Steric control of Mg-Mg bond formation <i>vs.</i> N<sub>2</sub> activation in the reduction of bulky magnesium diamide complexes.
Mondal, Rahul; Evans, Matthew J.; Nguyen, Dat T.; Rajeshkumar, Thayalan; Maron, Laurent; Jones, Cameron; Chemical communications (Cambridge, England) 60 (2024) 1016–1019; doi:10.1039/d3cc05787a

data_7132515
_publ_section_title
;
 Steric control of Mg-Mg bond formation <i>vs.</i> N<sub>2</sub>
 activation in the reduction of bulky magnesium diamide complexes.
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1016
_journal_page_last               1019
_journal_paper_doi               10.1039/d3cc05787a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C98 H134 K2 Mg2 N4 O2, C6 H14'
_chemical_formula_sum            'C104 H148 K2 Mg2 N4 O2'
_chemical_formula_weight         1613.08
_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   mixed
_atom_sites_solution_primary     fmap
_audit_creation_date             2023-10-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-11-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.877(2)
_cell_angle_beta                 90.703(2)
_cell_angle_gamma                106.972(2)
_cell_formula_units_Z            2
_cell_length_a                   16.5142(3)
_cell_length_b                   16.8828(3)
_cell_length_c                   17.9517(3)
_cell_measurement_reflns_used    19482
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      79.1990
_cell_measurement_theta_min      4.4380
_cell_volume                     4785.76(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'w/ scans'
_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  0.0953
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.844
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35909
_diffrn_reflns_point_group_measured_fraction_full 0.844
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.928
_diffrn_reflns_theta_min         4.452
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       needle
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1124
_refine_ls_number_reflns         16821
_refine_ls_number_restraints     302
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1298P)^2^+5.1595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13814
_reflns_number_total             16821
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9391\% 
around [0.68 0.73 -0.03] (reciprocal) or [0.71 0.71 0.00] (direct)
;
_cod_data_source_file            d3cc05787a2.cif
_cod_data_source_block           cj1632
_cod_depositor_comments
'Adding full bibliography for 7132515--7132520.cif.'
_cod_database_code               7132515
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C4-C10 = C4-C99
 1.52 with sigma of 0.01
 C110-C109 = C109-C108 = C108-C107 = C107-C106 = C106-C105
 1.52 with sigma of 0.01
 C10-C12 = C10-C11
 1.54 with sigma of 0.01
 C99-C101 = C99-C100
 1.54 with sigma of 0.01
 C40-C47 = C40-C102
 1.52 with sigma of 0.01
 C47-C48 = C47-C49
 1.54 with sigma of 0.01
 C102-C103 = C102-C104
 1.54 with sigma of 0.01
 C116-C115 = C115-C114 = C114-C113 = C113-C112 = C112-C111
 1.52 with sigma of 0.01
 C110-C108 = C107-C105
 2.53 with sigma of 0.01
 C3-C10 = C3-C99
 2.52 with sigma of 0.01
 C5-C10 = C5-C99
 2.52 with sigma of 0.01
 C39-C47 = C39-C102
 2.52 with sigma of 0.01
 C35-C47 = C35-C102
 2.52 with sigma of 0.01
 C115-C113 = C114-C112
 2.54 with sigma of 0.01
 C109-C107 = C108-C106
 2.54 with sigma of 0.01
 C116-C114 = C113-C111
 2.53 with sigma of 0.01
 C110-C109 \\sim C109-C108 \\sim C108-C107 \\sim C107-C106 \\sim C106-C105
 with sigma of 0.02
 C110-C108 \\sim C108-C106 \\sim C109-C107 \\sim C107-C105
 with sigma of 0.04
 C116-C115 \\sim C115-C114 \\sim C114-C113 \\sim C113-C112 \\sim C112-C111
 with sigma of 0.02
 C116-C114 \\sim C114-C112 \\sim C115-C113 \\sim C113-C111
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C11 \\sim C10 \\sim C12 \\sim C5 \\sim C4 \\sim C3: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C110 \\sim C109 \\sim C108 \\sim C107 \\sim C106 \\sim C105: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C100 \\sim C99 \\sim C101 \\sim C5 \\sim C4 \\sim C3: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C49 \\sim C47 \\sim C48 \\sim C35 \\sim C40 \\sim C39: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C104 \\sim C102 \\sim C103 \\sim C35 \\sim C40 \\sim C39: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
C116 \\sim C115 \\sim C114 \\sim C113 \\sim C112 \\sim C111: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C101) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C110, C109, C108, C107, C106, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C10, C12, C5, C4, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C100, C99, C101, C5, C4, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C47, C48, C35, C40, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C104, C102, C103, C35, C40, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C116, C115, C114, C113, C112, C111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C103)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C102)=Sof(H102)=Sof(C104)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=
 Sof(H49B)=Sof(H49C)=FVAR(1)
 Sof(C99)=Sof(H99)=Sof(C100)=Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C101)=Sof(H10J)=
 Sof(H10K)=Sof(H10L)=1-FVAR(2)
 Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=FVAR(2)
 Fixed Sof: C110(0.5) H(0.5) HA(0.5) HB(0.5) C109(0.5) HC(0.5) HD(0.5)
 C108(0.5) HE(0.5) HF(0.5) C107(0.5) HG(0.5) HH(0.5) C106(0.5) HI(0.5) HJ(0.5)
 C105(0.5) HK(0.5) HL(0.5) HM(0.5) C116(0.5) HN(0.5) HO(0.5) HP(0.5) C115(0.5)
 HQ(0.5) HR(0.5) C114(0.5) HS(0.5) HT(0.5) C113(0.5) HU(0.5) HV(0.5) C112(0.5)
 HW(0.5) HX(0.5) C111(0.5) HY(0.5) HZ(0.5) H1(0.5)
5.a Ternary CH refined with riding coordinates:
 C96(H96), C56(H56), C47(H47), C41(H41), C44(H44), C7(H7), C13(H13), C90(H90),
 C93(H93), C62(H62), C59(H59), C10(H10), C102(H102), C99(H99)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C79(H79A,H79B), C34(H34A,H34B), C83(H83A,H83B), C109(HC,HD),
 C108(HE,HF), C107(HG,HH), C106(HI,HJ), C115(HQ,HR), C114(HS,HT), C113(HU,HV),
 C112(HW,HX)
5.c Me refined with riding coordinates:
 C110(H,HA,HB)
5.d Aromatic/amide H refined with riding coordinates:
 C26(H26), C37(H37), C75(H75), C20(H20), C73(H73), C39(H39), C18(H18),
 C69(H69), C5(H5), C67(H67), C52(H52), C24(H24), C88(H88), C86(H86), C3(H3),
 C54(H54)
5.e Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C43(H43A,H43B,H43C), C57(H57A,H57B,
 H57C), C80(H80A,H80B,H80C), C8(H8A,H8B,H8C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C58(H58A,H58B,H58C), C9(H9A,H9B,H9C), C94(H94A,H94B,H94C),
 C81(H81A,H81B,H81C), C42(H42A,H42B,H42C), C14(H14A,H14B,H14C), C60(H60A,H60B,
 H60C), C91(H91A,H91B,H91C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C), C78(H78A,
 H78B,H78C), C98(H98A,H98B,H98C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C),
 C92(H92A,H92B,H92C), C11(H11A,H11B,H11C), C64(H64A,H64B,H64C), C61(H61A,H61B,
 H61C), C63(H63A,H63B,H63C), C33(H33A,H33B,H33C), C82(H82A,H82B,H82C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C12(H12A,H12B,H12C), C105(HK,HL,HM), C116(HN,
 HO,HP), C111(HY,HZ,H1), C103(H10A,H10B,H10C), C104(H10D,H10E,H10F), C100(H10G,
 H10H,H10I), C101(H10J,H10K,H10L)
;
_shelx_res_checksum              31671
_shelx_hkl_checksum              41650
_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 5.666
_oxdiff_exptl_absorpt_empirical_full_min 0.227
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2