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_7132517
_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_sum            'C103 H144 K2 Mg2 N4 O3'
_chemical_formula_weight         1613.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-11-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      80.1690
_cell_measurement_theta_min      3.6000
_cell_volume                     9900.38(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_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  0.0310
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48050
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.358
_diffrn_reflns_theta_min         3.622
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 7393 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1168
_refine_ls_number_reflns         19586
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0860P)^2^+2.3074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.718
_reflns_Friedel_fraction_full    0.899
_reflns_Friedel_fraction_max     0.821
_reflns_number_gt                18588
_reflns_number_total             19586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05787a2.cif
_cod_data_source_block           cj1635
_cod_depositor_comments
'Adding full bibliography for 7132515--7132520.cif.'
_cod_database_code               7132517
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.716
_oxdiff_exptl_absorpt_empirical_full_max 1.805
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              58012
_shelx_hkl_checksum              20772