Mg-Mg bond polarization induced by a superbulky β-diketiminate ligand.
Rösch, Bastian; Gentner, Thomas Xaver; Eyselein, Jonathan; Friedrich, Alexander; Langer, Jens; Harder, Sjoerd; Chemical communications (Cambridge, England) 56 (2020) 11402–11405; doi:10.1039/d0cc05200k

data_7127086
_publ_section_title
;
 Mg-Mg bond polarization induced by a superbulky \b-diketiminate ligand.
;
_journal_issue                   77
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11402
_journal_page_last               11405
_journal_paper_doi               10.1039/d0cc05200k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '1(C21 H35 N O)'
_chemical_formula_sum            'C21 H35 N O'
_chemical_formula_weight         317.50
_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             2020-07-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2020-07-30 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.387(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.9088(3)
_cell_length_b                   20.8368(11)
_cell_length_c                   19.7657(10)
_cell_measurement_reflns_used    5824
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      72.0650
_cell_measurement_theta_min      4.7120
_cell_volume                     4037.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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   -116.00 -17.00   1.00    4.00    --  -41.48 -38.00 -90.00   99
  2  \w    -87.00 -10.00   1.00    4.00    --  -41.48 125.00  60.00   77
  3  \w    103.00 167.00   1.00   16.00    --  104.33  77.00  30.00   64
  4  \w     31.00 114.00   1.00   16.00    --  104.33 -45.00 -60.00   83
  5  \w     23.00  49.00   1.00   16.00    --  104.33 -94.00 -30.00   26
  6  \w     36.00 131.00   1.00   16.00    --  104.33 -77.00 -90.00   95
  7  \w     32.00 163.00   1.00   16.00    --  104.33   0.00-150.00  131
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0015040000
_diffrn_orient_matrix_UB_12      -0.0643975000
_diffrn_orient_matrix_UB_13      0.0380249000
_diffrn_orient_matrix_UB_21      0.1113390000
_diffrn_orient_matrix_UB_22      0.0251217000
_diffrn_orient_matrix_UB_23      0.0562757000
_diffrn_orient_matrix_UB_31      -0.1106339000
_diffrn_orient_matrix_UB_32      0.0263963000
_diffrn_orient_matrix_UB_33      0.0399608000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14248
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.816
_diffrn_reflns_theta_min         3.099
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00075(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         7787
_refine_ls_number_restraints     1943
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+5.4735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6687
_reflns_number_total             7787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05200k2.cif
_cod_data_source_block           hasj200604b
_cod_depositor_comments
'Adding full bibliography for 7127086--7127091.cif.'
_cod_database_code               7127086
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C42H70N2O2
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.824
_reflns_odcompleteness_completeness 99.60
_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. Restrained distances
 N2-C27A \\sim N2-C27
 with sigma of 0.02
 C37A-C36A \\sim C37-C36 \\sim C35A-C34A \\sim C35-C34 \\sim C39A-C40A \\sim
C40-C39 \\sim C42-C41 ~
 C42A-C41A
 with sigma of 0.02
 C32-C38 \\sim C32A-C38A \\sim C33-C28 \\sim C28A-C33A
 with sigma of 0.02
 C38A-C41A \\sim C41-C38 \\sim C39-C38 \\sim C39A-C38A \\sim C36A-C33A \\sim
C36-C33 \\sim C34A-C33A ~
 C34-C33
 with sigma of 0.02
 C26A-C24A \\sim C24A-C25A \\sim C25A-C26A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A \\sim C23-C25 \\sim C23A-C25A \\sim C23A-C26A \\sim
C23-C26
 with sigma of 0.02
 C22-C23 \\sim C22-C23A
 with sigma of 0.02
 C4A-C5A \\sim C5A-C3A \\sim C4A-C3A \\sim C3-C4 \\sim C4-C5 \\sim C3-C5
 with sigma of 0.02
 C3A-C2A \\sim C3-C2 \\sim C4A-C2A \\sim C4-C2 \\sim C5-C2 \\sim C5A-C2A
 with sigma of 0.02
 C28-C27 \\sim C28A-C27A \\sim C32-C27 \\sim C32A-C27A
 with sigma of 0.02
 C30-C29 \\sim C30A-C29A \\sim C31A-C30A \\sim C31-C30
 with sigma of 0.02
 C32A-C31A \\sim C32-C31 \\sim C29A-C28A \\sim C29-C28
 with sigma of 0.02
 C31A-C27A \\sim C27A-C29A
 with sigma of 0.02
 C32A-C30A \\sim C30A-C28A
 with sigma of 0.02
 C29A-C31A \\sim C28A-C32A
 with sigma of 0.02
 C27A-C30A \\sim C27-C30
 with sigma of 0.02
3. Restrained planarity
 C28A, C29A, C30A, C27A, C32A, C31A
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim
C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim
C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim C33A \\sim
C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A \\sim
C42A: within 4A with sigma of 0.02 and sigma for terminal atoms of 0.04 within
4A
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C24A \\sim C25A \\sim C26A: within 4A
with sigma of 0.02 and sigma for terminal atoms of 0.03 within 4A
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C2A \\sim C3A \\sim C4A \\sim C5A: within
4A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
C32 \\sim C38 \\sim C32A \\sim C38A: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 3A
5. Rigid body (RIGU) restrains
 C32A, C38A, C39A, C41A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C22, C23A, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C32A)=Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(H30A)=Sof(C29A)=Sof(H29A)=
 Sof(C28A)=Sof(C27A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34c)=Sof(H34d)=
 Sof(C35A)=Sof(H35d)=Sof(H35e)=Sof(H35f)=Sof(C36A)=Sof(H36c)=Sof(H36d)=
 Sof(C37A)=Sof(H37d)=Sof(H37e)=Sof(H37f)=Sof(C38A)=Sof(H38A)=Sof(C39A)=
 Sof(H39c)=Sof(H39d)=Sof(C40A)=Sof(H40d)=Sof(H40e)=Sof(H40f)=Sof(C41A)=
 Sof(H41c)=Sof(H41d)=Sof(C42A)=Sof(H42d)=Sof(H42e)=Sof(H42f)=1-FVAR(1)
 Sof(C27)=Sof(C28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=
 Sof(C32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=FVAR(1)
 Sof(C23A)=Sof(C24A)=Sof(H24d)=Sof(H24e)=Sof(H24f)=Sof(C25A)=Sof(H25d)=
 Sof(H25e)=Sof(H25f)=Sof(C26A)=Sof(H26d)=Sof(H26e)=Sof(H26f)=1-FVAR(2)
 Sof(C23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(2)
 Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=1-FVAR(3)
 Sof(C2A)=Sof(C3A)=Sof(H3Aa)=Sof(H3Ab)=Sof(H3Ac)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=
 Sof(H4Ac)=Sof(C5A)=Sof(H5Aa)=Sof(H5Ab)=Sof(H5Ac)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C12(H12), C17(H17), C33(H33), C38(H38), C33A(H33A), C38A(H38A)
7.b Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C15(H15a,H15b), C18(H18a,H18b), C20(H20a,H20b), C34(H34A,
 H34B), C36(H36A,H36B), C39(H39A,H39B), C41(H41A,H41B), C34A(H34c,H34d),
 C36A(H36c,H36d), C39A(H39c,H39d), C41A(H41c,H41d)
7.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C29(H29), C30(H30), C31(H31), C31A(H31A),
 C30A(H30A), C29A(H29A)
7.d Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C16(H16a,H16b,H16c), C19(H19a,H19b,H19c), C21(H21a,H21b,
 H21c), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3A(H3Aa,H3Ab,H3Ac),
 C4A(H4Aa,H4Ab,H4Ac), C5A(H5Aa,H5Ab,H5Ac), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C40(H40A,
 H40B,H40C), C42(H42A,H42B,H42C), C24A(H24d,H24e,H24f), C25A(H25d,H25e,H25f),
 C26A(H26d,H26e,H26f), C35A(H35d,H35e,H35f), C37A(H37d,H37e,H37f), C40A(H40d,
 H40e,H40f), C42A(H42d,H42e,H42f)
;
_olex2_date_sample_data_collection 2020-06-04
_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 1.909
_oxdiff_exptl_absorpt_empirical_full_min 0.530