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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/7/70/70/7707035.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_7707035
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            'C20 H16 N6 Sn'
_chemical_formula_weight         459.08
_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_method           SHELXL-2017/1
_audit_update_record
;
2020-09-21 deposited with the CCDC.	2021-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.129(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8487(6)
_cell_length_b                   9.2747(4)
_cell_length_c                   16.9821(9)
_cell_measurement_reflns_used    38955
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1809.76(15)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0349
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38955
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.533
_diffrn_reflns_theta_min         2.473
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6017
_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    1.685
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.587
_exptl_crystal_size_mid          0.567
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4154
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0226
_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)+(0.0249P)²+1.2224P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3733
_reflns_number_total             4154
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00717c4.cif
_cod_data_source_block           ld190306sn1
_cod_depositor_comments
'Adding full bibliography for 7707027--7707037.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7707035
_shelx_shelxl_version_number     2017/1
_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 0.802
;
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
Sn1 Sn 0.24428(2) 0.38494(2) 0.60324(2) 0.02420(5) Uani 1 1 d . . . . .
N1 N 0.23619(14) 0.63538(19) 0.61054(10) 0.0227(3) Uani 1 1 d . . . . .
C1 C 0.17501(16) 0.6517(2) 0.53220(12) 0.0207(4) Uani 1 1 d . . . . .
C2 C 0.25580(17) 0.7473(2) 0.66156(12) 0.0275(4) Uani 1 1 d . . . . .
H2 H 0.297611 0.731829 0.716188 0.033 Uiso 1 1 calc R U . . .
N2 N 0.16158(14) 0.51973(18) 0.49575(10) 0.0220(3) Uani 1 1 d . . . . .
N3 N 0.07281(15) 0.59579(18) 0.36195(10) 0.0238(3) Uani 1 1 d . . . . .
C3 C 0.21761(18) 0.8842(2) 0.63779(14) 0.0290(4) Uani 1 1 d . . . . .
H3 H 0.231932 0.962544 0.674906 0.035 Uiso 1 1 calc R U . . .
C4 C 0.15690(19) 0.9035(2) 0.55692(14) 0.0291(4) Uani 1 1 d . . . . .
H4 H 0.130339 0.997197 0.538598 0.035 Uiso 1 1 calc R U . . .
N4 N 0.32386(14) 0.24663(18) 0.49681(10) 0.0235(3) Uani 1 1 d . . . . .
N5 N 0.41984(14) 0.40024(18) 0.58996(10) 0.0223(3) Uani 1 1 d . . . . .
C5 C 0.13473(17) 0.7895(2) 0.50313(12) 0.0252(4) Uani 1 1 d . . . . .
H5 H 0.093582 0.803398 0.448196 0.030 Uiso 1 1 calc R U . . .
C6 C 0.09923(15) 0.4900(2) 0.41731(11) 0.0197(4) Uani 1 1 d . . . . .
N6 N 0.46274(14) 0.50537(18) 0.71346(10) 0.0234(3) Uani 1 1 d . . . . .
C7 C 0.01552(18) 0.5588(2) 0.28627(13) 0.0272(4) Uani 1 1 d . . . . .
H7 H -0.003830 0.633550 0.247021 0.033 Uiso 1 1 calc R U . . .
C9 C 0.00993(17) 0.3118(2) 0.31969(13) 0.0273(4) Uani 1 1 d . . . . .
H9 H -0.011277 0.214713 0.305492 0.033 Uiso 1 1 calc R U . . .
C8 C -0.01723(18) 0.4201(2) 0.26147(13) 0.0282(4) Uani 1 1 d . . . . .
H8 H -0.056682 0.399389 0.206903 0.034 Uiso 1 1 calc R U . . .
C10 C 0.06739(17) 0.3459(2) 0.39757(13) 0.0248(4) Uani 1 1 d . . . . .
H10 H 0.085607 0.272967 0.437939 0.030 Uiso 1 1 calc R U . . .
C11 C 0.43003(17) 0.3031(2) 0.53135(12) 0.0214(4) Uani 1 1 d . . . . .
C12 C 0.31295(19) 0.1502(2) 0.43684(13) 0.0279(4) Uani 1 1 d . . . . .
H12 H 0.237917 0.112231 0.412985 0.033 Uiso 1 1 calc R U . . .
C13 C 0.4062(2) 0.1034(2) 0.40813(14) 0.0328(5) Uani 1 1 d . . . . .
H13 H 0.395974 0.035755 0.364957 0.039 Uiso 1 1 calc R U . . .
C14 C 0.5146(2) 0.1584(3) 0.44439(15) 0.0347(5) Uani 1 1 d . . . . .
H14 H 0.580535 0.126959 0.426512 0.042 Uiso 1 1 calc R U . . .
C15 C 0.52884(18) 0.2582(2) 0.50606(14) 0.0298(5) Uani 1 1 d . . . . .
H15 H 0.603648 0.295717 0.530921 0.036 Uiso 1 1 calc R U . . .
C16 C 0.50435(16) 0.4656(2) 0.64933(11) 0.0204(4) Uani 1 1 d . . . . .
C17 C 0.53433(19) 0.5747(2) 0.77476(13) 0.0275(4) Uani 1 1 d . . . . .
H17 H 0.504382 0.603670 0.819337 0.033 Uiso 1 1 calc R U . . .
C18 C 0.64900(19) 0.6069(2) 0.77754(14) 0.0305(5) Uani 1 1 d . . . . .
H18 H 0.697303 0.654220 0.823074 0.037 Uiso 1 1 calc R U . . .
C19 C 0.69079(19) 0.5673(3) 0.71124(15) 0.0329(5) Uani 1 1 d . . . . .
H19 H 0.768885 0.588886 0.710462 0.039 Uiso 1 1 calc R U . . .
C20 C 0.61935(18) 0.4967(2) 0.64630(13) 0.0284(4) Uani 1 1 d . . . . .
H20 H 0.647322 0.469595 0.600535 0.034 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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
N5 Sn1 N2 96.89(6) . . ?
N5 Sn1 N1 89.61(6) . . ?
N2 Sn1 N1 57.96(6) . . ?
N5 Sn1 N4 55.26(6) . . ?
N2 Sn1 N4 82.40(6) . . ?
N1 Sn1 N4 124.12(5) . . ?
C2 N1 C1 120.98(18) . . ?
C2 N1 Sn1 143.78(14) . . ?
C1 N1 Sn1 94.49(12) . . ?
N1 C1 N2 108.63(17) . . ?
N1 C1 C5 119.86(18) . . ?
N2 C1 C5 131.49(18) . . ?
N1 C2 C3 122.32(19) . . ?
N1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C1 N2 C6 126.26(16) . . ?
C1 N2 Sn1 98.76(12) . . ?
C6 N2 Sn1 134.45(13) . . ?
C6 N3 C7 117.44(17) . . ?
C2 C3 C4 117.45(19) . . ?
C2 C3 H3 121.3 . . ?
C4 C3 H3 121.3 . . ?
C5 C4 C3 121.4(2) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C12 N4 C11 119.62(17) . . ?
C12 N4 Sn1 152.04(14) . . ?
C11 N4 Sn1 87.95(11) . . ?
C11 N5 C16 130.15(16) . . ?
C11 N5 Sn1 106.97(12) . . ?
C16 N5 Sn1 120.10(13) . . ?
C4 C5 C1 117.97(19) . . ?
C4 C5 H5 121.0 . . ?
C1 C5 H5 121.0 . . ?
N3 C6 N2 120.47(17) . . ?
N3 C6 C10 121.63(18) . . ?
N2 C6 C10 117.88(17) . . ?
C17 N6 C16 118.16(18) . . ?
N3 C7 C8 124.7(2) . . ?
N3 C7 H7 117.7 . . ?
C8 C7 H7 117.7 . . ?
C10 C9 C8 119.61(19) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C7 C8 C9 117.21(19) . . ?
C7 C8 H8 121.4 . . ?
C9 C8 H8 121.4 . . ?
C9 C10 C6 119.43(19) . . ?
C9 C10 H10 120.3 . . ?
C6 C10 H10 120.3 . . ?
N4 C11 N5 109.34(16) . . ?
N4 C11 C15 120.49(19) . . ?
N5 C11 C15 130.17(19) . . ?
N4 C12 C13 122.8(2) . . ?
N4 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C14 C13 C12 117.7(2) . . ?
C14 C13 H13 121.2 . . ?
C12 C13 H13 121.2 . . ?
C15 C14 C13 121.0(2) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C11 118.4(2) . . ?
C14 C15 H15 120.8 . . ?
C11 C15 H15 120.8 . . ?
N6 C16 N5 111.55(16) . . ?
N6 C16 C20 121.40(18) . . ?
N5 C16 C20 126.99(18) . . ?
N6 C17 C18 124.3(2) . . ?
N6 C17 H17 117.9 . . ?
C18 C17 H17 117.9 . . ?
C17 C18 C19 117.3(2) . . ?
C17 C18 H18 121.3 . . ?
C19 C18 H18 121.3 . . ?
C20 C19 C18 120.2(2) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C16 118.6(2) . . ?
C19 C20 H20 120.7 . . ?
C16 C20 H20 120.7 . . ?
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
Sn1 N5 2.1512(16) . ?
Sn1 N2 2.2321(16) . ?
Sn1 N1 2.3293(17) . ?
Sn1 N4 2.5756(16) . ?
N1 C2 1.336(3) . ?
N1 C1 1.359(2) . ?
C1 N2 1.364(3) . ?
C1 C5 1.410(3) . ?
C2 C3 1.374(3) . ?
C2 H2 0.9500 . ?
N2 C6 1.384(2) . ?
N3 C6 1.342(2) . ?
N3 C7 1.343(3) . ?
C3 C4 1.398(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
N4 C12 1.338(3) . ?
N4 C11 1.357(3) . ?
N5 C11 1.370(3) . ?
N5 C16 1.376(3) . ?
C5 H5 0.9500 . ?
C6 C10 1.407(3) . ?
N6 C17 1.336(3) . ?
N6 C16 1.352(3) . ?
C7 C8 1.380(3) . ?
C7 H7 0.9500 . ?
C9 C10 1.369(3) . ?
C9 C8 1.391(3) . ?
C9 H9 0.9500 . ?
C8 H8 0.9500 . ?
C10 H10 0.9500 . ?
C11 C15 1.405(3) . ?
C12 C13 1.382(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.380(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C20 1.406(3) . ?
C17 C18 1.381(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
