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_7709105
_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         'C63 H91 Mg2 N4 P, C6 H14'
_chemical_formula_sum            'C69 H105 Mg2 N4 P'
_chemical_formula_weight         1070.15
_chemical_name_systematic
;
 [{N(2,6-iPr-C6H3)}2(CMe)2CH]2Mg2(tBuCP)*hex
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 111.490(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8841(4)
_cell_length_b                   11.3716(2)
_cell_length_c                   29.3532(5)
_cell_measurement_reflns_used    11377
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.6740
_cell_measurement_theta_min      3.2350
_cell_volume                     6796.9(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            31352
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.258
_diffrn_reflns_theta_min         3.236
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93965
_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            orange
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0594P)^2^+4.4468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5921
_reflns_number_total             7167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03990c2.cif
_cod_data_source_block           DW499
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7709105
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.937
_shelx_res_checksum              808
_shelx_hkl_checksum              74636