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_7705030
_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         'C148 H123.52 Mg2 N4 O0.48'
_chemical_formula_sum            'C168 H145 Mg2 N5 O0.25'
_chemical_formula_weight         2286.50
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 111.7680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3074(3)
_cell_length_b                   23.7367(2)
_cell_length_c                   24.8704(3)
_cell_measurement_reflns_used    29272
_cell_measurement_temperature    154.4(8)
_cell_measurement_theta_max      72.5770
_cell_measurement_theta_min      4.1420
_cell_volume                     12778.2(3)
_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      154.4(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -62.00 -11.00   1.00   10.00    --  -42.62  77.00-120.00   51
  2  \w    -85.00 -47.00   1.00   10.00    --  -42.62 125.00 -30.00   38
  3  \w   -111.00 -18.00   1.00   10.00    --  -42.62 -38.00   0.00   93
  4  \w     -7.00  30.00   1.00   10.00    --  -42.62  77.00-120.00   37
  5  \w   -116.00 -22.00   1.00   10.00    --  -42.62 -57.00 120.00   94
  6  \w     27.00  53.00   1.00   10.00    --   42.62-125.00 -30.00   26
  7  \w     39.00 113.00   1.00   30.00    --  104.49-125.00-120.00   74
  8  \w     36.00  70.00   1.00   30.00    --  104.49 -95.00  90.00   34
  9  \w     29.00  65.00   1.00   30.00    --  104.49 -77.00 150.00   36
 10  \w     41.00 113.00   1.00   30.00    --  104.49-125.00   0.00   72
 11  \w    106.00 150.00   1.00   30.00    --  104.49  77.00-150.00   44
 12  \w     36.00  95.00   1.00   30.00    --  104.49 -45.00-150.00   59
 13  \w    103.00 178.00   1.00   30.00    --  104.49  77.00   0.00   75
 14  \w     33.00 130.00   1.00   30.00    --  104.49 -45.00 -60.00   97
 15  \w    107.00 166.00   1.00   30.00    --  104.49  77.00-120.00   59
 16  \w     83.00 178.00   1.00   30.00    --  104.49  30.00 -30.00   95
 17  \w     41.00 126.00   1.00   30.00    --  104.49-143.00-168.98   85
 18  \w     69.00 113.00   1.00   30.00    --  104.49-125.00 -60.00   44
 19  \w     65.00 108.00   1.00   30.00    --  104.49-106.00  42.01   43
;
_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      -0.0400499000
_diffrn_orient_matrix_UB_12      0.0041164000
_diffrn_orient_matrix_UB_13      0.0371458000
_diffrn_orient_matrix_UB_21      0.0419809000
_diffrn_orient_matrix_UB_22      0.0473228000
_diffrn_orient_matrix_UB_23      0.0361180000
_diffrn_orient_matrix_UB_31      -0.0412278000
_diffrn_orient_matrix_UB_32      0.0441909000
_diffrn_orient_matrix_UB_33      -0.0420466000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            92563
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.790
_diffrn_reflns_theta_min         3.724
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.673
_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    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             4856
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1452
_refine_ls_number_reflns         25118
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0686P)^2^+5.0648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19811
_reflns_number_total             25118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02523b2.cif
_cod_data_source_block           xstr1089
_cod_depositor_comments
'Adding full bibliography for 7705030--7705034.cif.'
_cod_database_code               7705030
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C162 H140 N4 Mg2'
_chemical_oxdiff_usercomment     CB-145
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.904
_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
HA \\sim OB \\sim O0AA \\sim H: within 1A with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Others
 Sof(O0AA)=Sof(OB)=1-FVAR(1)
 Sof(H)=Sof(HA)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C40(H40), C110(H110), C114(H114), C118(H118), C77(H77), C79(H79), C36(H36),
 C44(H44), C120(H120), C106(H106), C107(H107), C39(H39), C5(H5), C55(H55),
 C61(H61), C105(H105), C27(H27), C46(H46), C3(H3), C103(H103), C125(H125),
 C94(H94), C111(H111), C131(H131), C37(H37), C23(H23), C97(H97), C104(H104),
 C129(H129), C57(H57), C113(H113), C10(H10), C60(H60), C29(H29), C54(H54),
 C26(H26), C14(H14), C101(H101), C59(H59), C135(H135), C64(H64), C33(H33),
 C148(H148), C51(H51), C58(H58), C24(H24), C84(H84), C128(H128), C16(H16),
 C70(H70), C98(H98), C68(H68), C133(H133), C126(H126), C20(H20), C132(H132),
 C25(H25), C18(H18), C127(H127), C74(H74), C19(H19), C134(H134), C142(H142),
 C88(H88), C90(H90), C32(H32), C52(H52), C53(H53), C12(H12), C93(H93),
 C100(H100), C31(H31), C13(H13), C30(H30), C11(H11), C65(H65), C17(H17),
 C99(H99), C71(H71), C147(H147), C67(H67), C87(H87), C92(H92), C144(H144),
 C86(H86), C66(H66), C85(H85), C73(H73), C138(H138), C72(H72), C91(H91),
 C141(H141), C140(H140), C139(H139), C146(H146), C145(H145)
4.b Idealised Me refined as rotating group:
 C122(H12A,H12B,H12C), C81(H81A,H81B,H81C), C7(H7A,H7B,H7C), C41(H41A,H41B,
 H41C), C48(H48A,H48B,H48C), C115(H11A,H11B,H11C)
;
_shelx_res_checksum              3176
_shelx_fab_checksum              39125
_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 2.098
_oxdiff_exptl_absorpt_empirical_full_min 0.599