Isolation and Crystallographic Characterization of Gd3N@D2(35)-C88 through Non-Chromatographic Methods.
Stevenson, Steven; Arvola, Kristine D.; Fahim, Muska; Martin, Benjamin R.; Ghiassi, Kamran B.; Olmstead, Marilyn M.; Balch, Alan L.; Inorganic chemistry 55 (2015) 62–; doi:10.1021/acs.inorgchem.5b01814

data_4344821
_publ_section_title
;
 Isolation and Crystallographic Characterization of Gd3N@D2(35)-C88
 through Non-Chromatographic Methods.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              62
_journal_paper_doi               10.1021/acs.inorgchem.5b01814
_journal_volume                  55
_journal_year                    2015
_chemical_formula_moiety         'C88 Gd3 N, C36 H44 N4 Ni, 2 (C7 H8)'
_chemical_formula_sum            'C138 H60 Gd3 N5 Ni'
_chemical_formula_weight         2318.37
_chemical_name_common            'Gd3N@D2(35)-C88 . Ni(OEP) . 2 toluene'
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.599(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2389(16)
_cell_length_b                   15.3624(9)
_cell_length_c                   20.5877(12)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.283
_cell_measurement_theta_min      2.804
_cell_volume                     7956.8(8)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'Apex2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 CMOS detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            89654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         40.310
_diffrn_reflns_theta_min         2.143
_diffrn_source                   'ALS, Beamline 11.3.1'
_exptl_absorpt_coefficient_mu    3.471
_exptl_absorpt_correction_T_max  0.4420
_exptl_absorpt_correction_T_min  0.3766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_description       block
_exptl_crystal_F_000             4572
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.394
_refine_diff_density_min         -3.061
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         19828
_refine_ls_number_restraints     847
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1356P)^2^+52.5090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2424
_refine_ls_wR_factor_ref         0.2670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15548
_reflns_number_total             19828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01814_si_002.cif
_cod_data_source_block           kbg239
_cod_database_code               4344821
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.516
_shelx_estimated_absorpt_t_max   0.819
_shelx_res_checksum              95574
_shelx_hkl_checksum              49187