Crystallographic identification of Eu@C2n (2n = 88, 86 and 84): completing a transformation map for existing metallofullerenes
Bao, Lipiao; Yu, Pengyuan; Pan, Changwang; Shen, Wangqiang; Lu, Xing; Chemical Science  (2019) –; doi:10.1039/C8SC04906H

data_1550367
_publ_section_title
;
 Crystallographic identification of Eu@C2n (2n = 88, 86 and 84):
 completing a transformation map for existing metallofullerenes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04906H
_journal_year                    2019
_chemical_formula_moiety         '2(C86 Eu), 3(C36 H44 N4 Ni)'
_chemical_formula_sum            'C280 H132 Eu2 N12 Ni3'
_chemical_formula_weight         4144.02
_chemical_name_common            'Eu@C1(7)-C86 Ni(OEP)'
_chemical_name_systematic        'Eu@C1(7)-C86 Ni(OEP)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-09-16 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.995(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.307(5)
_cell_length_b                   18.191(5)
_cell_length_c                   22.087(6)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.031
_cell_measurement_theta_min      2.560
_cell_volume                     9587(4)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD MX-300'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6525
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            65568
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        23.048
_diffrn_reflns_theta_max         23.192
_diffrn_reflns_theta_min         1.292
_diffrn_source                   'SSRF, Beamline B17B1'
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             4212
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
The unit cell may contain benzene and/or carbon disulfide molecules 
which have been treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1094
_refine_ls_number_reflns         9101
_refine_ls_number_restraints     7959
_refine_ls_restrained_S_all      1.473
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.1407
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+80.1851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2961
_refine_ls_wR_factor_ref         0.3150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5816
_reflns_number_total             9101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04906h2.cif
_cod_data_source_block           lb206
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1550367
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.925
_exptl_absorpt_special_details   SADABS
_shelx_res_checksum              4492
_shelx_fab_checksum              41175