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_7048865
_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         'C44 H65 Mg N3 O2'
_chemical_formula_sum            'C44 H65 Mg N3 O2'
_chemical_formula_weight         692.30
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2018-10-18 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                100.865(2)
_cell_angle_beta                 95.075(2)
_cell_angle_gamma                101.435(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9221(2)
_cell_length_b                   10.1350(2)
_cell_length_c                   23.6908(5)
_cell_measurement_reflns_used    19544
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.8440
_cell_measurement_theta_min      4.5460
_cell_volume                     2044.39(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_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    -66.00  34.00   1.00    1.00    --  -37.03  19.00-120.00  100
  2  \w   -106.00 -18.00   1.00    1.00    --  -37.03 -38.00 -30.00   88
  3  \w   -107.00  -8.00   1.00    1.00    --  -37.03 -19.00 -60.00   99
  4  \w     24.00  91.00   1.00    1.00    --   37.03-126.00-180.00   67
  5  \w    -30.00  54.00   1.00    1.00    --   37.03 -57.00-180.00   84
  6  \w     24.00  91.00   1.00    1.00    --   37.03-126.00 120.00   67
  7  \w    -32.00 106.00   1.00    1.00    --   37.03   0.00   0.00  138
  8  \w     24.00  91.00   1.00    1.00    --   37.03-126.00 -60.00   67
  9  \w      1.00  76.00   1.00    1.00    --   37.03 -99.00  60.00   75
 10  \w     24.00  91.00   1.00    1.00    --   37.03-126.00-120.00   67
 11  \w     18.00 106.00   1.00    1.00    --   37.03  38.00 -30.00   88
 12  \w     24.00  91.00   1.00    1.00    --   37.03-126.00 -30.00   67
 13  \w    -30.00  54.00   1.00    1.00    --   37.03 -57.00 -60.00   84
 14  \w     41.00 109.00   1.00    2.00    --  110.47 -95.00 120.00   68
 15  \w     57.00 151.00   1.00    2.00    --  110.47 178.00  90.00   94
 16  \w     44.00 129.00   1.00    2.00    --  110.47 -61.00 120.00   85
 17  \w     42.00 128.00   1.00    2.00    --  110.47 -45.00  60.00   86
 18  \w     44.00 129.00   1.00    2.00    --  110.47 -61.00   0.00   85
 19  \w    101.00 178.00   1.00    2.00    --  110.47 112.00  30.00   77
 20  \w     57.00 151.00   1.00    2.00    --  110.47 178.00  60.00   94
 21  \w     42.00 128.00   1.00    2.00    --  110.47 -45.00 -30.00   86
 22  \w     89.00 178.00   1.00    2.00    --  110.47  30.00 -60.00   89
 23  \w     41.00 132.00   1.00    2.00    --  110.47 -30.00 -30.00   91
 24  \w     41.00 116.00   1.00    2.00    --  110.47-112.00  30.00   75
 25  \w     42.00 128.00   1.00    2.00    --  110.47 -45.00-120.00   86
 26  \w     41.00 109.00   1.00    2.00    --  110.47 -95.00-150.00   68
 27  \w     40.00 149.00   1.00    2.00    --  110.47 -15.00  90.00  109
 28  \w   -106.00 -18.00   1.00    1.00    --  -37.03 -38.00-150.00   88
 29  \w    -54.00  30.00   1.00    1.00    --  -37.03  57.00  30.00   84
 30  \w   -104.00 -20.00   1.00    1.00    --  -37.03 -57.00-180.00   84
 31  \w   -104.00 -20.00   1.00    1.00    --  -37.03 -57.00  90.00   84
 32  \w   -105.00 -10.00   1.00    1.00    --  -37.03 -77.00 -90.00   95
 33  \w    -30.00  54.00   1.00    1.00    --   37.03 -57.00-150.00   84
 34  \w     20.00 104.00   1.00    1.00    --   37.03  57.00-120.00   84
 35  \w     10.00 105.00   1.00    1.00    --   37.03  77.00  60.00   95
 36  \w     10.00 105.00   1.00    1.00    --   37.03  77.00  30.00   95
 37  \w     10.00 105.00   1.00    1.00    --   37.03  77.00 150.00   95
 38  \w     10.00 105.00   1.00    1.00    --   37.03  77.00-150.00   95
 39  \w     10.00 105.00   1.00    1.00    --   37.03  77.00 -30.00   95
 40  \w     72.00 178.00   1.00    2.00    --  110.47  15.00 150.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0452802000
_diffrn_orient_matrix_UB_12      0.1534751000
_diffrn_orient_matrix_UB_13      -0.0023528000
_diffrn_orient_matrix_UB_21      -0.0091579000
_diffrn_orient_matrix_UB_22      0.0401439000
_diffrn_orient_matrix_UB_23      0.0654372000
_diffrn_orient_matrix_UB_31      0.1715788000
_diffrn_orient_matrix_UB_32      -0.0022611000
_diffrn_orient_matrix_UB_33      0.0131550000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30124
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.974
_diffrn_reflns_theta_min         3.833
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         8024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0710P)^2^+0.5520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7334
_reflns_number_total             8024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00090a2.cif
_cod_data_source_block           rws0319
_cod_depositor_comments
'Adding full bibliography for 7048864--7048869.cif.'
_cod_database_code               7048865
_chemical_oxdiff_formula         'C1 H1 N1 Mg1 O1'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C38(H38), C31(H31), C21(H21), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C00M(H00A,H00B), C00U(H00F,H00G), C9(H9A,H9B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C34(H34), C36(H36), C19(H19), C8(H8), C17(H17), C35(H35), C7(H7),
 C18(H18), C3(H3), C6(H6), C5(H5), C4(H4)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C00P(H00C,H00D,H00E), C39(H39A,H39B,H39C), C25(H25A,H25B,
 H25C), C40(H40A,H40B,H40C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C16(H16A,
 H16B,H16C), C23(H23A,H23B,H23C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C),
 C22(H22A,H22B,H22C), C01E(H01A,H01B,H01C)
;
_shelx_shelxl_version_number     2017/1
_olex2_date_sample_data_collection 2018-03-19
_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 2.906
_oxdiff_exptl_absorpt_empirical_full_min 0.594