Synthesis and structures of dinuclear cryptates with Zn(ii), Cd(ii) and Hg(ii): tuning the cascade binding mode with metal ions
Yan, Feng; Zhuang, Xiao-Mei; Lu, Tong-Bu; CrystEngComm 17 (2015) 5832–; doi:10.1039/C5CE00817D

data_7221133
_publ_section_title
;
 Synthesis and structures of dinuclear cryptates with Zn(ii), Cd(ii) and
 Hg(ii): tuning the cascade binding mode with metal ions
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5832
_journal_paper_doi               10.1039/C5CE00817D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'2(C36 H54 Cd2 N8 O H), 6(C3 H7 N O), 3(Cd I4)'
_chemical_formula_sum            'C90 H152 Cd7 I12 N22 O8'
_chemical_formula_weight         3979.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-09 deposited with the CCDC.
2015-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.6212(4)
_cell_length_b                   17.6212(4)
_cell_length_c                   71.599(2)
_cell_measurement_temperature    150(2)
_cell_volume                     19253.4(8)
_computing_cell_refinement       'RAPID AUTO V2.40'
_computing_data_collection       'RAPID AUTO V2.40'
_computing_data_reduction        'RAPID AUTO V2.40'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scan'
_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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       92
_diffrn_reflns_limit_l_min       -92
_diffrn_reflns_number            58156
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    4.077
_exptl_absorpt_correction_T_max  0.221
_exptl_absorpt_correction_T_min  0.213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T (1995) Program for absorption correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11244
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.37
_refine_diff_density_max         2.138
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+161.2851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                4518
_reflns_number_total             4923
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00817d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7221133--7221140.cif.'
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7221133