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#$Date: 2021-06-05 21:53:30 +0300 (Sat, 05 Jun 2021) $
#$Revision: 266085 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/70/7707028.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_7707028
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            'C12 H12 Cl Ge N3'
_chemical_formula_weight         306.29
_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
_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                90
_cell_angle_beta                 95.358(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9626(5)
_cell_length_b                   9.3447(5)
_cell_length_c                   17.4878(10)
_cell_measurement_reflns_used    33637
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1295.55(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0643
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33637
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         2.474
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.551
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3951
_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    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.592
_exptl_crystal_size_mid          0.392
_exptl_crystal_size_min          0.382
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2972
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0301
_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)+(0.0136P)²+1.4804P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2561
_reflns_number_total             2972
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00717c4.cif
_cod_data_source_block           ld190513Ge1
_cod_depositor_comments
'Adding full bibliography for 7707027--7707037.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7707028
_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 0.530
;
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 0.82089(3) 0.63505(3) 0.50200(2) 0.02309(8) Uani 1 1 d . U . . .
Cl1 Cl 0.91415(7) 0.79695(7) 0.41797(4) 0.03085(14) Uani 1 1 d . U . . .
N1 N 0.6368(2) 0.76927(19) 0.53517(10) 0.0197(4) Uani 1 1 d . U . . .
C1 C 0.5153(3) 0.7122(2) 0.48440(12) 0.0183(4) Uani 1 1 d . U . . .
N2 N 0.5963(2) 0.61217(19) 0.44393(11) 0.0214(4) Uani 1 1 d . U . . .
C2 C 0.6062(3) 0.8716(2) 0.58573(12) 0.0213(4) Uani 1 1 d . U . . .
C3 C 0.4433(3) 0.9229(2) 0.58584(13) 0.0238(5) Uani 1 1 d . U . . .
H3 H 0.4179 0.9962 0.6207 0.029 Uiso 1 1 calc R U . . .
N3 N 0.3671(2) 0.5435(2) 0.35836(11) 0.0275(4) Uani 1 1 d . U . . .
C4 C 0.3170(3) 0.8661(2) 0.53441(13) 0.0240(5) Uani 1 1 d . U . . .
H4 H 0.2053 0.9016 0.5347 0.029 Uiso 1 1 calc R U . . .
C5 C 0.3487(3) 0.7593(2) 0.48278(13) 0.0211(4) Uani 1 1 d . U . . .
H5 H 0.2617 0.7203 0.4481 0.025 Uiso 1 1 calc R U . . .
C7 C 0.5309(3) 0.5313(2) 0.38222(12) 0.0206(4) Uani 1 1 d . U . . .
C6 C 0.7526(3) 0.9245(3) 0.63747(14) 0.0305(5) Uani 1 1 d . U . . .
H6A H 0.8361 0.9674 0.6066 0.046 Uiso 1 1 calc R U . . .
H6B H 0.8040 0.8444 0.6673 0.046 Uiso 1 1 calc R U . . .
H6C H 0.7138 0.9966 0.6725 0.046 Uiso 1 1 calc R U . . .
C8 C 0.3048(3) 0.4626(3) 0.29827(14) 0.0317(5) Uani 1 1 d . U . . .
C9 C 0.4022(3) 0.3674(3) 0.26176(13) 0.0325(5) Uani 1 1 d . U . . .
H9 H 0.3541 0.3110 0.2201 0.039 Uiso 1 1 calc R U . . .
C10 C 0.5717(4) 0.3555(3) 0.28695(14) 0.0336(6) Uani 1 1 d . U . . .
H10 H 0.6413 0.2902 0.2628 0.040 Uiso 1 1 calc R U . . .
C11 C 0.6389(3) 0.4388(3) 0.34736(14) 0.0269(5) Uani 1 1 d . U . . .
H11 H 0.7554 0.4335 0.3648 0.032 Uiso 1 1 calc R U . . .
C12 C 0.1204(4) 0.4841(4) 0.27447(19) 0.0579(9) Uani 1 1 d . U . . .
H12A H 0.0928 0.4446 0.2229 0.087 Uiso 1 1 calc R U . . .
H12B H 0.0943 0.5866 0.2741 0.087 Uiso 1 1 calc R U . . .
H12C H 0.0536 0.4351 0.3109 0.087 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'
Cl Cl 0.1484 0.1585 '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 64.99(7) . . ?
N2 Ge1 Cl1 94.24(6) . . ?
N1 Ge1 Cl1 93.48(5) . . ?
C2 N1 C1 123.29(19) . . ?
C2 N1 Ge1 143.19(15) . . ?
C1 N1 Ge1 93.39(13) . . ?
N1 C1 N2 105.34(18) . . ?
N1 C1 C5 120.4(2) . . ?
N2 C1 C5 134.2(2) . . ?
C1 N2 C7 128.10(19) . . ?
C1 N2 Ge1 96.16(13) . . ?
C7 N2 Ge1 135.71(15) . . ?
N1 C2 C3 118.4(2) . . ?
N1 C2 C6 117.2(2) . . ?
C3 C2 C6 124.3(2) . . ?
C2 C3 C4 119.2(2) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C7 N3 C8 118.2(2) . . ?
C5 C4 C3 122.2(2) . . ?
C5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C4 C5 C1 116.4(2) . . ?
C4 C5 H5 121.8 . . ?
C1 C5 H5 121.8 . . ?
N3 C7 N2 118.9(2) . . ?
N3 C7 C11 122.6(2) . . ?
N2 C7 C11 118.5(2) . . ?
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 . . ?
N3 C8 C9 122.7(2) . . ?
N3 C8 C12 114.8(2) . . ?
C9 C8 C12 122.5(2) . . ?
C8 C9 C10 118.6(2) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 119.7(2) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C7 118.2(2) . . ?
C10 C11 H11 120.9 . . ?
C7 C11 H11 120.9 . . ?
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 . . ?
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 N2 1.9843(18) . ?
Ge1 N1 2.0536(18) . ?
Ge1 Cl1 2.2812(6) . ?
N1 C2 1.340(3) . ?
N1 C1 1.359(3) . ?
C1 N2 1.370(3) . ?
C1 C5 1.396(3) . ?
N2 C7 1.379(3) . ?
C2 C3 1.384(3) . ?
C2 C6 1.492(3) . ?
C3 C4 1.390(3) . ?
C3 H3 0.9500 . ?
N3 C7 1.337(3) . ?
N3 C8 1.351(3) . ?
C4 C5 1.384(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C7 C11 1.398(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 C9 1.376(4) . ?
C8 C12 1.502(4) . ?
C9 C10 1.385(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
