#------------------------------------------------------------------------------
#$Date: 2022-02-08 00:54:25 +0200 (Tue, 08 Feb 2022) $
#$Revision: 272841 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/96/7129672.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_7129672
loop_
_publ_author_name
'Hadlington, Terrance J.'
'Keil, Philip Maximilian'
_publ_section_title
;
 Accessing cationic tetrylene-nickel(0) systems featuring donor-acceptor
 E-Ni triple bonds (E = Ge, Sn)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00422D
_journal_year                    2022
_chemical_formula_moiety         'C42 H76 Cl2 N2 Si2 Sn2'
_chemical_formula_sum            'C42 H76 Cl2 N2 Si2 Sn2'
_chemical_formula_weight         973.50
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-02-03 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                101.80(3)
_cell_angle_beta                 96.15(3)
_cell_angle_gamma                109.26(3)
_cell_formula_units_Z            1
_cell_length_a                   9.148(2)
_cell_length_b                   9.655(2)
_cell_length_c                   15.011(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.50
_cell_measurement_theta_min      1.92
_cell_volume                     1203.1(6)
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_collection       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0131
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16820
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.663
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0167
_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)+(0.0270P)²+0.2471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4323
_reflns_number_total             4727
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc00422d2.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        1203.1(5)
_cod_database_code               7129672
_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.
;
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
Sn1 Sn 0.93406(2) 0.32806(2) 0.88197(2) 0.02858(4) Uani 1 1 d . . . . .
Si1 Si 0.74515(4) 0.53570(4) 0.77101(3) 0.01903(8) Uani 1 1 d . . . . .
Cl1 Cl 1.15756(5) 0.59410(5) 0.95383(3) 0.04102(11) Uani 1 1 d . . . . .
N1 N 0.78333(13) 0.37393(12) 0.78776(8) 0.0184(2) Uani 1 1 d . . . . .
C1 C 0.70104(15) 0.22425(15) 0.72446(9) 0.0171(3) Uani 1 1 d . . . . .
C6 C 0.56306(16) 0.12273(15) 0.74376(10) 0.0189(3) Uani 1 1 d . . . . .
C2 C 0.76170(16) 0.17450(15) 0.64565(10) 0.0192(3) Uani 1 1 d . . . . .
C5 C 0.48705(17) -0.02183(16) 0.68272(10) 0.0237(3) Uani 1 1 d . . . . .
H5 H 0.394330 -0.089718 0.695254 0.028 Uiso 1 1 calc R U . . .
C3 C 0.68080(18) 0.02947(16) 0.58718(10) 0.0235(3) Uani 1 1 d . . . . .
H3 H 0.720603 -0.003233 0.534117 0.028 Uiso 1 1 calc R U . . .
C10 C 0.49355(17) 0.16064(16) 0.82904(10) 0.0226(3) Uani 1 1 d . . . . .
H10 H 0.550974 0.270464 0.860901 0.027 Uiso 1 1 calc R U . . .
C16 C 0.53346(17) 0.47064(16) 0.70669(11) 0.0236(3) Uani 1 1 d . . . . .
H16 H 0.468607 0.394091 0.736411 0.028 Uiso 1 1 calc R U . . .
C7 C 0.91518(17) 0.27084(17) 0.62284(11) 0.0258(3) Uani 1 1 d . . . . .
H7 H 0.953892 0.373087 0.667733 0.031 Uiso 1 1 calc R U . . .
C19 C 0.88322(17) 0.63378(16) 0.69769(11) 0.0252(3) Uani 1 1 d . . . . .
H19 H 0.868172 0.553830 0.639793 0.030 Uiso 1 1 calc R U . . .
C13 C 0.77585(19) 0.66230(17) 0.89149(11) 0.0296(3) Uani 1 1 d . . . . .
H13 H 0.869019 0.653963 0.928269 0.035 Uiso 1 1 calc R U . . .
C4 C 0.54409(18) -0.06750(16) 0.60487(10) 0.0255(3) Uani 1 1 d . . . . .
H4 H 0.489715 -0.164998 0.563678 0.031 Uiso 1 1 calc R U . . .
C21 C 1.05862(19) 0.68847(18) 0.74196(12) 0.0329(4) Uani 1 1 d . . . . .
H21A H 1.123406 0.724626 0.697596 0.049 Uiso 1 1 calc R U . . .
H21B H 1.082168 0.604274 0.758838 0.049 Uiso 1 1 calc R U . . .
H21C H 1.082123 0.771375 0.797675 0.049 Uiso 1 1 calc R U . . .
C18 C 0.5087(2) 0.3889(2) 0.60416(11) 0.0323(4) Uani 1 1 d . . . . .
H18A H 0.397530 0.357136 0.575447 0.048 Uiso 1 1 calc R U . . .
H18B H 0.538554 0.299409 0.599232 0.048 Uiso 1 1 calc R U . . .
H18C H 0.574377 0.457771 0.572304 0.048 Uiso 1 1 calc R U . . .
C12 C 0.31769(18) 0.13436(19) 0.80357(13) 0.0328(4) Uani 1 1 d . . . . .
H12A H 0.303403 0.194078 0.760127 0.049 Uiso 1 1 calc R U . . .
H12B H 0.278983 0.165798 0.859783 0.049 Uiso 1 1 calc R U . . .
H12C H 0.258428 0.026425 0.774545 0.049 Uiso 1 1 calc R U . . .
C20 C 0.8467(2) 0.76275(19) 0.66526(14) 0.0392(4) Uani 1 1 d . . . . .
H20A H 0.855427 0.843382 0.719442 0.059 Uiso 1 1 calc R U . . .
H20B H 0.739412 0.722721 0.628701 0.059 Uiso 1 1 calc R U . . .
H20C H 0.922139 0.803909 0.627065 0.059 Uiso 1 1 calc R U . . .
C14 C 0.6378(2) 0.6050(2) 0.94147(13) 0.0417(4) Uani 1 1 d . . . . .
H14A H 0.669881 0.657480 1.007559 0.063 Uiso 1 1 calc R U . . .
H14B H 0.608622 0.495524 0.934000 0.063 Uiso 1 1 calc R U . . .
H14C H 0.547029 0.625517 0.914610 0.063 Uiso 1 1 calc R U . . .
C15 C 0.8178(3) 0.83345(18) 0.89930(14) 0.0465(5) Uani 1 1 d . . . . .
H15A H 0.730599 0.848974 0.863938 0.070 Uiso 1 1 calc R U . . .
H15B H 0.913628 0.872068 0.874372 0.070 Uiso 1 1 calc R U . . .
H15C H 0.835628 0.887887 0.964550 0.070 Uiso 1 1 calc R U . . .
C8 C 0.8938(2) 0.2930(2) 0.52474(12) 0.0360(4) Uani 1 1 d . . . . .
H8A H 0.860152 0.194537 0.479327 0.054 Uiso 1 1 calc R U . . .
H8B H 0.994109 0.360210 0.514837 0.054 Uiso 1 1 calc R U . . .
H8C H 0.813595 0.338530 0.517304 0.054 Uiso 1 1 calc R U . . .
C11 C 0.5156(2) 0.06715(19) 0.89751(11) 0.0339(4) Uani 1 1 d . . . . .
H11A H 0.457500 -0.040920 0.868299 0.051 Uiso 1 1 calc R U . . .
H11B H 0.475500 0.097900 0.953265 0.051 Uiso 1 1 calc R U . . .
H11C H 0.628001 0.084933 0.914565 0.051 Uiso 1 1 calc R U . . .
C17 C 0.4625(2) 0.5966(2) 0.71508(14) 0.0396(4) Uani 1 1 d . . . . .
H17A H 0.522796 0.675484 0.687349 0.059 Uiso 1 1 calc R U . . .
H17B H 0.467365 0.641116 0.780652 0.059 Uiso 1 1 calc R U . . .
H17C H 0.352336 0.552835 0.682567 0.059 Uiso 1 1 calc R U . . .
C9 C 1.0404(2) 0.1994(2) 0.63570(15) 0.0448(5) Uani 1 1 d . . . . .
H9A H 1.054824 0.188005 0.699092 0.067 Uiso 1 1 calc R U . . .
H9B H 1.140454 0.265063 0.624630 0.067 Uiso 1 1 calc R U . . .
H9C H 1.005794 0.099591 0.591592 0.067 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'
Si Si 0.0817 0.0704 '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'
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
N1 Sn1 Cl1 102.88(4) . . ?
N1 Sn1 Cl1 103.19(4) . 2_767 ?
Cl1 Sn1 Cl1 80.56(4) . 2_767 ?
N1 Si1 C13 105.81(7) . . ?
N1 Si1 C16 108.21(7) . . ?
C13 Si1 C16 111.70(8) . . ?
N1 Si1 C19 110.21(6) . . ?
C13 Si1 C19 112.12(8) . . ?
C16 Si1 C19 108.70(7) . . ?
Sn1 Cl1 Sn1 99.44(4) . 2_767 ?
C1 N1 Si1 121.90(9) . . ?
C1 N1 Sn1 101.47(8) . . ?
Si1 N1 Sn1 136.61(7) . . ?
C6 C1 C2 119.02(12) . . ?
C6 C1 N1 120.01(12) . . ?
C2 C1 N1 120.88(12) . . ?
C5 C6 C1 119.11(13) . . ?
C5 C6 C10 117.43(13) . . ?
C1 C6 C10 123.44(13) . . ?
C3 C2 C1 119.30(13) . . ?
C3 C2 C7 117.70(13) . . ?
C1 C2 C7 122.98(13) . . ?
C4 C5 C6 121.44(14) . . ?
C4 C3 C2 121.43(14) . . ?
C6 C10 C12 111.96(13) . . ?
C6 C10 C11 111.13(12) . . ?
C12 C10 C11 109.34(13) . . ?
C18 C16 C17 109.40(13) . . ?
C18 C16 Si1 113.59(11) . . ?
C17 C16 Si1 114.70(12) . . ?
C2 C7 C8 112.69(13) . . ?
C2 C7 C9 109.90(13) . . ?
C8 C7 C9 110.19(14) . . ?
C21 C19 C20 110.00(13) . . ?
C21 C19 Si1 113.39(11) . . ?
C20 C19 Si1 115.72(11) . . ?
C14 C13 C15 109.80(14) . . ?
C14 C13 Si1 112.66(11) . . ?
C15 C13 Si1 116.62(12) . . ?
C5 C4 C3 119.62(14) . . ?
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 N1 2.0826(13) . ?
Sn1 Cl1 2.6203(13) . ?
Sn1 Cl1 2.7291(8) 2_767 ?
Si1 N1 1.7692(12) . ?
Si1 C13 1.8983(17) . ?
Si1 C16 1.9032(17) . ?
Si1 C19 1.9079(16) . ?
N1 C1 1.4575(18) . ?
C1 C6 1.420(2) . ?
C1 C2 1.423(2) . ?
C6 C5 1.404(2) . ?
C6 C10 1.522(2) . ?
C2 C3 1.397(2) . ?
C2 C7 1.525(2) . ?
C5 C4 1.380(2) . ?
C3 C4 1.383(2) . ?
C10 C12 1.535(2) . ?
C10 C11 1.539(2) . ?
C16 C18 1.534(2) . ?
C16 C17 1.547(2) . ?
C7 C8 1.532(2) . ?
C7 C9 1.534(2) . ?
C19 C21 1.537(2) . ?
C19 C20 1.546(2) . ?
C13 C14 1.542(2) . ?
C13 C15 1.545(2) . ?
