Low-Nuclearity Magnesium Hydride Complexes Stabilized by N-Heterocyclic Carbenes
Freeman, Lucas; Walley, Jacob; Dickie, Diane Amanda; Gilliard, Robert J.; Dalton Transactions  (2019) –; doi:10.1039/C9DT03915E

data_7701832
_publ_section_title
;
 Low-Nuclearity Magnesium Hydride Complexes Stabilized by N-Heterocyclic
 Carbenes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03915E
_journal_year                    2019
_chemical_formula_moiety         'C24 H64 Mg2 N4 Si8'
_chemical_formula_sum            'C24 H64 Mg2 N4 Si8'
_chemical_formula_weight         682.13
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_update_record
;
2019-08-22 deposited with the CCDC.	2019-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.891(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5402(9)
_cell_length_b                   16.7067(13)
_cell_length_c                   20.9436(17)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.430
_cell_measurement_theta_min      2.259
_cell_volume                     3989.4(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service v2017.5.0.0'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8.3333
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59939
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.571
_diffrn_reflns_theta_min         1.567
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0575 before and 0.0380 after correction. The Ratio of minimum to maximum transmission is 0.8747. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes'
_exptl_crystal_size_max          0.856
_exptl_crystal_size_mid          0.396
_exptl_crystal_size_min          0.298
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         13286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0324P)^2^+3.8881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11072
_reflns_number_total             13286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03915e2.cif
_cod_data_source_block           1
_cod_database_code               7701832
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.771
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C15(H15A,H15B), C9(H9A,H9B), C16(H16A,H16B), C10(H10A,H10B),
 C4(H4A,H4B), C3(H3A,H3B), C21(H21A,H21B)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C17(H17C,H17B,H17A), C6(H6C,H6B,H6A), C8(H8C,H8B,H8A),
 C5(H5A,H5B,H5C), C20(H20B,H20C,H20A), C7(H7A,H7C,H7B), C23(H23C,H23B,H23A),
 C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C18(H18B,H18A,H18C), C1(H1A,H1B,H1C),
  C19(H19C,H19A,H19B), C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C14(H14B,H14C,H14A)
;
_shelx_res_checksum              38197
_olex2_submission_special_instructions 'No special instructions were received'