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_7122984
_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         'C12 H32 B Mg N4, C32 H36 B'
_chemical_formula_sum            'C44 H68 B2 Mg N4'
_chemical_formula_weight         698.95
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 90.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.870(2)
_cell_length_b                   15.682(3)
_cell_length_c                   11.922(2)
_cell_measurement_reflns_used    20596
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      90.00
_cell_measurement_theta_min      3.72
_cell_volume                     2219.2(7)
_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 0.903
_diffrn_measured_fraction_theta_max 0.918
_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  0.0246
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.903
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12825
_diffrn_reflns_point_group_measured_fraction_full 0.827
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         68.235
_diffrn_reflns_theta_min         4.672
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.8271
_exptl_absorpt_correction_T_min  0.1104
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       rod
_exptl_crystal_F_000             764
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: thf and cyclohexane'
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.03(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6907
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0637
_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^)+(0.1207P)^2^+1.0311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1732
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.736
_reflns_Friedel_fraction_max     0.777
_reflns_number_gt                6357
_reflns_number_total             6907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00490d2.cif
_cod_data_source_block           3
_cod_database_code               7122984
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.798
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              92536