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_7127089
_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         'C86 H138 Mg2 N4'
_chemical_formula_sum            'C86 H138 Mg2 N4'
_chemical_formula_weight         1276.62
_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                91.446(3)
_cell_angle_beta                 95.022(3)
_cell_angle_gamma                97.171(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0072(4)
_cell_length_b                   16.9342(8)
_cell_length_c                   21.7042(7)
_cell_measurement_reflns_used    7965
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.5480
_cell_measurement_theta_min      4.0270
_cell_volume                     3995.9(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 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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.961
_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   -115.00 -17.00   1.00   10.00    --  -41.19 -38.00 -90.00   98
  2  \w    -87.00  -8.00   1.00   10.00    --  -41.19 125.00  60.00   79
  3  \w    -87.00  -9.00   1.00   10.00    --  -41.19 125.00 150.00   78
  4  \w   -110.00 -26.00   1.00   10.00    --  -41.19 -38.00   0.00   84
  5  \w     32.00 118.00   1.00   40.00    --  104.37 -45.00-150.00   86
  6  \w    103.00 178.00   1.00   40.00    --  104.37  77.00 150.00   75
  7  \w     44.00 152.00   1.00   40.00    --  104.37 -15.00 -30.00  108
  8  \w    106.00 162.00   1.00   40.00    --  104.37  77.00 -60.00   56
  9  \w    106.00 169.00   1.00   40.00    --  104.37  77.00   0.00   63
 10  \w     38.00 106.00   1.00   40.00    --  104.37 -94.00  60.00   68
 11  \w     34.00 121.00   1.00   40.00    --  104.37 -61.00  60.00   87
 12  \w     37.00 112.00   1.00   40.00    --  104.37-125.00-120.00   75
 13  \w     37.00 112.00   1.00   40.00    --  104.37-125.00  30.00   75
 14  \w     55.00 107.00   1.00   40.00    --  104.37 -98.00-117.25   52
;
_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      0.0659750000
_diffrn_orient_matrix_UB_12      0.0832026000
_diffrn_orient_matrix_UB_13      -0.0117886000
_diffrn_orient_matrix_UB_21      0.1183828000
_diffrn_orient_matrix_UB_22      -0.0210707000
_diffrn_orient_matrix_UB_23      0.0355074000
_diffrn_orient_matrix_UB_31      0.0412241000
_diffrn_orient_matrix_UB_32      -0.0324304000
_diffrn_orient_matrix_UB_33      -0.0606968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0921
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26690
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.747
_diffrn_reflns_theta_min         4.065
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.828
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       plate
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         15298
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0845
_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^)+(0.1447P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2180
_refine_ls_wR_factor_ref         0.2475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10756
_reflns_number_total             15298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05200k2.cif
_cod_data_source_block           hasj190725a
_cod_depositor_comments
'Adding full bibliography for 7127086--7127091.cif.'
_cod_database_code               7127089
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C86H140Mg2N4
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.910
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     42.60
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C35 \\sim C35A-C34A \\sim C34-C37 \\sim C34A-C37 \\sim C19-C18 \\sim
C18A-C19 \\sim C21-C18 ~
 C18A-C21A
 with sigma of 0.02
 C35A-C36A \\sim C36-C35 \\sim C38-C37 \\sim C22-C21 \\sim C21A-C22A \\sim
C19-C20
 with sigma of 0.02
 C27A-C26 \\sim C27-C26
 with sigma of 0.02
 C18-C13 \\sim C18A-C13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C35 \\sim C36 \\sim C34A \\sim C35A \\sim C36A: within 4A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 4A
C13 \\sim C19 \\sim C18 \\sim C21 \\sim C18A \\sim C21A: within 4A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 4A
4. Rigid body (RIGU) restrains
 C13, C19, C18A, C21A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H37c)=Sof(H37d)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35c)=Sof(H35d)=
 Sof(C36A)=Sof(H36d)=Sof(H36e)=Sof(H36f)=1-FVAR(1)
 Sof(H37a)=Sof(H37b)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35a)=Sof(H35b)=Sof(C36)=
 Sof(H36a)=Sof(H36b)=Sof(H36c)=FVAR(1)
 Sof(H19c)=Sof(H19d)=Sof(C18A)=Sof(H18A)=Sof(C21A)=Sof(H21c)=Sof(H21d)=
 Sof(C22A)=Sof(H22d)=Sof(H22e)=Sof(H22f)=1-FVAR(2)
 Sof(H19a)=Sof(H19b)=Sof(C18)=Sof(H18)=Sof(C21)=Sof(H21a)=Sof(H21b)=Sof(C22)=
 Sof(H22a)=Sof(H22b)=Sof(H22c)=FVAR(2)
 Sof(H26c)=Sof(H26d)=Sof(C27A)=Sof(H27d)=Sof(H27e)=Sof(H27f)=1-FVAR(3)
 Sof(H26a)=Sof(H26b)=Sof(C27)=Sof(H27a)=Sof(H27b)=Sof(H27c)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C23(H23), C39(H39), C61(H61), C66(H66), C77(H77), C82(H82), C18(H18),
 C34(H34), C18A(H18A), C34A(H34A)
6.b Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C19(H19c,H19d), C24(H24a,H24b), C26(H26a,H26b), C26(H26c,
 H26d), C37(H37c,H37d), C37(H37a,H37b), C40(H40a,H40b), C42(H42a,H42b),
 C62(H62a,H62b), C64(H64a,H64b), C67(H67a,H67b), C69(H69a,H69b), C78(H78a,H78b),
  C80(H80a,H80b), C83(H83a,H83b), C85(H85a,H85b), C21(H21a,H21b), C35(H35a,
 H35b), C21A(H21c,H21d), C35A(H35c,H35d)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C15(H15), C16(H16), C30(H30), C31(H31), C32(H32), C45(H45),
 C57(H57), C58(H58), C59(H59), C73(H73), C74(H74), C75(H75)
6.d Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C11(H11a,H11b,H11c), C20(H20a,H20b,H20c), C25(H25a,H25b,H25c),
 C38(H38a,H38b,H38c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c), C48(H48a,H48b,
 H48c), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c), C52(H52a,H52b,H52c), C53(H53a,
 H53b,H53c), C54(H54a,H54b,H54c), C63(H63a,H63b,H63c), C65(H65a,H65b,H65c),
 C68(H68a,H68b,H68c), C70(H70a,H70b,H70c), C79(H79a,H79b,H79c), C81(H81a,H81b,
 H81c), C84(H84a,H84b,H84c), C86(H86a,H86b,H86c), C22(H22a,H22b,H22c), C27(H27a,
 H27b,H27c), C36(H36a,H36b,H36c), C22A(H22d,H22e,H22f), C27A(H27d,H27e,H27f),
 C36A(H36d,H36e,H36f)
;
_shelx_res_checksum              72795
_olex2_date_sample_data_collection 2019-07-25
_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 3.309
_oxdiff_exptl_absorpt_empirical_full_min 0.437