Cationic Magnesium Hydride [MgH]+ Stabilized by an NNNN-Type Macrocycle
Okuda, Jun; Lemmerz, Lara E.; Mukherjee, Debabrata; Spaniol, Thomas Paul; Laurent, Maron; Menard, Gabriel; Wong, Anthony; Chemical Communications  (2019) –; doi:10.1039/C9CC00490D

data_7122986
_publ_section_title
;
 Cationic Magnesium Hydride [MgH]+ Stabilized by an NNNN-Type Macrocycle
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00490D
_journal_year                    2019
_chemical_formula_moiety         'C24 H58 Mg2 N8, 2(C32 H36 B), 2(C4 H8 O)'
_chemical_formula_sum            'C96 H146 B2 Mg2 N8 O2'
_chemical_formula_weight         1514.44
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-01-18 deposited with the CCDC.    2019-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.3501(5)
_cell_length_b                   12.34279(12)
_cell_length_c                   20.1258(2)
_cell_measurement_reflns_used    70160
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.36
_cell_measurement_theta_min      4.20
_cell_volume                     9029.67(18)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.131.0 (STOE, 2017)'
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area LANA 1.71.4.0 (STOE, 2017)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-92 (Altomare)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Counting Detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63436
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.893
_diffrn_reflns_theta_min         4.330
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.1317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'STOE X-Red 32'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       plate
_exptl_crystal_F_000             3312
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf and n-hexane'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.579
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 5071 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         16234
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1092P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1621
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.889
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                13365
_reflns_number_total             16234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00490d2.cif
_cod_data_source_block           2
_cod_database_code               7122986
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.746
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              12738