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_7127091
_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         'C43 H70 N2'
_chemical_formula_sum            'C43 H70 N2'
_chemical_formula_weight         615.01
_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   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                90
_cell_angle_beta                 112.986(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9665(2)
_cell_length_b                   23.6431(4)
_cell_length_c                   15.0792(3)
_cell_measurement_reflns_used    8286
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.5780
_cell_measurement_theta_min      3.6680
_cell_volume                     3927.54(15)
_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  (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 0.996
_diffrn_measured_fraction_theta_max 0.965
_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    -43.00 -13.00   1.00    1.50    --  -41.48 125.00  30.00   30
  2  \w   -116.00 -18.00   1.00    1.50    --  -41.48 -38.00-180.00   98
  3  \w    -85.00  -7.00   1.00    1.50    --  -41.48 125.00 120.00   78
  4  \w    102.00 175.00   1.00    6.00    --  104.33 125.00  30.00   73
  5  \w     38.00 106.00   1.00    6.00    --  104.33 -94.00 -30.00   68
  6  \w    107.00 158.00   1.00    6.00    --  104.33  77.00-180.00   51
  7  \w     75.00 177.00   1.00    6.00    --  104.33  61.00 120.00  102
  8  \w     28.00 132.00   1.00    6.00    --  104.33 -77.00  60.00  104
;
_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      0.0140520000
_diffrn_orient_matrix_UB_12      -0.0075966000
_diffrn_orient_matrix_UB_13      -0.0965808000
_diffrn_orient_matrix_UB_21      -0.1203082000
_diffrn_orient_matrix_UB_22      -0.0332188000
_diffrn_orient_matrix_UB_23      -0.0400234000
_diffrn_orient_matrix_UB_31      -0.0698857000
_diffrn_orient_matrix_UB_32      0.0555625000
_diffrn_orient_matrix_UB_33      -0.0371830000
_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  0.0198
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14599
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.699
_diffrn_reflns_theta_min         3.692
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (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    1.040
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.00063(7)
_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   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0437P)^2^+0.8725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6689
_reflns_number_total             7553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05200k2.cif
_cod_data_source_block           hasj200604a
_cod_depositor_comments
'Adding full bibliography for 7127086--7127091.cif.'
_cod_original_cell_volume        3927.57(16)
_cod_database_code               7127091
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C43 H70 N2'
_reflns_odcompleteness_completeness 99.57
_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
 C8-C11A \\sim C8-C11 \\sim C8-C10A \\sim C8-C10 \\sim C9-C8 \\sim C9A-C8
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C8, C9A, C10A, C11A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C9A)=Sof(H9Aa)=Sof(H9Ab)=Sof(H9Ac)=Sof(C10A)=Sof(H10d)=Sof(H10e)=
 Sof(H10f)=Sof(C11A)=Sof(H11d)=Sof(H11e)=Sof(H11f)=1-FVAR(1)
 Sof(C9)=Sof(H9a)=Sof(H9b)=Sof(H9c)=Sof(C10)=Sof(H10a)=Sof(H10b)=Sof(H10c)=
 Sof(C11)=Sof(H11a)=Sof(H11b)=Sof(H11c)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C18(H18), C23(H23), C34(H34), C39(H39)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C19(H19a,H19b), C21(H21a,H21b), C24(H24a,H24b), C26(H26a,H26b),
 C35(H35a,H35b), C37(H37a,H37b), C40(H40a,H40b), C42(H42a,H42b)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C30(H30), C31(H31), C32(H32)
5.d Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C20(H20a,H20b,H20c),
 C22(H22a,H22b,H22c), C25(H25a,H25b,H25c), C27(H27a,H27b,H27c), C36(H36a,H36b,
 H36c), C38(H38a,H38b,H38c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c), C9(H9a,
 H9b,H9c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C9A(H9Aa,H9Ab,H9Ac),
 C10A(H10d,H10e,H10f), C11A(H11d,H11e,H11f)
;
_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 1.161
_oxdiff_exptl_absorpt_empirical_full_min 0.870