Metal-binding studies of linear rigid-axle [2]pseudorotaxanes with in situ generated anionic metal halide complexes
Fernando, Isurika R.; Mo, Yirong; Mezei, Gellert; CrystEngComm 16 (2014) 7320–; doi:10.1039/C4CE00789A

data_7216361
_publ_section_title
;
 Metal-binding studies of linear rigid-axle [2]pseudorotaxanes with in
 situ generated anionic metal halide complexes
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              7320
_journal_paper_doi               10.1039/C4CE00789A
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C58 H67.5 Br4 Cd Cl1.5 N4 O12'
_chemical_formula_weight         1497.87
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                91.8350(10)
_cell_angle_beta                 100.9020(10)
_cell_angle_gamma                92.9550(10)
_cell_formula_units_Z            4
_cell_length_a                   11.1323(2)
_cell_length_b                   20.1613(3)
_cell_length_c                   28.3599(5)
_cell_measurement_reflns_used    9164
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.63
_cell_measurement_theta_min      2.17
_cell_volume                     6236.29(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1536
_diffrn_reflns_av_unetI/netI     0.2103
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            174034
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.530
_diffrn_reflns_theta_min         1.012
_exptl_absorpt_coefficient_mu    3.039
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6604
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       prism
_exptl_crystal_F_000             3012
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.076
_refine_diff_density_max         2.811
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1452
_refine_ls_number_reflns         37707
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.2281
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1064P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15215
_reflns_number_total             37707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00789a2.cif
_cod_data_source_block           2[CdBr4]+0.5CHCl3+1.5CH3OH+0.5H2O
_cod_depositor_comments
'Adding full bibliography for 7216357--7216370.cif.'
_cod_original_formula_sum        'C58 H67.50 Br4 Cd Cl1.50 N4 O12'
_cod_database_code               7216361
_shelx_estimated_absorpt_t_min   0.569
_shelx_estimated_absorpt_t_max   0.802