Sterically shielded primary anilides of the alkaline-earth metals of the type (thf)nAe(NH-Ar*)2 (Ae = Mg, Ca, Sr, and Ba; Ar* = bulky aryl)
Westerhausen, Matthias; Schüler, Philipp; Krieck, Sven; Görls, Helmar; Liebing, Phil; Dalton Transactions  (2022) –; doi:10.1039/D2DT01121B

data_7710273
_publ_section_title
;
 Sterically shielded primary anilides of the alkaline-earth metals of the
 type (thf)nAe(NH-Ar*)2 (Ae = Mg, Ca, Sr, and Ba; Ar* = bulky aryl)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01121B
_journal_year                    2022
_chemical_formula_moiety         'C45 H53 Mg N O2'
_chemical_formula_sum            'C45 H53 Mg N O2'
_chemical_formula_weight         664.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-02-16 deposited with the CCDC.	2022-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.620(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.9665(5)
_cell_length_b                   17.3376(4)
_cell_length_c                   18.9540(5)
_cell_measurement_reflns_used    40739
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.484
_cell_measurement_theta_min      1.470
_cell_volume                     7563.0(3)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi + omega - scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40739
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.470
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.362
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8671
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0884
_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^)+(0.0638P)^2^+30.1321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6309
_reflns_number_total             8671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01121b2.cif
_cod_data_source_block           FO7475_2bBu
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7710273
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.991
_shelx_estimated_absorpt_t_max   0.993
_exptl_absorpt_special_details
; 
 The following wavelength and cell were deduced by SADABS from the 
 direction cosines etc. They are given here for emergency use only: 
 CELL 0.71079   27.928   17.331   18.949   89.992  124.578   90.010 
;
_shelx_res_checksum              30083
_shelx_hkl_checksum              77459