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_1552412
_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_absolute_configuration unk
_chemical_formula_moiety         'C198 H174 Mg6 N12'
_chemical_formula_sum            'C198 H174 Mg6 N12'
_chemical_formula_weight         2867.46
_chemical_properties_physical    Air-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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-11-02
_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                 102.678(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   18.2173(8)
_cell_length_b                   30.2552(11)
_cell_length_c                   33.8828(13)
_cell_measurement_reflns_used    16616
_cell_measurement_temperature    173
_cell_measurement_theta_max      67.11
_cell_measurement_theta_min      2.85
_cell_volume                     18219.8(13)
_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    'Superflip (Palatinus, et al., 2007)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.973
_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  0.1371
_diffrn_reflns_av_unetI/netI     0.1269
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            192610
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.682
_diffrn_reflns_theta_min         2.486
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.618
_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            black
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6072.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexanes'
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.363
_refine_ls_abs_structure_details
;
 Flack x determined using 10902 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.42(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     3985
_refine_ls_number_reflns         63773
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1505
_refine_ls_R_factor_gt           0.0894
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1535P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2648
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.937
_reflns_Friedel_fraction_max     0.921
_reflns_number_gt                34281
_reflns_number_total             63773
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9sc03857d2.cif
_cod_data_source_block           2c''
_cod_database_code               1552412
_shelx_res_checksum              80346
_shelx_fab_checksum              38385