Magnesium hydrides bearing sterically demanding amidinate ligands: synthesis, reactivity and catalytic application.
Bakewell, Clare; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11354–11360; doi:10.1039/d0dt02523b

data_7705033
_publ_section_title
;
 Magnesium hydrides bearing sterically demanding amidinate ligands:
 synthesis, reactivity and catalytic application.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11354
_journal_page_last               11360
_journal_paper_doi               10.1039/d0dt02523b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C80 H79 Mg N3 Si2, C7 H8'
_chemical_formula_sum            'C87 H87 Mg N3 Si2'
_chemical_formula_weight         1255.08
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-16 deposited with the CCDC.	2020-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                84.511(2)
_cell_angle_beta                 69.542(2)
_cell_angle_gamma                64.578(2)
_cell_formula_units_Z            2
_cell_length_a                   15.6130(3)
_cell_length_b                   17.0913(3)
_cell_length_c                   17.1689(3)
_cell_measurement_reflns_used    34689
_cell_measurement_temperature    150.41(14)
_cell_measurement_theta_max      72.5720
_cell_measurement_theta_min      4.8750
_cell_volume                     3868.84(15)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.41(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -59.00 -20.00   1.00    1.26    --  -42.62 -77.00-150.00   39
  2  \w    -85.00 -12.00   1.00    1.26    --  -42.62 -77.00 -30.00   73
  3  \w    -59.00 -10.00   1.00    1.26    --  -42.62 -77.00  30.00   49
  4  \w   -118.00 -59.00   1.00    1.26    --  -42.62 -77.00-120.00   59
  5  \w    -36.00 -10.00   1.00    1.26    --  -42.62 -77.00-120.00   26
  6  \w    -93.00  -2.00   1.00    1.26    --  -42.62 125.00  60.00   91
  7  \w    -58.00 -14.00   1.00    1.26    --  -42.62 -57.00-120.00   44
  8  \w    -59.00  31.00   1.00    1.26    --  -42.62  38.00 -90.00   90
  9  \w   -113.00 -24.00   1.00    1.26    --  -42.62 -38.00 120.00   89
 10  \w    -72.00 -10.00   1.00    1.26    --  -42.62 -77.00 120.00   62
 11  \w   -112.00 -81.00   1.00    1.26    --  -42.62 -77.00 120.00   31
 12  \w      1.00  71.00   1.00    1.26    --   42.62 -99.00   0.00   70
 13  \w      2.00  73.00   1.00    1.26    --   42.62  19.00   0.00   71
 14  \w     87.00 119.00   1.00    1.26    --   42.62  19.00   0.00   32
 15  \w     75.00 113.00   1.00    5.05    --  104.49-125.00  30.00   38
 16  \w     75.00 162.00   1.00    5.05    --  104.49  62.00 148.51   87
 17  \w     75.00 146.00   1.00    5.05    --  104.49  64.00-173.30   71
 18  \w     73.00  99.00   1.00    5.05    --  104.49  71.00 168.72   26
 19  \w     76.00 102.00   1.00    5.05    --  104.49  59.00 -10.35   26
 20  \w     73.00  99.00   1.00    5.05    --  104.49  72.00  19.55   26
 21  \w     75.00 176.00   1.00    5.05    --  104.49  62.00 -47.90  101
 22  \w     22.00 101.00   1.00    5.05    --  104.49 -94.00 -90.00   79
 23  \w     31.00 118.00   1.00    5.05    --  104.49-125.00-180.00   87
 24  \w     72.00  98.00   1.00    5.05    --  104.49  77.00 150.00   26
 25  \w     95.00 167.00   1.00    5.05    --  104.49 125.00 -30.00   72
 26  \w     23.00 103.00   1.00    5.05    --  104.49 -94.00  60.00   80
 27  \w     72.00  98.00   1.00    5.05    --  104.49  77.00 -90.00   26
 28  \w     75.00 101.00   1.00    5.05    --  104.49  61.00 -30.00   26
 29  \w     77.00 136.00   1.00    5.05    --  104.49  60.00 112.10   59
 30  \w     72.00  98.00   1.00    5.05    --  104.49  77.00  60.00   26
 31  \w     75.00 114.00   1.00    5.05    --  104.49  61.00  90.00   39
 32  \w     72.00 177.00   1.00    5.05    --  104.49  77.00-120.00  105
 33  \w     74.00  99.00   1.00    5.05    --  104.49  72.00-130.83   25
 34  \w     75.00 177.00   1.00    5.05    --  104.49  61.00-144.61  102
 35  \w     31.00 115.00   1.00    5.05    --  104.49 -45.00 -90.00   84
 36  \w     76.00 134.00   1.00    5.05    --  104.49  61.00 -60.00   58
 37  \w     72.00  98.00   1.00    5.05    --  104.49  77.00-150.00   26
 38  \w    146.00 173.00   1.00    5.05    --  104.49  61.00   0.00   27
 39  \w     78.00 107.00   1.00    5.05    --  104.49 -94.00-180.00   29
 40  \w     72.00  98.00   1.00    5.05    --  104.49  77.00   0.00   26
 41  \w     72.00  98.00   1.00    5.05    --  104.49  75.00-102.54   26
 42  \w    115.00 141.00   1.00    5.05    --  104.49  61.00  90.00   26
 43  \w     73.00  98.00   1.00    5.05    --  104.49  77.00 -60.00   25
 44  \w     75.00 139.00   1.00    5.05    --  104.49  61.00   0.00   64
 45  \w     38.00  69.00   1.00    5.05    --  104.49 -94.00-180.00   31
 46  \w     75.00 157.00   1.00    5.05    --  104.49  61.00 120.00   82
 47  \w     72.00  99.00   1.00    5.05    --  104.49  77.00-180.00   27
 48  \w     74.00 101.00   1.00    5.05    --  104.49  68.00  34.65   27
 49  \w     74.00 177.00   1.00    5.05    --  104.49  68.00  51.82  103
 50  \w     73.00  99.00   1.00    5.05    --  104.49  71.00  -0.86   26
 51  \w     74.00 101.00   1.00    5.05    --  104.49  68.00  90.67   27
 52  \w     74.00 100.00   1.00    5.05    --  104.49  66.00 132.24   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0246146000
_diffrn_orient_matrix_UB_12      0.0736958000
_diffrn_orient_matrix_UB_13      0.0606300000
_diffrn_orient_matrix_UB_21      0.0850387000
_diffrn_orient_matrix_UB_22      -0.0615449000
_diffrn_orient_matrix_UB_23      0.0320612000
_diffrn_orient_matrix_UB_31      0.0754373000
_diffrn_orient_matrix_UB_32      0.0279772000
_diffrn_orient_matrix_UB_33      -0.0671275000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66096
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.769
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene/hexane'
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         15170
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0532P)^2^+1.6308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13228
_reflns_number_total             15170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02523b2.cif
_cod_data_source_block           xstr1057
_cod_depositor_comments
'Adding full bibliography for 7705030--7705034.cif.'
_cod_original_cell_volume        3868.85(14)
_cod_database_code               7705033
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mg C85 H79 N3 Si'
_chemical_oxdiff_usercomment     CB-122
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
 C86-C85 \\sim C85-C84 \\sim C84-C83 \\sim C83-C82 \\sim C82-C81 \\sim C81-C86
 with sigma of 0.02
 C86-C82 \\sim C86-C84 \\sim C81-C83 \\sim C85-C81 \\sim C84-C82 \\sim C85-C83
 with sigma of 0.04
 C87-C81 \\sim C87-C85
 with sigma of 0.04
3. Restrained planarity
 C87, C86, C85, C84, C83, C82, C81
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C87 \\sim C86 \\sim C85 \\sim C84 \\sim C83 \\sim C82 \\sim C81: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C87, C86, C85, C84, C83, C82, C81
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C27(H27), C23(H23), C53(H53), C26(H26), C24(H24), C25(H25),
 C12(H12), C11(H11), C31(H31), C72(H72), C71(H71), C59(H59), C19(H19), C70(H70),
  C85(H85), C84(H84), C83(H83), C82(H82), C81(H81)
6.b Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C48(H48A,H48B,H48C), C7(H7A,H7B,H7C), C80(H80A,H80B,
 H80C), C75(H75A,H75B,H75C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C87(H87A,
 H87B,H87C)
;
_shelx_res_checksum              48867
_shelx_fab_checksum              94310
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.699
_oxdiff_exptl_absorpt_empirical_full_min 0.684