A polymeric solvent-free variant of a hydridomagnesium inverse crown
David V. Graham; Alan R. Kennedy; Robert E. Mulvey; Charles T. O'Hara; Acta Crystallographica Section C 62 (2006) m366–m368; doi:10.1107/S0108270106025091

data_2015503
_publ_section_title
;
 A polymeric solvent-free variant of a hydridomagnesium inverse crown
;
_journal_coeditor_code           HJ3015
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m366
_journal_page_last               m368
_journal_paper_doi               10.1107/S0108270106025091
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mg2 Na2 H2 (C6 H14 N1)4]'
_chemical_formula_moiety         'C24 H58 Mg2 N4 Na2'
_chemical_formula_sum            'C24 H58 Mg2 N4 Na2'
_chemical_formula_weight         497.34
_chemical_name_systematic
;
Tetra-\m~2~-diisopropylamido-di-\m~2~-hydrido-dimagnesium(II)disodium(I)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                82.419(3)
_cell_angle_beta                 83.897(3)
_cell_angle_gamma                68.916(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2448(4)
_cell_length_b                   10.1118(5)
_cell_length_c                   20.1990(9)
_cell_measurement_reflns_used    27877
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1554.36(13)
_computing_cell_refinement       'DENZO and COLLECT'
_computing_data_collection
;
COLLECT (Nonius, 1988) and DENZO (Otwinowski & Minor, 1997)
;
_computing_data_reduction        DENZO
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_sigmaI/netI    0.1130
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27877
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.02
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut tablet'
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1503
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.9833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                3944
_reflns_number_total             7078
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hj3015.cif
_cod_data_source_block           I
_cod_database_code               2015503
_cod_database_fobs_code          2015503