#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:53:30 +0300 (Sat, 05 Jun 2021) $
#$Revision: 266085 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/70/7707036.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_7707036
loop_
_publ_author_name
'Zechovský, Jan'
'Mrózek, Ondřej'
'Samsonov, Maksim'
'Jambor, Roman'
'R°uŽička, Aleš'
'Dostál, Libor'
_publ_section_title
;
 Coordination capabilities of bis-(2-pyridyl)amides in the field of
 divalent germanium, tin and lead compounds.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6321
_journal_page_last               6332
_journal_paper_doi               10.1039/d1dt00717c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C24 H24 Ge N6'
_chemical_formula_weight         469.08
_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_method           SHELXL-2014/7
_audit_update_record
;
2020-09-21 deposited with the CCDC.	2021-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                111.554(2)
_cell_angle_beta                 96.379(2)
_cell_angle_gamma                110.358(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8339(5)
_cell_length_b                   12.1659(6)
_cell_length_c                   12.3964(6)
_cell_measurement_reflns_used    36087
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1117.25(10)
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36087
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         2.492
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.591
_exptl_crystal_size_mid          0.575
_exptl_crystal_size_min          0.228
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5147
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0258
_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)+(0.0298P)²+0.6353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4703
_reflns_number_total             5147
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00717c4.cif
_cod_data_source_block           ld190507Ge1
_cod_depositor_comments
'Adding full bibliography for 7707027--7707037.cif.'
_cod_database_code               7707036
_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.
;
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.588
;
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 0.24340(2) 0.12874(2) 0.44229(2) 0.02156(6) Uani 1 1 d . U . . .
N1 N 0.40872(16) 0.15847(13) 0.58784(12) 0.0214(3) Uani 1 1 d . U . . .
C1 C 0.53978(18) 0.17003(14) 0.53784(14) 0.0198(3) Uani 1 1 d . U . . .
N2 N 0.48881(16) 0.17404(12) 0.43222(12) 0.0207(3) Uani 1 1 d . U . . .
C2 C 0.5872(2) 0.18437(16) 0.35810(14) 0.0244(3) Uani 1 1 d . U . . .
C3 C 0.7464(2) 0.19106(16) 0.38936(16) 0.0277(3) Uani 1 1 d . U . . .
H3 H 0.8186 0.2002 0.3388 0.033 Uiso 1 1 calc R U . . .
N3 N 0.53567(17) 0.16254(14) 0.76648(12) 0.0254(3) Uani 1 1 d . U . . .
C4 C 0.7996(2) 0.18426(16) 0.49563(16) 0.0277(3) Uani 1 1 d . U . . .
H4 H 0.9079 0.1866 0.5160 0.033 Uiso 1 1 calc R U . . .
N4 N 0.26806(17) 0.30709(13) 0.51507(12) 0.0224(3) Uani 1 1 d . U . . .
C5 C 0.69895(19) 0.17417(15) 0.57220(15) 0.0242(3) Uani 1 1 d . U . . .
H5 H 0.7360 0.1702 0.6451 0.029 Uiso 1 1 calc R U . . .
N5 N 0.18786(17) 0.36242(14) 0.69434(12) 0.0268(3) Uani 1 1 d . U . . .
C6 C 0.5179(3) 0.1905(2) 0.24594(17) 0.0370(4) Uani 1 1 d . U . . .
H6A H 0.6057 0.2086 0.2049 0.055 Uiso 1 1 calc R U . . .
H6B H 0.4791 0.2601 0.2670 0.055 Uiso 1 1 calc R U . . .
H6C H 0.4235 0.1070 0.1924 0.055 Uiso 1 1 calc R U . . .
N6 N 0.17125(16) 0.25485(12) 0.31841(11) 0.0203(3) Uani 1 1 d . U . . .
C7 C 0.39799(19) 0.14579(14) 0.69271(14) 0.0213(3) Uani 1 1 d . U . . .
C8 C 0.5206(2) 0.14875(18) 0.86829(16) 0.0310(4) Uani 1 1 d . U . . .
C9 C 0.3715(2) 0.1179(2) 0.89878(16) 0.0356(4) Uani 1 1 d . U . . .
H9 H 0.3654 0.1081 0.9710 0.043 Uiso 1 1 calc R U . . .
C10 C 0.2293(2) 0.10127(19) 0.82189(17) 0.0328(4) Uani 1 1 d . U . . .
H10 H 0.1248 0.0802 0.8411 0.039 Uiso 1 1 calc R U . . .
C11 C 0.2420(2) 0.11566(16) 0.71837(15) 0.0259(3) Uani 1 1 d . U . . .
H11 H 0.1470 0.1054 0.6649 0.031 Uiso 1 1 calc R U . . .
C12 C 0.6807(3) 0.1717(2) 0.94760(19) 0.0463(5) Uani 1 1 d . U . . .
H12A H 0.7420 0.1309 0.8976 0.069 Uiso 1 1 calc R U . . .
H12B H 0.6542 0.1336 1.0041 0.069 Uiso 1 1 calc R U . . .
H12C H 0.7501 0.2656 0.9928 0.069 Uiso 1 1 calc R U . . .
C13 C 0.31051(19) 0.38427(15) 0.64113(14) 0.0209(3) Uani 1 1 d . U . . .
C14 C 0.2257(2) 0.42872(18) 0.81468(16) 0.0305(4) Uani 1 1 d . U . . .
C15 C 0.3859(3) 0.51920(18) 0.88379(16) 0.0351(4) Uani 1 1 d . U . . .
H15 H 0.4089 0.5659 0.9686 0.042 Uiso 1 1 calc R U . . .
C16 C 0.5121(3) 0.5406(2) 0.82754(18) 0.0432(5) Uani 1 1 d . U . . .
H16 H 0.6237 0.6017 0.8734 0.052 Uiso 1 1 calc R U . . .
C17 C 0.4750(2) 0.47217(19) 0.70352(17) 0.0348(4) Uani 1 1 d . U . . .
H17 H 0.5598 0.4852 0.6627 0.042 Uiso 1 1 calc R U . . .
C18 C 0.0834(3) 0.3954(3) 0.8701(2) 0.0552(6) Uani 1 1 d . U . . .
H18A H -0.0105 0.4054 0.8311 0.083 Uiso 1 1 calc R U . . .
H18B H 0.1211 0.4540 0.9565 0.083 Uiso 1 1 calc R U . . .
H18C H 0.0469 0.3051 0.8589 0.083 Uiso 1 1 calc R U . . .
C19 C 0.20413(18) 0.34136(15) 0.43371(13) 0.0193(3) Uani 1 1 d . U . . .
C20 C 0.10107(19) 0.27340(15) 0.22887(14) 0.0221(3) Uani 1 1 d . U . . .
C21 C 0.0653(2) 0.38052(16) 0.25026(15) 0.0266(3) Uani 1 1 d . U . . .
H21 H 0.0154 0.3916 0.1853 0.032 Uiso 1 1 calc R U . . .
C22 C 0.1039(2) 0.47144(16) 0.36892(16) 0.0268(3) Uani 1 1 d . U . . .
H22 H 0.0824 0.5465 0.3855 0.032 Uiso 1 1 calc R U . . .
C23 C 0.1729(2) 0.45317(15) 0.46220(14) 0.0236(3) Uani 1 1 d . U . . .
H23 H 0.1989 0.5142 0.5436 0.028 Uiso 1 1 calc R U . . .
C24 C 0.0634(2) 0.17066(18) 0.10331(15) 0.0315(4) Uani 1 1 d . U . . .
H24A H 0.0566 0.2074 0.0456 0.047 Uiso 1 1 calc R U . . .
H24B H -0.0440 0.0971 0.0844 0.047 Uiso 1 1 calc R U . . .
H24C H 0.1529 0.1405 0.0982 0.047 Uiso 1 1 calc R U . . .
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
N4 Ge1 N1 92.15(5) . . ?
N4 Ge1 N2 96.00(5) . . ?
N1 Ge1 N2 64.20(5) . . ?
C1 N1 C7 127.79(13) . . ?
C1 N1 Ge1 95.50(9) . . ?
C7 N1 Ge1 135.46(10) . . ?
N2 C1 N1 106.16(13) . . ?
N2 C1 C5 120.31(14) . . ?
N1 C1 C5 133.50(15) . . ?
C2 N2 C1 122.46(13) . . ?
C2 N2 Ge1 143.32(11) . . ?
C1 N2 Ge1 93.25(9) . . ?
N2 C2 C3 119.24(15) . . ?
N2 C2 C6 117.32(15) . . ?
C3 C2 C6 123.43(15) . . ?
C2 C3 C4 119.20(15) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C7 N3 C8 117.80(14) . . ?
C5 C4 C3 121.65(15) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C19 N4 C13 121.78(13) . . ?
C19 N4 Ge1 112.56(10) . . ?
C13 N4 Ge1 124.12(10) . . ?
C4 C5 C1 117.11(15) . . ?
C4 C5 H5 121.4 . . ?
C1 C5 H5 121.4 . . ?
C13 N5 C14 118.35(15) . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C20 N6 C19 119.09(13) . . ?
N3 C7 N1 119.32(14) . . ?
N3 C7 C11 122.49(14) . . ?
N1 C7 C11 118.20(14) . . ?
N3 C8 C9 122.98(16) . . ?
N3 C8 C12 114.77(16) . . ?
C9 C8 C12 122.24(17) . . ?
C8 C9 C10 118.83(16) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C11 C10 C9 119.15(16) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C7 118.75(15) . . ?
C10 C11 H11 120.6 . . ?
C7 C11 H11 120.6 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 C17 123.23(15) . . ?
N5 C13 N4 116.78(14) . . ?
C17 C13 N4 119.91(15) . . ?
N5 C14 C15 122.28(16) . . ?
N5 C14 C18 115.83(17) . . ?
C15 C14 C18 121.87(18) . . ?
C16 C15 C14 118.79(17) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C15 C16 C17 119.50(17) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.3 . . ?
C13 C17 C16 117.85(17) . . ?
C13 C17 H17 121.1 . . ?
C16 C17 H17 121.1 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N6 C19 N4 112.65(13) . . ?
N6 C19 C23 121.79(14) . . ?
N4 C19 C23 125.56(14) . . ?
N6 C20 C21 122.23(14) . . ?
N6 C20 C24 115.89(14) . . ?
C21 C20 C24 121.88(15) . . ?
C20 C21 C22 118.53(15) . . ?
C20 C21 H21 120.7 . . ?
C22 C21 H21 120.7 . . ?
C23 C22 C21 120.23(15) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C19 118.08(15) . . ?
C22 C23 H23 121.0 . . ?
C19 C23 H23 121.0 . . ?
C20 C24 H24A 109.5 . . ?
C20 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C20 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
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 N4 1.9387(13) . ?
Ge1 N1 2.0215(13) . ?
Ge1 N2 2.0733(13) . ?
N1 C1 1.3619(19) . ?
N1 C7 1.374(2) . ?
C1 N2 1.360(2) . ?
C1 C5 1.401(2) . ?
N2 C2 1.342(2) . ?
C2 C3 1.383(2) . ?
C2 C6 1.494(2) . ?
C3 C4 1.390(3) . ?
C3 H3 0.9500 . ?
N3 C7 1.342(2) . ?
N3 C8 1.348(2) . ?
C4 C5 1.380(2) . ?
C4 H4 0.9500 . ?
N4 C19 1.3624(19) . ?
N4 C13 1.418(2) . ?
C5 H5 0.9500 . ?
N5 C13 1.329(2) . ?
N5 C14 1.344(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N6 C20 1.340(2) . ?
N6 C19 1.3508(19) . ?
C7 C11 1.402(2) . ?
C8 C9 1.375(3) . ?
C8 C12 1.503(3) . ?
C9 C10 1.394(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.369(2) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C17 1.384(2) . ?
C14 C15 1.380(3) . ?
C14 C18 1.503(3) . ?
C15 C16 1.379(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C23 1.407(2) . ?
C20 C21 1.386(2) . ?
C20 C24 1.504(2) . ?
C21 C22 1.391(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.373(2) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
