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_7705032
_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         'C59 H69 Mg N3 Si2'
_chemical_formula_sum            'C59 H69 Mg N3 Si2'
_chemical_formula_weight         900.66
_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   geom
_atom_sites_solution_primary     direct
_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                97.5417(18)
_cell_angle_beta                 99.133(2)
_cell_angle_gamma                116.233(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3496(3)
_cell_length_b                   12.7732(3)
_cell_length_c                   19.2070(4)
_cell_measurement_reflns_used    22460
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1540
_cell_measurement_theta_min      4.0560
_cell_volume                     2612.97(13)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_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 0.982
_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   -112.00 -10.00   1.00    1.00    --  -42.62 -77.00 -90.00  102
  2  \w   -117.00 -10.00   1.00    1.00    --  -42.62 -77.00  60.00  107
  3  \w    -74.00 -17.00   1.00    1.00    --  -42.62 -77.00 150.00   57
  4  \w    -65.00  29.00   1.00    1.00    --  -42.62  57.00-180.00   94
  5  \w    -50.00 -14.00   1.00    1.00    --  -42.62 -57.00 150.00   36
  6  \w    -68.00  26.00   1.00    1.00    --  -42.62  57.00 -30.00   94
  7  \w    -95.00 -21.00   1.00    1.00    --  -42.62 -38.00 -90.00   74
  8  \w    -42.00 -11.00   1.00    1.00    --  -42.62 -77.00-150.00   31
  9  \w   -118.00 -80.00   1.00    1.00    --  -42.62 -77.00-150.00   38
 10  \w    -58.00 -10.00   1.00    1.00    --  -42.62 -77.00 -30.00   48
 11  \w   -117.00 -85.00   1.00    1.00    --  -42.62 -77.00 150.00   32
 12  \w     25.00  75.00   1.00    1.00    --   42.62-125.00 -90.00   50
 13  \w      2.00  71.00   1.00    1.00    --   42.62 -99.00  60.00   69
 14  \w      7.00  32.00   1.00    1.00    --   42.62  87.00 -19.06   25
 15  \w     33.00 116.00   1.00    3.94    --  106.06-125.00  30.00   83
 16  \w     73.00  99.00   1.00    3.94    --  106.06  77.00   0.00   26
 17  \w     30.00 139.00   1.00    3.94    --  106.06 -77.00  30.00  109
 18  \w     77.00 138.00   1.00    3.94    --  106.06  61.00 150.00   61
 19  \w     73.00 102.00   1.00    3.94    --  106.06  77.00  60.00   29
 20  \w     75.00 101.00   1.00    3.94    --  106.06  71.00  20.79   26
 21  \w     73.00 177.00   1.00    3.94    --  106.06  77.00  81.76  104
 22  \w     73.00 175.00   1.00    3.94    --  106.06  77.00-150.00  102
 23  \w    103.00 133.00   1.00    3.94    --  106.06  77.00 120.00   30
 24  \w     73.00 101.00   1.00    3.94    --  106.06  77.00 -30.00   28
 25  \w     77.00 141.00   1.00    3.94    --  106.06  61.00 -30.00   64
 26  \w    146.00 172.00   1.00    3.94    --  106.06  61.00 150.00   26
 27  \w     77.00 102.00   1.00    3.94    --  106.06  61.00 120.00   25
 28  \w     30.00 135.00   1.00    3.94    --  106.06 -77.00-180.00  105
 29  \w     73.00  99.00   1.00    3.94    --  106.06  77.00  30.00   26
 30  \w    108.00 140.00   1.00    3.94    --  106.06  77.00  30.00   32
 31  \w     78.00 103.00   1.00    3.94    --  106.06  61.00-150.00   25
 32  \w    127.00 154.00   1.00    3.94    --  106.06  61.00 -78.03   27
 33  \w     73.00  99.00   1.00    3.94    --  106.06  77.00 150.00   26
 34  \w     77.00 105.00   1.00    3.94    --  106.06  61.00 -90.00   28
 35  \w     73.00  98.00   1.00    3.94    --  106.06  77.00-180.00   25
 36  \w    111.00 178.00   1.00    3.94    --  106.06  77.00-120.00   67
 37  \w     77.00 166.00   1.00    3.94    --  106.06  61.00-180.00   89
 38  \w     77.00 175.00   1.00    3.94    --  106.06  61.00 -60.00   98
 39  \w     73.00  98.00   1.00    3.94    --  106.06  77.00 -60.00   25
 40  \w     73.00  98.00   1.00    3.94    --  106.06  77.00-120.00   25
 41  \w     88.00 117.00   1.00    3.94    --  106.06-125.00-180.00   29
 42  \w     73.00  99.00   1.00    3.94    --  106.06  77.00 120.00   26
 43  \w     77.00 103.00   1.00    3.94    --  106.06  61.00-120.00   26
 44  \w    143.00 174.00   1.00    3.94    --  106.06  77.00  30.00   31
 45  \w     77.00 172.00   1.00    3.94    --  106.06  61.00  60.00   95
 46  \w     78.00 103.00   1.00    3.94    --  106.06  61.00 -78.03   25
 47  \w     75.00 177.00   1.00    3.94    --  106.06  71.00  -6.10  102
;
_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      -0.0728189000
_diffrn_orient_matrix_UB_12      -0.0701146000
_diffrn_orient_matrix_UB_13      -0.0782099000
_diffrn_orient_matrix_UB_21      -0.0775515000
_diffrn_orient_matrix_UB_22      -0.1102504000
_diffrn_orient_matrix_UB_23      0.0284059000
_diffrn_orient_matrix_UB_31      -0.0961508000
_diffrn_orient_matrix_UB_32      0.0446486000
_diffrn_orient_matrix_UB_33      0.0059958000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41210
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.514
_diffrn_reflns_theta_min         3.962
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.677
_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    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene/hexane'
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0385
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9018
_reflns_number_total             10353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02523b2.cif
_cod_data_source_block           xstr0963
_cod_depositor_comments
'Adding full bibliography for 7705030--7705034.cif.'
_cod_original_cell_volume        2612.97(12)
_cod_database_code               7705032
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mg Si2 C59 H69 N3'
_chemical_oxdiff_usercomment     CB-049
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C41(H41), C28(H28), C10(H10), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25), C19(H19), C53(H53), C47(H47), C36(H36), C32(H32), C5(H5),
 C3(H3), C30(H30), C34(H34), C33(H33), C52(H52), C49(H49), C18(H18), C15(H15),
 C51(H51), C46(H46), C40(H40), C50(H50), C4(H4), C37(H37), C31(H31), C16(H16),
 C45(H45), C43(H43), C38(H38), C39(H39), C44(H44)
2.c Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C54(H54a,H54b,H54c), C12(H12a,H12b,H12c), C11(H11a,H11b,
 H11c), C20(H20a,H20b,H20c), C57(H57a,H57b,H57c), C55(H55a,H55b,H55c), C8(H8a,
 H8b,H8c), C9(H9a,H9b,H9c), C59(H59a,H59b,H59c), C56(H56a,H56b,H56c), C58(H58a,
 H58b,H58c)
;
_shelx_res_checksum              32831
_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 1.332
_oxdiff_exptl_absorpt_empirical_full_min 0.762