A series of neutral alkaline earth metal hydride complexes supported by a bulky, unsymmetrical β-diketiminate ligand, [{(<sup>Dip/TCHP</sup>Nacnac)M(μ-H)}<sub>2</sub>] (M = Mg, Ca, Sr or Ba).
Kennedy, Dominic B.; Evans, Matthew J.; Jones, Dafydd D. L.; Parr, Joseph M.; Hill, Michael S.; Jones, Cameron; Chemical communications (Cambridge, England) 60 (2024) 10894–10897; doi:10.1039/d4cc04286g

data_7133687
_publ_section_title
;
 A series of neutral alkaline earth metal hydride complexes supported by a
 bulky, unsymmetrical &#x3b2;-diketiminate ligand,
 [{(<sup>Dip/TCHP</sup>Nacnac)M(&#x3bc;-H)}<sub>2</sub>] (M = Mg, Ca, Sr
 or Ba).
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10894
_journal_page_last               10897
_journal_paper_doi               10.1039/d4cc04286g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_sum            'C82 H120 Mg2 N4'
_chemical_formula_weight         1210.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     fmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-08-21 deposited with the CCDC.	2024-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.123(3)
_cell_length_b                   14.871(3)
_cell_length_c                   17.362(4)
_cell_measurement_reflns_used    47314
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.381
_cell_measurement_theta_min      1.173
_cell_volume                     3904.6(14)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 13.3
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  MX2
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2105
_diffrn_reflns_av_unetI/netI     0.1275
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47314
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.381
_diffrn_reflns_theta_min         1.173
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  'Value not reported by XDS'
_exptl_absorpt_correction_T_min  'Value not reported by XDS'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.030
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 655 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7831
_refine_ls_number_restraints     645
_refine_ls_restrained_S_all      0.849
_refine_ls_R_factor_all          0.1882
_refine_ls_R_factor_gt           0.0839
_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^)+(0.1395P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2184
_refine_ls_wR_factor_ref         0.2935
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                2471
_reflns_number_total             7831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04286g2.cif
_cod_data_source_block           cj1700
_cod_depositor_comments
'Adding full bibliography for 7133684--7133690.cif.'
_cod_database_code               7133687
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.999
_shelx_estimated_absorpt_t_max   1.000
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_smtbx_masks_special_details
;
The unit cell contains 2 benzene solvates that were poorly ordered, such
that a suitable crystallographic model could not be derived. Consequently,
these solvates were treated as a diffuse contribution to the overall 
scattering without specific atom positions using the Olex2 implementation of
SQUEEZE (Acta Cryst. (2015). C71, 9-18), also known as Solvent Mask. 
(Acta Cryst. A 1990, A46, 194., J. Appl. Cryst., 42: 339-341. & J. Molec. 
Biol. 1994, 243, 100).
;
_shelx_res_checksum              52490
_shelx_hkl_checksum              73167
_shelx_fab_checksum              90506