Reactivity of a β-diketiminate-supported magnesium alkyl complex toward small molecules.
Ren, Wenshan; Zhang, Shaohui; Xu, Ziyi; Ma, Xuebing; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3109–3115; doi:10.1039/c9dt00090a

data_7048869
_publ_section_title
;
 Reactivity of a \b-diketiminate-supported magnesium alkyl complex toward
 small molecules.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3109
_journal_page_last               3115
_journal_paper_doi               10.1039/c9dt00090a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(C33 H46 Mg N4), C7 H8'
_chemical_formula_sum            'C73 H100 Mg2 N8'
_chemical_formula_weight         1138.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.23 svn.r2946 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2018-10-18 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                72.837(3)
_cell_angle_beta                 75.308(3)
_cell_angle_gamma                63.308(4)
_cell_formula_units_Z            2
_cell_length_a                   13.3001(5)
_cell_length_b                   14.3346(5)
_cell_length_c                   21.0947(8)
_cell_measurement_reflns_used    30256
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.5430
_cell_measurement_theta_min      3.8800
_cell_volume                     3398.4(2)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega   57.00  109.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  178.0000   30.0000 52

  2 omega  -32.00   56.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -38.0000  120.0000 88

  3 omega    3.00   32.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   90.0000  146.8663 29

  4 omega   10.00  105.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   77.0000  -90.0000 95

  5 omega    1.00   76.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -99.0000 -180.0000 75

  6 omega   57.00  109.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  178.0000  120.0000 52

  7 omega    1.00   76.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -99.0000   90.0000 75

  8 omega   20.00  104.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000  120.0000 84

  9 omega   20.00  104.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000   30.0000 84

 10 omega   20.00  104.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000 -120.0000 84

 11 omega    2.00   29.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   91.0000  -48.9382 27

 12 omega    8.00  108.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   19.0000  120.0000 100

 13 omega   38.00   91.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

 14 omega   39.00  110.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -150.0000 71

 15 omega   91.00  176.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 85

 16 omega   39.00  110.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  -30.0000 71

 17 omega   57.00  150.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 93

 18 omega   39.00  110.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000 -120.0000 71

 19 omega   39.00  110.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   90.0000 71

 20 omega   91.00  176.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   60.0000 85

 21 omega   38.00   91.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

 22 omega   38.00  116.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000 -180.0000 78

 23 omega   38.00   91.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 24 omega   40.00   98.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 58

 25 omega   38.00  116.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -112.0000   60.0000 78

 26 omega   40.00   98.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 58

 27 omega   38.00   91.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 28 omega   40.00   98.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 58

 29 omega   40.00   98.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000    0.0000 58

 30 omega   70.00  178.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000    0.0000 108

 31 omega   57.00  109.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  178.0000  -30.0000 52

 32 omega   10.00  105.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   77.0000   60.0000 95

 33 omega  -32.00   56.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -38.0000   30.0000 88

 34 omega   20.00  104.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000 -150.0000 84

 35 omega  -30.00   54.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -57.0000  -30.0000 84

 36 omega   20.00  104.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000  -30.0000 84

 37 omega    2.00   28.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   92.0000   -9.6288 26

 38 omega   20.00  104.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   57.0000  150.0000 84

 39 omega   10.00  105.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   77.0000  150.0000 95

 40 omega   18.00  106.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   38.0000 -150.0000 88

 41 omega   10.00  105.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703   77.0000 -120.0000 95

 42 omega  -31.00   64.00   1.0000    1.3300
omega____ theta____ kappa____ phi______ frames
    -       36.9703  -77.0000  -90.0000 95

 43 omega   81.00  176.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 95

 44 omega   87.00  178.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -90.0000 91

 45 omega   70.00  178.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  150.0000 108

 46 omega   90.00  175.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 85

 47 omega   81.00  176.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

 48 omega   81.00  176.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 95

 49 omega   81.00  176.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 95

 50 omega   81.00  176.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 95

 51 omega   81.00  176.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95

 52 omega   81.00  176.00   1.0000    5.3100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0950127000
_diffrn_orient_matrix_UB_12      -0.0621152000
_diffrn_orient_matrix_UB_13      -0.0500909000
_diffrn_orient_matrix_UB_21      -0.0101973000
_diffrn_orient_matrix_UB_22      0.1060685000
_diffrn_orient_matrix_UB_23      -0.0496229000
_diffrn_orient_matrix_UB_31      0.0895651000
_diffrn_orient_matrix_UB_32      0.0051040000
_diffrn_orient_matrix_UB_33      0.0314745000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62621
_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         71.876
_diffrn_reflns_theta_min         4.083
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         13121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0580P)^2^+1.0890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11966
_reflns_number_total             13121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00090a2.cif
_cod_data_source_block           rwsh20160506
_cod_depositor_comments
'Adding full bibliography for 7048864--7048869.cif.'
_cod_database_code               7048869
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C1 N1 H1 Mg1'
_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:
 C24(H24), C7(H7), C40(H40), C31(H31), C14(H14), C64(H64), C57(H57), C47(H47)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C36(H36), C19(H19), C37(H37), C52(H52), C12(H12), C29(H29),
 C45(H45), C27(H27), C10(H10), C43(H43), C62(H62), C28(H28), C11(H11), C60(H60),
  C44(H44), C61(H61), C69(H69), C73(H73), C70(H70), C71(H71), C72(H72)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C21(H21A,H21B,H21C), C35(H35A,H35B,H35C), C54(H54A,H54B,
 H54C), C9(H9A,H9B,H9C), C51(H51A,H51B,H51C), C18(H18A,H18B,H18C), C32(H32A,
 H32B,H32C), C66(H66A,H66B,H66C), C41(H41A,H41B,H41C), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C16(H16A,H16B,H16C), C65(H65A,H65B,H65C), C42(H42A,H42B,
 H42C), C33(H33A,H33B,H33C), C15(H15A,H15B,H15C), C49(H49A,H49B,H49C), C8(H8A,
 H8B,H8C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C67(H67A,H67B,H67C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              21205
_olex2_submission_special_instructions 'No special instructions were received'