Internal and External Factors in the Structural Organization in Cocrystals of the Mixed-Metal Endohedrals (GdSc2N@Ih-C80, Gd2ScN@Ih-C80, and TbSc2N@Ih-C80) and Nickel(II) Octaethylporphyrin
Steven Stevenson; Christopher J. Chancellor; Hon Man Lee; Marilyn M. Olmstead; Alan L. Balch; Inorganic Chemistry 47 (2008) 1420–1427; doi:10.1021/ic701824q

data_4304337
_publ_section_title
;
Internal and External Factors in the Structural Organization in Cocrystals
of the Mixed-Metal Endohedrals (GdSc2N@Ih-C80, Gd2ScN@Ih-C80, and
TbSc2N@Ih-C80) and Nickel(II) Octaethylporphyrin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1420
_journal_page_last               1427
_journal_paper_doi               10.1021/ic701824q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'Gd2Sc1N@C80 . NiOEP . 2 C6H6'
_chemical_formula_sum            'C128 H56 Gd2 N5 Ni Sc'
_chemical_formula_weight         2081.95
_chemical_name_systematic
;
 Gd2Sc1N@C80(Ih) . NiOEP . 2 C6H6
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.2160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.3061(11)
_cell_length_b                   15.0474(7)
_cell_length_c                   39.377(2)
_cell_measurement_reflns_used    8492
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      55.637
_cell_measurement_theta_min      5.027
_cell_volume                     14932.3(12)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics
'XP, SHELXTL 5.1(Sheldrick, 1994), ORTEP-3 for Windows(Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            81538
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.161
_exptl_absorpt_correction_T_max  0.9341
_exptl_absorpt_correction_T_min  0.8194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             8288
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1270
_refine_ls_number_reflns         13529
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+49.3081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                11034
_reflns_number_total             13529
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701824q-file001.cif
_cod_data_source_block           cjc110
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        14932.2(13)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4304337