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_7705034
_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         'C122 H112 Mg2 N4, 2(C6 H6)'
_chemical_formula_sum            'C134 H124 Mg2 N4'
_chemical_formula_weight         1838.98
_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     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                88.579(2)
_cell_angle_beta                 74.671(2)
_cell_angle_gamma                79.266(2)
_cell_formula_units_Z            2
_cell_length_a                   15.3790(4)
_cell_length_b                   17.8137(5)
_cell_length_c                   23.3393(5)
_cell_measurement_reflns_used    22213
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.4650
_cell_measurement_theta_min      3.9060
_cell_volume                     6056.6(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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.969
_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    -87.00  -7.00   1.00    7.50    --  -42.75 125.00  60.00   80
  2  \w   -115.00 -20.00   1.00    7.50    --  -42.75 -38.00-180.00   95
  3  \w   -108.00 -57.00   1.00    7.50    --  -42.75 -38.00  30.00   51
  4  \w   -110.00 -83.00   1.00    7.50    --  -42.75 -38.00 -90.00   27
  5  \w   -107.00 -15.00   1.00    7.50    --  -42.75 -57.00 -60.00   92
  6  \w     87.00 114.00   1.00   30.00    --  104.49 -77.00 -30.00   27
  7  \w     45.00  92.00   1.00   30.00    --  104.49 -45.00 -90.00   47
  8  \w     88.00 115.00   1.00   30.00    --  104.49 -77.00 120.00   27
  9  \w     66.00 113.00   1.00   30.00    --  104.49-125.00 -60.00   47
 10  \w     72.00 113.00   1.00   30.00    --  104.49-125.00 150.00   41
 11  \w     35.00 124.00   1.00   30.00    --  104.49 -45.00 120.00   89
 12  \w     43.00 121.00   1.00   30.00    --  104.49 -45.00  30.00   78
 13  \w     69.00 113.00   1.00   30.00    --  104.49-125.00-150.00   44
 14  \w    105.00 178.00   1.00   30.00    --  104.49  77.00-180.00   73
 15  \w    146.00 176.00   1.00   30.00    --  104.49  77.00  30.00   30
 16  \w     37.00 113.00   1.00   30.00    --  104.49-125.00  60.00   76
 17  \w     17.00 170.00   1.00   30.00    --  104.49   0.00-180.00  153
 18  \w     24.00 107.00   1.00   30.00    --  104.49 -98.00 -42.12   83
;
_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      0.0650211000
_diffrn_orient_matrix_UB_12      -0.0239287000
_diffrn_orient_matrix_UB_13      0.0400918000
_diffrn_orient_matrix_UB_21      -0.0490132000
_diffrn_orient_matrix_UB_22      -0.0672579000
_diffrn_orient_matrix_UB_23      0.0223546000
_diffrn_orient_matrix_UB_31      0.0674309000
_diffrn_orient_matrix_UB_32      -0.0515448000
_diffrn_orient_matrix_UB_33      -0.0507972000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45049
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.749
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.645
_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    1.008
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1273
_refine_ls_number_reflns         23357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+1.1642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19471
_reflns_number_total             23357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02523b2.cif
_cod_data_source_block           xstr1177
_cod_depositor_comments
'Adding full bibliography for 7705030--7705034.cif.'
_cod_database_code               7705034
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mg2 C122 H106 N4'
_chemical_oxdiff_usercomment     'CB-219 B'
_reflns_odcompleteness_completeness 99.79
_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.a Ternary CH refined with riding coordinates:
 C41(H41), C110(H110), C28(H28), C97(H97), C7(H7), C79(H79), C10(H10), C76(H76)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C19(H19), C15(H15), C23(H23), C16(H16), C92(H92), C18(H18),
 C36(H36), C94(H94), C84(H84), C88(H88), C40(H40), C34(H34), C47(H47), C30(H30),
  C43(H43), C32(H32), C105(H105), C33(H33), C31(H31), C37(H37), C39(H39),
 C116(H116), C38(H38), C3(H3), C122(H122), C46(H46), C87(H87), C74(H74), C5(H5),
  C118(H118), C53(H53), C112(H112), C44(H44), C85(H85), C4(H4), C106(H106),
 C73(H73), C45(H45), C115(H115), C72(H72), C49(H49), C109(H109), C114(H114),
 C69(H69), C65(H65), C107(H107), C113(H113), C119(H119), C61(H61), C108(H108),
 C121(H121), C120(H120), C52(H52), C57(H57), C51(H51), C50(H50), C103(H103),
 C99(H99), C60(H60), C66(H66), C68(H68), C127(H127), C126(H126), C128(H128),
 C134(H134), C67(H67), C59(H59), C129(H129), C58(H58), C133(H133), C125(H125),
 C102(H102), C100(H100), C123(H123), C130(H130), C101(H101), C124(H124),
 C132(H132), C131(H131)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C20(H20A,H20B,H20C), C96(H96A,H96B,H96C), C8(H8A,H8B,
 H8C), C80(H80A,H80B,H80C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C11(H11A,H11B,
 H11C), C81(H81A,H81B,H81C), C78(H78A,H78B,H78C), C77(H77A,H77B,H77C), C89(H89A,
 H89B,H89C)
;
_shelx_res_checksum              79013
_shelx_fab_checksum              7524
_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 1.394
_oxdiff_exptl_absorpt_empirical_full_min 0.800