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_7109016
_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            'C30 H26 N3 Ni0.5 S'
_chemical_formula_weight         489.95
_chemical_name_common            work
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 99.406(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.620(6)
_cell_length_b                   23.084(12)
_cell_length_c                   22.693(12)
_cell_measurement_temperature    293(2)
_cell_volume                     5488(5)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11777
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.9632
_exptl_absorpt_correction_T_min  0.9456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2002'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1734P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2223
_refine_ls_wR_factor_ref         0.2769
_reflns_number_gt                2447
_reflns_number_total             3936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40521d.txt
_cod_data_source_block           C:\1tolII.CIF
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C30 H26 N3 Ni0.50 S'
_cod_database_code               7109016