Solid-vapour reactions as a post-synthetic modification tool for molecular crystals: the enclathration of benzene and toluene by Werner complexes
Matteo Lusi; Leonard J. Barbour; Chem.Commun. 49 (2013) 2634–; doi:10.1039/c3cc40521d

data_7109015
_publ_section_title
;
 Solid-vapour reactions as a post-synthetic modification tool for
 molecular crystals: the enclathration of benzene and toluene by Werner
 complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              2634
_journal_paper_doi               10.1039/c3cc40521d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C60 H52 N6 Ni S2'
_chemical_formula_weight         979.91
_chemical_name_common            ml108
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   43.6737(9)
_cell_length_b                   10.2287(2)
_cell_length_c                   22.9715(4)
_cell_measurement_temperature    100(2)
_cell_volume                     10261.9(3)
_computing_cell_refinement       'SMART (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-Seed (Barbour,2001;Atwood&Barbour,2003)'
_computing_publication_material  'X-Seed (Barbour,2001;Atwood&Barbour,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.858
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17282
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         34.55
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.9513
_exptl_absorpt_correction_T_min  0.8633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2002'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.375(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         8191
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+3.7190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                7131
_reflns_number_total             8191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40521d.txt
_cod_data_source_block           C:1tolI.CIF
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               7109015