#------------------------------------------------------------------------------
#$Date: 2022-05-03 02:15:34 +0300 (Tue, 03 May 2022) $
#$Revision: 274814 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/01/7710140.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_7710140
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 H41 Cl Ge N2'
_chemical_formula_sum            'C30 H41 Cl Ge N2'
_chemical_formula_weight         537.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-17
_audit_creation_method
;
Olex2 1.2
(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                 117.354(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.622(7)
_cell_length_b                   10.372(3)
_cell_length_c                   17.159(7)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      54.836
_cell_measurement_theta_min      4.441
_cell_volume                     2785.6(18)
_computing_cell_refinement       'C H O Ag P F'
_computing_data_reduction        'C H O Ag P F'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39101
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.066
_diffrn_reflns_theta_min         2.456
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1791 before and 0.1041 after correction.
The Ratio of minimum to maximum transmission is 0.8370.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5298
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0435
_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/[σ²(Fo²)+(0.0530P)²+3.0394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4233
_reflns_number_total             5298
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00981a5.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        2785.5(19)
_cod_database_code               7710140
_shelx_shelxl_version_number     2018/3
_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   0.850
_shelx_estimated_absorpt_t_min   0.786
_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. Rigid bond restraints
 Cl1, Ge1, N2, N1, C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Ternary CH refined with riding coordinates:
 C16(H16), C25(H25), C13(H13), C28(H28)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C6(H6), C10(H10), C23(H23), C21(H21), C22(H22)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C17(H17A,H17B,
 H17C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C18(H18A,
 H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.22926(2) 0.42312(3) 0.64656(2) 0.03075(12) Uani 1 1 d . U . . .
Cl1 Cl 0.29018(5) 0.54021(7) 0.57487(5) 0.04134(18) Uani 1 1 d . U . . .
N1 N 0.32095(14) 0.4258(2) 0.76272(14) 0.0317(4) Uani 1 1 d . U . . .
N2 N 0.19969(15) 0.5894(2) 0.69268(15) 0.0343(4) Uani 1 1 d . U . . .
C1 C 0.32952(18) 0.5353(3) 0.81204(17) 0.0315(5) Uani 1 1 d . U . . .
C7 C 0.36447(17) 0.3110(3) 0.80834(16) 0.0302(6) Uani 1 1 d . . . . .
C8 C 0.43741(17) 0.2695(3) 0.80315(17) 0.0310(6) Uani 1 1 d . . . . .
C19 C 0.12068(19) 0.6594(3) 0.64295(18) 0.0382(7) Uani 1 1 d . . . . .
C12 C 0.33189(18) 0.2429(3) 0.85712(18) 0.0336(6) Uani 1 1 d . . . . .
C9 C 0.47676(18) 0.1560(3) 0.84665(18) 0.0351(7) Uani 1 1 d . . . . .
H9 H 0.525821 0.125139 0.843049 0.042 Uiso 1 1 calc R . . . .
C2 C 0.2568(2) 0.6228(3) 0.77057(17) 0.0362(6) Uani 1 1 d . U . . .
C20 C 0.1216(2) 0.7769(3) 0.6036(2) 0.0416(7) Uani 1 1 d . . . . .
C24 C 0.0447(2) 0.5999(3) 0.63232(19) 0.0407(7) Uani 1 1 d . . . . .
C11 C 0.3744(2) 0.1311(3) 0.90061(19) 0.0396(7) Uani 1 1 d . . . . .
H11 H 0.354039 0.084140 0.934734 0.047 Uiso 1 1 calc R . . . .
C6 C 0.3937(2) 0.5626(3) 0.89350(18) 0.0397(6) Uani 1 1 d . U . . .
H6 H 0.439143 0.502459 0.920213 0.048 Uiso 1 1 calc R . . . .
C10 C 0.4456(2) 0.0880(3) 0.89469(19) 0.0387(7) Uani 1 1 d . . . . .
H10 H 0.473196 0.010938 0.923907 0.046 Uiso 1 1 calc R . . . .
C16 C 0.47309(19) 0.3427(3) 0.75129(19) 0.0368(7) Uani 1 1 d . . . . .
H16 H 0.439069 0.423780 0.729611 0.044 Uiso 1 1 calc R . . . .
C25 C 0.0445(2) 0.4765(3) 0.6796(2) 0.0432(7) Uani 1 1 d . . . . .
H25 H 0.097355 0.427401 0.690702 0.052 Uiso 1 1 calc R . . . .
C13 C 0.25116(19) 0.2847(3) 0.86181(19) 0.0381(7) Uani 1 1 d . . . . .
H13 H 0.233167 0.369514 0.830940 0.046 Uiso 1 1 calc R . . . .
C5 C 0.3959(2) 0.6819(3) 0.9425(2) 0.0491(7) Uani 1 1 d . U . . .
H5A H 0.385593 0.659003 0.992778 0.059 Uiso 1 1 calc R . . . .
H5B H 0.453616 0.720658 0.966133 0.059 Uiso 1 1 calc R . . . .
C28 C 0.2016(2) 0.8428(3) 0.6109(2) 0.0467(8) Uani 1 1 d . . . . .
H28 H 0.251844 0.787938 0.648548 0.056 Uiso 1 1 calc R . . . .
C14 C 0.2665(2) 0.3049(3) 0.9556(2) 0.0494(8) Uani 1 1 d . . . . .
H14A H 0.280739 0.222223 0.986695 0.074 Uiso 1 1 calc GR . . . .
H14B H 0.214762 0.340097 0.955261 0.074 Uiso 1 1 calc GR . . . .
H14C H 0.313935 0.365393 0.985270 0.074 Uiso 1 1 calc GR . . . .
C15 C 0.1787(2) 0.1898(3) 0.8137(2) 0.0517(9) Uani 1 1 d . . . . .
H15A H 0.166493 0.184769 0.751966 0.078 Uiso 1 1 calc GR . . . .
H15B H 0.127479 0.218931 0.817255 0.078 Uiso 1 1 calc GR . . . .
H15C H 0.195353 0.104407 0.840721 0.078 Uiso 1 1 calc GR . . . .
C23 C -0.0320(2) 0.6623(4) 0.5791(2) 0.0503(9) Uani 1 1 d . . . . .
H23 H -0.084543 0.623925 0.569636 0.060 Uiso 1 1 calc R . . . .
C30 C 0.1985(2) 0.8551(3) 0.5205(2) 0.0502(8) Uani 1 1 d . . . . .
H30A H 0.193800 0.769095 0.494994 0.075 Uiso 1 1 calc GR . . . .
H30B H 0.250758 0.896990 0.526637 0.075 Uiso 1 1 calc GR . . . .
H30C H 0.148793 0.906963 0.482010 0.075 Uiso 1 1 calc GR . . . .
C21 C 0.0426(2) 0.8351(4) 0.5524(2) 0.0534(9) Uani 1 1 d . . . . .
H21 H 0.040790 0.915740 0.525327 0.064 Uiso 1 1 calc R . . . .
C22 C -0.0328(2) 0.7785(4) 0.5403(2) 0.0572(10) Uani 1 1 d . . . . .
H22 H -0.085614 0.820072 0.504768 0.069 Uiso 1 1 calc R . . . .
C17 C 0.5662(2) 0.3813(4) 0.8078(2) 0.0598(10) Uani 1 1 d . . . . .
H17A H 0.570874 0.433532 0.857398 0.090 Uiso 1 1 calc GR . . . .
H17B H 0.586180 0.431571 0.772416 0.090 Uiso 1 1 calc GR . . . .
H17C H 0.601331 0.303619 0.829818 0.090 Uiso 1 1 calc GR . . . .
C3 C 0.2498(2) 0.7319(3) 0.8236(2) 0.0477(5) Uani 1 1 d . U . . .
H3A H 0.217895 0.803385 0.783666 0.057 Uiso 1 1 calc R . . . .
H3B H 0.216779 0.703198 0.854027 0.057 Uiso 1 1 calc R . . . .
C27 C -0.0314(2) 0.3902(4) 0.6262(3) 0.0610(10) Uani 1 1 d . . . . .
H27A H -0.083728 0.430587 0.621162 0.092 Uiso 1 1 calc GR . . . .
H27B H -0.023336 0.306450 0.655447 0.092 Uiso 1 1 calc GR . . . .
H27C H -0.036137 0.377707 0.567513 0.092 Uiso 1 1 calc GR . . . .
C29 C 0.2149(3) 0.9764(4) 0.6535(3) 0.0657(11) Uani 1 1 d . . . . .
H29A H 0.166000 1.031666 0.617971 0.099 Uiso 1 1 calc GR . . . .
H29B H 0.267211 1.015049 0.657065 0.099 Uiso 1 1 calc GR . . . .
H29C H 0.220169 0.967987 0.712635 0.099 Uiso 1 1 calc GR . . . .
C26 C 0.0489(3) 0.5072(4) 0.7685(2) 0.0643(11) Uani 1 1 d . . . . .
H26A H 0.100009 0.558874 0.803224 0.096 Uiso 1 1 calc GR . . . .
H26B H 0.051609 0.426708 0.799542 0.096 Uiso 1 1 calc GR . . . .
H26C H -0.002090 0.555820 0.759765 0.096 Uiso 1 1 calc GR . . . .
C4 C 0.3318(2) 0.7789(3) 0.8876(2) 0.0553(6) Uani 1 1 d . U . . .
H4A H 0.322253 0.838591 0.927237 0.066 Uiso 1 1 calc R . . . .
H4B H 0.356788 0.829995 0.856303 0.066 Uiso 1 1 calc R . . . .
C18 C 0.4630(3) 0.2664(4) 0.6716(2) 0.0689(11) Uani 1 1 d . . . . .
H18A H 0.498582 0.188697 0.690829 0.103 Uiso 1 1 calc GR . . . .
H18B H 0.480971 0.319552 0.635787 0.103 Uiso 1 1 calc GR . . . .
H18C H 0.403034 0.241579 0.636739 0.103 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 0.0148 0.0070 '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'
Cl Cl 0.3294 0.5404 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.5487 0.7176 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 '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 Cl1 99.84(8) . . ?
N1 Ge1 N2 80.12(9) . . ?
N2 Ge1 Cl1 91.48(8) . . ?
C1 N1 Ge1 117.02(17) . . ?
C1 N1 C7 117.8(2) . . ?
C7 N1 Ge1 122.77(17) . . ?
C19 N2 Ge1 122.44(18) . . ?
C2 N2 Ge1 113.91(19) . . ?
C2 N2 C19 123.6(2) . . ?
N1 C1 C2 112.8(2) . . ?
C6 C1 N1 127.1(3) . . ?
C6 C1 C2 120.0(3) . . ?
C8 C7 N1 119.8(2) . . ?
C8 C7 C12 121.6(2) . . ?
C12 C7 N1 118.6(3) . . ?
C7 C8 C16 121.8(2) . . ?
C9 C8 C7 118.1(3) . . ?
C9 C8 C16 120.0(3) . . ?
C20 C19 N2 120.0(3) . . ?
C20 C19 C24 122.8(3) . . ?
C24 C19 N2 117.1(3) . . ?
C7 C12 C13 122.4(2) . . ?
C11 C12 C7 118.0(3) . . ?
C11 C12 C13 119.5(3) . . ?
C10 C9 C8 121.0(3) . . ?
N2 C2 C1 115.3(2) . . ?
N2 C2 C3 126.0(3) . . ?
C1 C2 C3 118.3(3) . . ?
C19 C20 C28 124.7(3) . . ?
C21 C20 C19 116.8(3) . . ?
C21 C20 C28 118.5(3) . . ?
C19 C24 C25 122.5(3) . . ?
C23 C24 C19 117.4(3) . . ?
C23 C24 C25 120.1(3) . . ?
C10 C11 C12 120.9(3) . . ?
C1 C6 C5 123.1(3) . . ?
C9 C10 C11 120.3(3) . . ?
C8 C16 C17 112.0(2) . . ?
C8 C16 C18 111.1(3) . . ?
C18 C16 C17 110.8(3) . . ?
C24 C25 C27 113.2(3) . . ?
C24 C25 C26 110.3(3) . . ?
C27 C25 C26 110.7(3) . . ?
C14 C13 C12 112.3(3) . . ?
C14 C13 C15 111.2(3) . . ?
C15 C13 C12 111.0(3) . . ?
C4 C5 C6 113.1(3) . . ?
C20 C28 C30 110.7(3) . . ?
C20 C28 C29 112.3(3) . . ?
C30 C28 C29 109.5(3) . . ?
C22 C23 C24 120.9(3) . . ?
C22 C21 C20 121.6(3) . . ?
C23 C22 C21 120.4(3) . . ?
C4 C3 C2 112.7(3) . . ?
C3 C4 C5 117.4(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 Cl1 2.3140(10) . ?
Ge1 N1 1.904(2) . ?
Ge1 N2 2.062(2) . ?
N1 C1 1.383(4) . ?
N1 C7 1.438(3) . ?
N2 C19 1.450(4) . ?
N2 C2 1.297(4) . ?
C1 C2 1.461(4) . ?
C1 C6 1.364(4) . ?
C7 C8 1.396(4) . ?
C7 C12 1.404(4) . ?
C8 C9 1.396(4) . ?
C8 C16 1.509(4) . ?
C19 C20 1.398(4) . ?
C19 C24 1.407(5) . ?
C12 C11 1.396(4) . ?
C12 C13 1.524(4) . ?
C9 C10 1.377(4) . ?
C2 C3 1.492(4) . ?
C20 C28 1.518(5) . ?
C20 C21 1.396(4) . ?
C24 C25 1.517(4) . ?
C24 C23 1.395(4) . ?
C11 C10 1.378(4) . ?
C6 C5 1.487(4) . ?
C16 C17 1.527(5) . ?
C16 C18 1.518(4) . ?
C25 C27 1.517(5) . ?
C25 C26 1.525(4) . ?
C13 C14 1.518(4) . ?
C13 C15 1.522(5) . ?
C5 C4 1.482(5) . ?
C28 C30 1.532(5) . ?
C28 C29 1.534(5) . ?
C23 C22 1.375(5) . ?
C21 C22 1.378(5) . ?
C3 C4 1.440(5) . ?
