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_7705031
_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         'C106 H103.37 Mg2 N4 O0.63'
_chemical_formula_sum            'C106 H103.39 Mg2 N4 O0.61'
_chemical_formula_weight         1491.62
_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             2020-07-16
_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                95.5850(10)
_cell_angle_beta                 97.1380(10)
_cell_angle_gamma                112.921(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5273(2)
_cell_length_b                   13.5524(2)
_cell_length_c                   28.3251(4)
_cell_measurement_reflns_used    39082
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      72.6000
_cell_measurement_theta_min      3.6210
_cell_volume                     4684.98(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      149.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4061
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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     -5.00  20.00   1.00    2.50    --   34.00  94.00-175.65   25
  2  \w     -3.00  22.00   1.00    2.50    --   34.00  89.00 -34.81   25
  3  \w      2.00  31.00   1.00    2.50    --   38.00  87.00 116.58   29
  4  \w   -116.00 -18.00   1.00    2.50    --  -42.75 -38.00-120.00   98
  5  \w   -122.00  -4.00   1.00    2.50    --  -42.75 -19.00 -30.00  118
  6  \w    -67.00  28.00   1.00    2.50    --  -42.75  38.00 -30.00   95
  7  \w    -67.00  31.00   1.00    2.50    --  -42.75  38.00  60.00   98
  8  \w      8.00  33.00   1.00    2.50    --   42.75  83.00  26.67   25
  9  \w      8.00  33.00   1.00    2.50    --   42.75  83.00-139.98   25
 10  \w     28.00  99.00   1.00    2.50    --   42.75-125.00-150.00   71
 11  \w     14.00  39.00   1.00    2.50    --   46.00  76.00 147.98   25
 12  \w     30.00  56.00   1.00    2.50    --   58.00  74.00-149.65   26
 13  \w     31.00  57.00   1.00    2.50    --   62.00  72.00  77.78   26
 14  \w    101.00 127.00   1.00    2.50    --   62.00  73.00 -59.95   26
 15  \w    109.00 134.00   1.00    2.50    --   62.00  74.00-113.39   25
 16  \w     31.00  57.00   1.00    2.50    --   62.00  74.00 112.11   26
 17  \w     30.00  58.00   1.00    2.50    --   62.00  73.00 155.13   28
 18  \w     30.00  56.00   1.00    2.50    --   62.00  74.00-113.39   26
 19  \w     30.00  60.00   1.00    2.50    --   62.00  73.00 -59.95   30
 20  \w     37.00  65.00   1.00    2.50    --   66.00  69.00  57.97   28
 21  \w    118.00 144.00   1.00    2.50    --   70.00  72.00 -21.34   26
 22  \w     39.00  65.00   1.00    2.50    --   70.00  72.00 -21.34   26
 23  \w     38.00  65.00   1.00    2.50    --   70.00  73.00  10.11   27
 24  \w     38.00  64.00   1.00    2.50    --   70.00  74.00 173.25   26
 25  \w     50.00  76.00   1.00   10.00    --   78.00  71.00 -88.30   26
 26  \w    112.00 139.00   1.00   10.00    --   78.00  62.00 -91.50   27
 27  \w     49.00  74.00   1.00   10.00    --   78.00  62.00 -91.50   25
 28  \w     49.00  83.00   1.00   10.00    --   78.00  68.00  29.13   34
 29  \w     48.00  74.00   1.00   10.00    --   78.00  66.00-128.10   26
 30  \w     50.00  75.00   1.00   10.00    --   82.00  73.00  78.74   25
 31  \w     53.00  78.00   1.00   10.00    --   82.00  66.00 117.98   25
 32  \w     55.00  80.00   1.00   10.00    --   86.00  69.00 132.39   25
 33  \w     59.00  86.00   1.00   10.00    --   90.00  71.00 174.54   27
 34  \w     61.00  99.00   1.00   10.00    --   90.00  72.00 -43.35   38
 35  \w    119.00 145.00   1.00   10.00    --   90.00  74.00 146.13   26
 36  \w     58.00  88.00   1.00   10.00    --   90.00  74.00 146.13   30
 37  \w    141.00 167.00   1.00   10.00    --   94.00  67.00 -63.31   26
 38  \w     64.00 100.00   1.00   10.00    --   94.00  67.00 -63.31   36
 39  \w     69.00  94.00   1.00   10.00    --   94.00  48.00-133.13   25
 40  \w     82.00 168.00   1.00   10.00    --  104.49  53.00 -32.75   86
 41  \w     77.00 151.00   1.00   10.00    --  104.49  61.00  60.00   74
 42  \w     37.00 107.00   1.00   10.00    --  104.49-102.00 170.89   70
 43  \w    114.00 178.00   1.00   10.00    --  104.49  72.00-147.71   64
 44  \w     75.00 158.00   1.00   10.00    --  104.49  61.00-180.00   83
 45  \w     74.00 100.00   1.00   10.00    --  104.49  72.00-147.71   26
 46  \w     44.00 106.00   1.00   10.00    --  104.49-125.00 150.00   62
 47  \w    113.00 164.00   1.00   10.00    --  104.49  61.00   0.00   51
 48  \w     75.00 101.00   1.00   10.00    --  104.49  61.00   0.00   26
 49  \w     76.00 166.00   1.00   10.00    --  104.49  61.00 -90.00   90
 50  \w    121.00 158.00   1.00   10.00    --  104.49 125.00  90.00   37
 51  \w     75.00 105.00   1.00   10.00    --  104.49 -94.00-150.00   30
 52  \w     34.00  70.00   1.00   10.00    --  104.49 -94.00-150.00   36
 53  \w    134.00 171.00   1.00   10.00    --  104.49  61.00  30.00   37
 54  \w     75.00 119.00   1.00   10.00    --  104.49  61.00  30.00   44
 55  \w     29.00  71.00   1.00   10.00    --  104.49 -94.00  60.00   42
 56  \w    126.00 159.00   1.00   10.00    --  104.49 125.00   0.00   33
 57  \w     77.00 108.00   1.00   10.00    --  104.49  61.00-120.00   31
 58  \w     75.00 175.00   1.00   10.00    --  104.49  61.00 120.00  100
 59  \w     22.00 106.00   1.00   10.00    --  104.49 -94.00  30.00   84
 60  \w     75.00 154.00   1.00   10.00    --  104.49  61.00  90.00   79
 61  \w     23.00 105.00   1.00   10.00    --  104.49 -94.00 -60.00   82
;
_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      -0.0257207000
_diffrn_orient_matrix_UB_12      0.0436661000
_diffrn_orient_matrix_UB_13      -0.0460876000
_diffrn_orient_matrix_UB_21      -0.1229643000
_diffrn_orient_matrix_UB_22      -0.0602835000
_diffrn_orient_matrix_UB_23      -0.0001526000
_diffrn_orient_matrix_UB_31      0.0009623000
_diffrn_orient_matrix_UB_32      0.1004429000
_diffrn_orient_matrix_UB_33      0.0309634000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            79427
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.773
_diffrn_reflns_theta_min         3.587
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.057
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene/hexane'
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1182
_refine_ls_number_reflns         18287
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0529P)^2^+1.8474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16638
_reflns_number_total             18287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02523b2.cif
_cod_data_source_block           xstr
_cod_depositor_comments
'Adding full bibliography for 7705030--7705034.cif.'
_cod_original_cell_volume        4684.98(13)
_cod_database_code               7705031
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C106 H104 N4 Mg2'
_chemical_oxdiff_usercomment     CB-125
_reflns_odcompleteness_completeness 99.95
_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. Uiso/Uaniso restraints and constraints
O7AA \\sim HD \\sim HE \\sim OF: within 1A with sigma of 0.001 and sigma for
terminal atoms of 0.001
3. Others
 Sof(O7AA)=Sof(OF)=1-FVAR(1)
 Sof(HD)=Sof(HE)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C016(H016), C01G(H01G), C01H(H01H), C01I(H01I), C01N(H01N), C01P(H01P),
 C01T(H01T), C01V(H01V), C01Y(H01Y), C01Z(H01Z), C021(H021), C022(H022),
 C026(H026), C027(H027), C028(H028), C02A(H02A), C02B(H02B), C02G(H02K),
 C02J(H02N), C02K(H02O), C02M(H02Q), C02O(H02U), C02P(H02V), C02T(H0AA),
 C02U(H1AA), C02V(H2AA), C02X(H4AA), C02Y(H5AA), C02Z(H6AA), C030(H030)
4.b Idealised Me refined as rotating group:
 C01M(H01A,H01B,H01E), C01S(H01M,H01Q,H01S), C02D(H02D,H02E,H02F), C02F(H02H,
 H02I,H02J), C02N(H02R,H02S,H02T), C02Q(H02W,H02X,H02Y), C02R(H02Z,H,HA),
 C02W(H3AA,HB,HC), C031(H03A,H03B,H03C), C032(H03D,H03E,H03F), C033(H03G,H03H,
 H03I), C034(H03J,H03K,H03L)
;
_shelx_res_checksum              24193
_shelx_fab_checksum              4594
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.561
_oxdiff_exptl_absorpt_empirical_full_min 0.772