Reduction of tert-butylphosphaalkyne and trimethylsilylnitrile with magnesium(I) dimers
Wilson, Daniel; Jones, Dafydd; Smith, Cory; Mehta, Meera; Jones, Cameron; Goicoechea, Jose M.; Dalton Transactions  (2022) –; doi:10.1039/D1DT03990C

data_7709109
_publ_section_title
;
 Reduction of tert-butylphosphaalkyne and trimethylsilylnitrile with
 magnesium(I) dimers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03990C
_journal_year                    2022
_chemical_formula_moiety         'C60 H84 Mg2 N4 O P2'
_chemical_formula_sum            'C60 H84 Mg2 N4 O P2'
_chemical_formula_weight         987.87
_chemical_name_systematic
;
 [{N(2,4,6-Me-C6H2)}2(CMe)2CH]2Mg2(tBuCP)2(THF)
;
_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-2018/1
_audit_update_record
;
2021-11-24 deposited with the CCDC.	2021-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                72.352(4)
_cell_angle_beta                 76.371(4)
_cell_angle_gamma                73.373(5)
_cell_formula_units_Z            2
_cell_length_a                   11.6939(7)
_cell_length_b                   14.1088(6)
_cell_length_c                   19.7110(8)
_cell_measurement_reflns_used    6297
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.0740
_cell_measurement_theta_min      2.3590
_cell_volume                     2929.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21050
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.489
_diffrn_reflns_theta_max         66.489
_diffrn_reflns_theta_min         2.384
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       rod
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         10271
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+0.7043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7541
_reflns_number_total             10271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03990c2.cif
_cod_data_source_block           DW450B
_cod_database_code               7709109
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.648
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              62914
_shelx_hkl_checksum              1200