 Uiso 1 1 calc R . . . .
C15 C 1.0329(4) 0.7394(4) -0.1453(2) 0.0444(11) Uani 1 1 d . . . . .
H15A H 1.0601 0.8141 -0.1320 0.067 Uiso 1 1 calc GR . . . .
H15B H 0.9732 0.7424 -0.1906 0.067 Uiso 1 1 calc GR . . . .
H15C H 1.0904 0.6933 -0.1557 0.067 Uiso 1 1 calc GR . . . .
C30 C 0.4700(4) 0.8067(4) -0.0619(2) 0.0530(13) Uani 1 1 d . . . . .
H30A H 0.4044 0.7878 -0.0462 0.080 Uiso 1 1 calc GR . . . .
H30B H 0.4672 0.7742 -0.1117 0.080 Uiso 1 1 calc GR . . . .
H30C H 0.4759 0.8871 -0.0650 0.080 Uiso 1 1 calc GR . . . .
C29 C 0.5604(4) 0.6387(4) 0.0061(3) 0.0556(13) Uani 1 1 d . . . . .
H29A H 0.6222 0.6135 0.0454 0.083 Uiso 1 1 calc GR . . . .
H29B H 0.5601 0.6017 -0.0419 0.083 Uiso 1 1 calc GR . . . .
H29C H 0.4941 0.6210 0.0212 0.083 Uiso 1 1 calc GR . . . .
C18 C 1.1062(4) 0.6564(4) 0.2569(2) 0.0485(12) Uani 1 1 d . . . . .
H18A H 1.0454 0.6124 0.2289 0.073 Uiso 1 1 calc GR . . . .
H18B H 1.0922 0.6811 0.3049 0.073 Uiso 1 1 calc GR . . . .
H18C H 1.1714 0.6112 0.2672 0.073 Uiso 1 1 calc GR . . . .
C14 C 0.9544(4) 0.5719(4) -0.0985(3) 0.0485(12) Uani 1 1 d . . . . .
H14A H 1.0149 0.5252 -0.1029 0.073 Uiso 1 1 calc GR . . . .
H14B H 0.8999 0.5714 -0.1467 0.073 Uiso 1 1 calc GR . . . .
H14C H 0.9232 0.5434 -0.0581 0.073 Uiso 1 1 calc GR . . . .
C17 C 1.2131(4) 0.8285(4) 0.2545(2) 0.0488(12) Uani 1 1 d . . . . .
H17A H 1.2799 0.7860 0.2654 0.073 Uiso 1 1 calc GR . . . .
H17B H 1.1969 0.8516 0.3022 0.073 Uiso 1 1 calc GR . . . .
H17C H 1.2210 0.8938 0.2246 0.073 Uiso 1 1 calc GR . . . .
C25 C 0.7999(4) 1.0930(4) 0.2360(3) 0.0543(13) Uani 1 1 d . . . . .
H25A H 0.7668 1.1330 0.1893 0.081 Uiso 1 1 calc GR . . . .
H25B H 0.8723 1.1218 0.2570 0.081 Uiso 1 1 calc GR . . . .
H25C H 0.7565 1.1028 0.2730 0.081 Uiso 1 1 calc GR . . . .
C27 C 0.8548(4) 0.9054(5) 0.2887(3) 0.0694(17) Uani 1 1 d . . . . .
H27A H 0.8114 0.9154 0.3257 0.104 Uiso 1 1 calc GR . . . .
H27B H 0.9281 0.9313 0.3105 0.104 Uiso 1 1 calc GR . . . .
H27C H 0.8564 0.8271 0.2757 0.104 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
N2 Ge1 N1 83.97(13) . . ?
C1 N1 Ge1 114.0(2) . . ?
C1 N1 C7 124.0(3) . . ?
C7 N1 Ge1 122.0(2) . . ?
C2 N2 Ge1 113.7(2) . . ?
C2 N2 C19 121.0(3) . . ?
C19 N2 Ge1 124.8(2) . . ?
C7 C12 C13 123.3(3) . . ?
C7 C12 C11 117.6(3) . . ?
C11 C12 C13 119.0(3) . . ?
N1 C1 C6 126.5(3) . . ?
C2 C1 N1 112.9(3) . . ?
C2 C1 C6 120.4(3) . . ?
C6 C5 C4 114.9(3) . . ?
N2 C2 C3 122.5(3) . . ?
C1 C2 N2 115.4(3) . . ?
C1 C2 C3 121.9(3) . . ?
C19 C20 C28 122.0(3) . . ?
C19 C20 C21 117.9(3) . . ?
C21 C20 C28 120.1(4) . . ?
C12 C13 C15 112.9(3) . . ?
C12 C13 C14 109.8(3) . . ?
C14 C13 C15 110.1(3) . . ?
C12 C7 N1 119.7(3) . . ?
C12 C7 C8 121.3(3) . . ?
C8 C7 N1 118.8(3) . . ?
C7 C8 C16 124.2(3) . . ?
C9 C8 C7 117.9(4) . . ?
C9 C8 C16 117.8(3) . . ?
C20 C28 C30 111.0(3) . . ?
C29 C28 C20 111.7(4) . . ?
C29 C28 C30 111.9(4) . . ?
C18 C16 C8 110.0(4) . . ?
C18 C16 C17 109.7(3) . . ?
C17 C16 C8 113.3(3) . . ?
C20 C19 N2 119.4(3) . . ?
C20 C19 C24 121.9(3) . . ?
C24 C19 N2 118.6(3) . . ?
C11 C10 C9 120.6(4) . . ?
C3 C4 C5 116.7(3) . . ?
C10 C11 C12 121.6(4) . . ?
C23 C22 C21 120.3(3) . . ?
C1 C6 C5 106.7(3) . . ?
C1 C6 C6 113.6(3) . 3_775 ?
C5 C6 C6 112.0(4) . 3_775 ?
C2 C3 C4 112.9(3) . . ?
C22 C23 C24 122.1(4) . . ?
C19 C24 C26 122.0(3) . . ?
C23 C24 C19 117.0(4) . . ?
C23 C24 C26 120.9(3) . . ?
C22 C21 C20 120.7(4) . . ?
C10 C9 C8 120.8(4) . . ?
C24 C26 C25 111.6(4) . . ?
C27 C26 C24 111.5(4) . . ?
C27 C26 C25 111.4(4) . . ?
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 1.878(3) . ?
Ge1 N2 1.863(3) . ?
N1 C1 1.404(5) . ?
N1 C7 1.451(4) . ?
N2 C2 1.391(4) . ?
N2 C19 1.440(4) . ?
C12 C13 1.521(5) . ?
C12 C7 1.403(5) . ?
C12 C11 1.406(5) . ?
C1 C2 1.359(5) . ?
C1 C6 1.512(5) . ?
C5 C4 1.542(5) . ?
C5 C6 1.535(5) . ?
C2 C3 1.492(5) . ?
C20 C28 1.522(5) . ?
C20 C19 1.397(5) . ?
C20 C21 1.411(5) . ?
C13 C15 1.529(5) . ?
C13 C14 1.529(6) . ?
C7 C8 1.410(5) . ?
C8 C16 1.534(5) . ?
C8 C9 1.407(5) . ?
C28 C30 1.533(6) . ?
C28 C29 1.503(7) . ?
C16 C18 1.530(6) . ?
C16 C17 1.533(6) . ?
C19 C24 1.412(5) . ?
C10 C11 1.363(6) . ?
C10 C9 1.373(6) . ?
C4 C3 1.505(5) . ?
C22 C23 1.373(6) . ?
C22 C21 1.374(6) . ?
C6 C6 1.547(7) 3_775 ?
C23 C24 1.393(5) . ?
C24 C26 1.517(6) . ?
C26 C25 1.523(7) . ?
C26 C27 1.504(6) . ?
