Accessing cationic tetrylene-nickel(0) systems featuring donor-acceptor E-Ni triple bonds (E = Ge, Sn)
Hadlington, Terrance J.; Keil, Philip Maximilian; Chemical Communications  (2022) –; doi:10.1039/D2CC00422D

data_7129674
_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         'C107 H95 B F24 N Ni P3 Si Sn, C6 H6'
_chemical_formula_sum            'C113 H101 B F24 N Ni P3 Si Sn'
_chemical_formula_weight         2238.15
_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                94.60(3)
_cell_angle_beta                 103.40(3)
_cell_angle_gamma                91.59(3)
_cell_formula_units_Z            2
_cell_length_a                   13.245(3)
_cell_length_b                   18.891(4)
_cell_length_c                   22.423(5)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.50
_cell_measurement_theta_min      1.92
_cell_volume                     5434(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w 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  0.1473
_diffrn_reflns_av_unetI/netI     0.2006
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71208
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.436
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            blue-purple
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       rod
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.755
_refine_diff_density_min         -1.657
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1323
_refine_ls_number_reflns         21204
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.2219
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1258P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2062
_refine_ls_wR_factor_ref         0.2688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9427
_reflns_number_total             21204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00422d2.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        5434.2(2)
_cod_database_code               7129674
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              48377
_shelx_hkl_checksum              1900