Hydrocarbon-soluble, hexaanionic fulleride complexes of magnesium
Lawrence, Samuel R.; Ohlin, C. André; Cordes, David Bradford; Slawin, Alexandra; Stasch, Andreas; Chemical Science  (2019) –; doi:10.1039/C9SC03857D

data_1552407
_publ_section_title
;
 Hydrocarbon-soluble, hexaanionic fulleride complexes of magnesium
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC03857D
_journal_year                    2019
_chemical_formula_moiety         'C118 H82 Mg2 N4, 2.5(C6 H6)'
_chemical_formula_sum            'C133 H97 Mg2 N4'
_chemical_formula_weight         1799.87
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2019-01-17
_audit_creation_method           'by CrystalStructure 4.3'
_audit_update_record
;
2019-05-08 deposited with the CCDC.    2019-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                96.351(3)
_cell_angle_beta                 103.923(5)
_cell_angle_gamma                91.039(5)
_cell_formula_units_Z            2
_cell_length_a                   14.551(3)
_cell_length_b                   14.651(2)
_cell_length_c                   22.814(4)
_cell_measurement_reflns_used    2335
_cell_measurement_temperature    173
_cell_measurement_theta_max      46.80
_cell_measurement_theta_min      18.40
_cell_volume                     4686.7(14)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku XtaLAB P100'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1266
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            50351
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.126
_diffrn_reflns_theta_min         3.038
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1894.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene'
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1272
_refine_ls_number_reflns         16648
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1044P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9849
_reflns_number_total             16648
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9sc03857d2.cif
_cod_data_source_block           3a''
_cod_database_code               1552407
_shelx_res_checksum              11696