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_7133686
_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            'C100 H138 Ca2 N4 O0.4'
_chemical_formula_weight         1482.70
_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
_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                106.3540(10)
_cell_angle_beta                 102.1740(10)
_cell_angle_gamma                113.558(2)
_cell_formula_units_Z            1
_cell_length_a                   12.5680(2)
_cell_length_b                   14.4876(2)
_cell_length_c                   14.5826(2)
_cell_measurement_reflns_used    19780
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      79.1300
_cell_measurement_theta_min      3.6160
_cell_volume                     2171.82(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.984
_diffrn_measured_fraction_theta_max 0.948
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27837
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.796
_diffrn_reflns_theta_min         6.392
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       plate
_exptl_crystal_F_000             809
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   0.807
_exptl_transmission_factor_min   0.725
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8957
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0680P)^2^+0.5892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8536
_reflns_number_total             8957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04286g2.cif
_cod_data_source_block           cj1697
_cod_depositor_comments
'Adding full bibliography for 7133684--7133690.cif.'
_cod_original_cell_volume        2171.82(6)
_cod_original_formula_sum        'C100 H138 Ca2 N4 O0.40'
_cod_database_code               7133686
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.807
_shelx_res_checksum              52833
_shelx_hkl_checksum              84879