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_7127090
_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         'C46.788 H77.577 Mg N2'
_chemical_formula_sum            'C46.79 H77.58 Mg N2'
_chemical_formula_weight         692.47
_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             2020-07-30
_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                97.526(2)
_cell_angle_beta                 99.465(2)
_cell_angle_gamma                105.672(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1571(4)
_cell_length_b                   10.6195(3)
_cell_length_c                   21.6789(5)
_cell_measurement_reflns_used    8278
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.7590
_cell_measurement_theta_min      4.1880
_cell_volume                     2182.57(12)
_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 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  (Sheldrick, 2015)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.962
_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   -108.00 -19.00   1.00    1.00    --  -41.39 -57.00 -30.00   89
  2  \w    -69.00  32.00   1.00    1.00    --  -41.39  57.00 120.00  101
  3  \w    -91.00 -54.00   1.00    1.00    --  -41.39 125.00-180.00   37
  4  \w    -64.00  33.00   1.00    1.00    --  -41.39  38.00 -90.00   97
  5  \w     37.00 117.00   1.00    3.00    --  106.30-125.00-120.00   80
  6  \w     60.00 171.00   1.00    3.00    --  106.30  15.00 -90.00  111
  7  \w     99.00 173.00   1.00    3.00    --  106.30 125.00  90.00   74
  8  \w     24.00 109.00   1.00    3.00    --  106.30 -94.00  30.00   85
  9  \w     43.00 134.00   1.00    3.00    --  106.30 -61.00  60.00   91
 10  \w     82.00 166.00   1.00    3.00    --  106.30  45.00 150.00   84
 11  \w     33.00 115.00   1.00    3.00    --  106.30-125.00 -30.00   82
 12  \w    119.00 173.00   1.00    3.00    --  106.30 125.00   0.00   54
 13  \w     43.00 115.00   1.00    3.00    --  106.30 -30.00 -30.00   72
;
_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      -0.0479736000
_diffrn_orient_matrix_UB_12      0.0983702000
_diffrn_orient_matrix_UB_13      -0.0379360000
_diffrn_orient_matrix_UB_21      -0.1537743000
_diffrn_orient_matrix_UB_22      -0.0773084000
_diffrn_orient_matrix_UB_23      -0.0033338000
_diffrn_orient_matrix_UB_31      0.0022285000
_diffrn_orient_matrix_UB_32      0.0886010000
_diffrn_orient_matrix_UB_33      0.0626362000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14348
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.664
_diffrn_reflns_theta_min         4.207
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.382
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_description       block
_exptl_crystal_F_000             769
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.328
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         8484
_refine_ls_number_restraints     688
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0435P)^2^+0.6750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7684
_reflns_number_total             8484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05200k2.cif
_cod_data_source_block           hasj190708a
_cod_depositor_comments
'Adding full bibliography for 7127086--7127091.cif.'
_cod_database_code               7127090
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C46.8 H77.6 Mg N2'
_reflns_odcompleteness_completeness 99.56
_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
 C33A-C28 \\sim C33-C28 \\sim C32-C33 \\sim C32A-C33A \\sim C31-C32A \\sim
C31-C32
 with sigma of 0.02
 C36-C35 \\sim C36A-C35A \\sim C38-C37 \\sim C38A-C37A
 with sigma of 0.02
 C37-C34 \\sim C37A-C34A \\sim C35-C34 \\sim C34A-C35A
 with sigma of 0.02
 C34-C33 \\sim C33A-C34A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C31 \\sim C32A \\sim C32 \\sim C33A \\sim C33 \\sim C28 \\sim C34A \\sim C35A
\\sim C36A \\sim C36 \\sim C35 \\sim C34 \\sim C37A \\sim C37 \\sim C38A \\sim
C38: within 4A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 4A
4. Rigid body (RIGU) restrains
 C37A, C35A, C34A, C33A, C32A, C28, C31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Mg1, C44A, C45A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H31a)=Sof(C34A)=Sof(H34A)=Sof(C36A)=Sof(H36d)=Sof(H36e)=Sof(H36f)=
 Sof(C37A)=Sof(H37c)=Sof(H37d)=Sof(C35A)=Sof(H35c)=Sof(H35d)=Sof(C38A)=
 Sof(H38d)=Sof(H38e)=Sof(H38f)=Sof(C33A)=Sof(C32A)=Sof(H32A)=Sof(C45A)=
 Sof(H45c)=Sof(H45d)=Sof(H45e)=Sof(C44A)=Sof(H44c)=Sof(H44d)=1-FVAR(1)
 Sof(C33)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C44)=Sof(H44a)=Sof(H44b)=Sof(C37)=
 Sof(H37a)=Sof(H37b)=Sof(C34)=Sof(H34)=Sof(C46)=Sof(H46a)=Sof(H46b)=Sof(C45)=
 Sof(H45a)=Sof(H45b)=Sof(C35)=Sof(H35a)=Sof(H35b)=Sof(C38)=Sof(H38a)=Sof(H38b)=
 Sof(H38c)=Sof(C36)=Sof(H36a)=Sof(H36b)=Sof(H36c)=Sof(C47)=Sof(H47a)=Sof(H47b)=
 Sof(H47c)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C23(H23), C18(H18), C39(H39), C34(H34), C34A(H34A)
6.b Secondary CH2 refined with riding coordinates:
 C40(H40a,H40b), C21(H21a,H21b), C19(H19a,H19b), C26(H26a,H26b), C44(H44a,
 H44b), C37(H37a,H37b), C24(H24a,H24b), C42(H42a,H42b), C46(H46a,H46b),
 C45(H45a,H45b), C35(H35a,H35b), C37A(H37c,H37d), C35A(H35c,H35d), C44A(H44c,
 H44d)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C30(H30), C16(H16), C14(H14), C31(H31), C31(H31a), C32(H32), C15(H15),
  C32A(H32A)
6.d Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C5(H5a,H5b,H5c), C11(H11a,H11b,H11c), C7(H7a,H7b,H7c),
 C10(H10a,H10b,H10c), C20(H20a,H20b,H20c), C6(H6a,H6b,H6c), C25(H25a,H25b,H25c),
  C22(H22a,H22b,H22c), C41(H41a,H41b,H41c), C27(H27a,H27b,H27c), C38(H38a,H38b,
 H38c), C36(H36a,H36b,H36c), C43(H43a,H43b,H43c), C47(H47a,H47b,H47c),
 C36A(H36d,H36e,H36f), C38A(H38d,H38e,H38f), C45A(H45c,H45d,H45e)
;
_shelx_res_checksum              20562
_olex2_date_sample_data_collection 2019-07-08
_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 1.331
_oxdiff_exptl_absorpt_empirical_full_min 0.729