Encapsulation of transition metal atoms into carbon nanotubes: a supramolecular approach
Jian Fan; Thomas W. Chamberlain; Yu Wang; Sihai Yang; Alexander J. Blake; Martin Schroder; Andrei N. Khlobystov; Chem.Commun. 47 (2011) 5696–; doi:10.1039/c1cc10427f

data_7106394
_publ_section_title
;
 Encapsulation of transition metal atoms into carbon nanotubes: a
 supramolecular approach
;
_journal_name_full               Chem.Commun.
_journal_page_first              5696
_journal_paper_doi               10.1039/c1cc10427f
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C85 H14 Cd1 O10, C H2 Cl2'
_chemical_formula_sum            'C86 H16 Cd Cl2 N6 O10'
_chemical_formula_weight         1476.35
_chemical_name_systematic
;
?
;
_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           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.364(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.351(2)
_cell_length_b                   17.1037(10)
_cell_length_c                   19.3682(11)
_cell_measurement_reflns_used    7276
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.09
_cell_measurement_theta_min      2.26
_cell_volume                     12021.2(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6911
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_sigmaI/netI    0.071
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53416
_diffrn_reflns_theta_full        21.33
_diffrn_reflns_theta_max         21.33
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5888
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.003
_platon_squeeze_details
;
Approximately 18% of the unit cell volume comprises a large region of
disordered solvent which could not be modelled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the
diffraction
from the solvent region and thereby produced a set of solvent-free
diffraction
intensities. SQUEEZE estimated a total count of 309 electrons per unit
cell,
which were assigned to be 8.0 DCM molecules per unit cell.
The final formula was calculated from the TGA combined with elemental
analysis data.
;
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.59
_refine_diff_density_rms         0.08
_refine_ls_extinction_coef       0.00112(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.00
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1838
_refine_ls_number_reflns         14586
_refine_ls_number_restraints     843
_refine_ls_restrained_S_all      0.98
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.09P)^2^+17.00P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.147
_refine_ls_wR_factor_ref         0.160
_reflns_number_gt                10162
_reflns_number_total             14586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10427f.txt
_cod_data_source_block           fulcdn
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7106394