Reversible metathesis of ammonia in an acyclic germylene–Ni0 complex
Keil, Philip M.; Szilvási, Tibor; Hadlington, Terrance J.; Chemical Science 12 (2021) 5582–5590; doi:10.1039/D1SC00450F

data_1560851
_publ_section_title
;
 Reversible metathesis of ammonia in an acyclic germylene--Ni0 complex
;
_journal_issue                   15
_journal_name_full               'Chemical Science'
_journal_page_first              5582
_journal_page_last               5590
_journal_paper_doi               10.1039/D1SC00450F
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C73 H69 Br Ge N Ni P3 Si'
_chemical_formula_sum            'C73 H69 Br Ge N Ni P3 Si'
_chemical_formula_weight         1292.50
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                98.60(3)
_cell_angle_beta                 92.00(3)
_cell_angle_gamma                91.30(3)
_cell_formula_units_Z            2
_cell_length_a                   12.680(3)
_cell_length_b                   15.530(3)
_cell_length_c                   19.470(4)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      1.92
_cell_volume                     3787.1(14)
_computing_structure_refinement  'SHELXL-2018/3 (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 0.998
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56477
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_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    1.288
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            purple-brown
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The unit cell contains two hexane molecules and two toluene molecules (one each per asymmetric unit) which have been treated
as a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.882
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         15676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0531
_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/[\s^2^(Fo^2^)+(0.1019P)^2^+1.2355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11572
_reflns_number_total             15676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00450f2.cif
_cod_data_source_block           compound_4-Br
_cod_depositor_comments
'Adding full bibliography for 1560843--1560857.cif.'
_cod_original_cell_volume        3787.1(13)
_cod_database_code               1560851
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              34466
_shelx_hkl_checksum              10518