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_1552409
_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         'C210 H198 Mg6 N12'
_chemical_formula_sum            'C210 H198 Mg6 N12'
_chemical_formula_weight         3035.78
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-11-14
_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                90.0000
_cell_angle_beta                 93.4861(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   26.4392(3)
_cell_length_b                   23.3427(3)
_cell_length_c                   27.4336(4)
_cell_measurement_reflns_used    35101
_cell_measurement_temperature    173
_cell_measurement_theta_max      67.80
_cell_measurement_theta_min      2.50
_cell_volume                     16899.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 5.811
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_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  0.0734
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            176295
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.308
_diffrn_reflns_theta_min         2.487
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6456.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexanes'
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     2194
_refine_ls_number_reflns         30656
_refine_ls_number_restraints     94
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0975P)^2^+39.1933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2379
_refine_ls_wR_factor_ref         0.2503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23264
_reflns_number_total             30656
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9sc03857d2.cif
_cod_data_source_block           2b'
_cod_database_code               1552409
_shelx_res_checksum              46939
_shelx_fab_checksum              44398