Diverse reactivity of a magnesium silanide toward ketones
Okokhere-Edeghoghon, Bibian; Hill, Michael S.; Mahon, Mary F.; McMullin, Claire L.; Chemical Communications  (2022) –; doi:10.1039/D2CC03966D

data_7130687
_publ_section_title
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 Diverse reactivity of a magnesium silanide toward ketones
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03966D
_journal_year                    2022
_chemical_formula_moiety         'C63 H70 F2 Mg N2 O2 Si'
_chemical_formula_sum            'C63 H70 F2 Mg N2 O2 Si'
_chemical_formula_weight         977.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2022-04-18 deposited with the CCDC.	2022-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.878(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7577(7)
_cell_length_b                   13.5109(3)
_cell_length_c                   22.2296(8)
_cell_measurement_reflns_used    6001
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.7790
_cell_measurement_theta_min      3.9500
_cell_volume                     5383.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38292
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.050
_diffrn_reflns_theta_min         3.938
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.616
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         10654
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0862P)^2^+1.7216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7393
_reflns_number_total             10654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03966d2.cif
_cod_data_source_block           s21msh106-cpd4
_cod_database_code               7130687
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F1-C40 \\sim F1A-C34A
 with sigma of 0.005
 F1-C41 \\sim C33A-F1A
 with sigma of 0.005
 F1-C39 \\sim C35A-F1A
 with sigma of 0.005
 C36-C34 \\sim C36A-C34A
 with sigma of 0.04
 C33-F1A \\sim C33A-F1A
 with sigma of 0.04
 C35-F1A \\sim C35A-F1A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C31A \\sim C32A
\\sim C33A \\sim C34A \\sim C35A \\sim C36A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: H40(0.15) F1(0.85) C31(0.85) C36(0.85) H36(0.85) C35(0.85)
 H35(0.85) C34(0.85) H34(0.85) C33(0.85) H33(0.85) C32(0.85) H32(0.85)
 F1A(0.15) C31A(0.15) C36A(0.15) H36A(0.15) C35A(0.15) H35A(0.15) C34A(0.15)
 C33A(0.15) H33A(0.15) C32A(0.15) H32A(0.15)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C55(H55)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C47(H47), C48(H48),
  C49(H49), C51(H51), C52(H52), C54(H54), C59(H59), C60(H60), C61(H61),
 C62(H62), C63(H63), C36(H36), C35(H35), C34(H34), C33(H33), C32(H32),
 C36A(H36A), C35A(H35A), C33A(H33A), C32A(H32A)
5.c Fitted hexagon refined as free rotating group:
 C31(C36,C35,C34,C33,C32), C31A(C36A,C35A,C34A,C33A,C32A)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C)
;
_shelx_res_checksum              62819
_shelx_hkl_checksum              38608
_olex2_submission_special_instructions 'No special instructions were received'