Isolation and Crystallographic Characterization of Sm@C2v(3)-C80 Through Cocrystal Formation with NiII(octaethylporphyrin) or Bis(ethylenedithio)tetrathiafulvalene
Hua Yang; Zhimin Wang; Hongxiao Jin; Bo Hong; Ziyang Liu; Christine M. Beavers; Marilyn M. Olmstead; Alan L. Balch; Inorganic Chemistry 52 (2013) 1275–1284; doi:10.1021/ic301794r

data_4333654
_publ_contact_author_address
;Advanced Light Source
Lawrence Berkeley National Lab
One Cyclotron Rd
MS 7-222
Berkeley, CA 94720
;
_publ_contact_author_email       cmbeavers@lbl.gov
_publ_contact_author_name        'Christine M. Beavers'
_publ_contact_author_phone       (510)495-2448
_publ_section_title
;
 Isolation and Crystallographic Characterization of Sm@C2v(3)-C80 Through
 Cocrystal Formation with NiII(octaethylporphyrin) or
 Bis(ethylenedithio)tetrathiafulvalene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1275
_journal_page_last               1284
_journal_paper_doi               10.1021/ic301794r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C80 Sm, C10 H8 S8, 0.5(C7 H8)'
_chemical_formula_sum            'C93.5 H12 S8 Sm'
_chemical_formula_weight         1541.86
_chemical_name_common            Sm@C2v-C80.BEDT-TTF.0.5toluene
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-07-22 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.688(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8264(6)
_cell_length_b                   21.5495(11)
_cell_length_c                   22.5795(11)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.6
_cell_measurement_theta_min      2.79
_cell_volume                     5158.6(5)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            91519
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    1.917
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.9273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS-2008/4 (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             3052
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.543
_refine_diff_density_min         -1.951
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1709
_refine_ls_number_reflns         11599
_refine_ls_number_restraints     3895
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1485P)^2^+22.5756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2593
_refine_ls_wR_factor_ref         0.2703
_reflns_number_gt                9344
_reflns_number_total             11599
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            ic301794r_si_002_1.cif
_cod_data_source_block           cb169
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C93.50 H12 S8 Sm'
_cod_database_code               4333654