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_7221134
_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_absolute_configuration unk
_chemical_formula_moiety
' (C36 H54 Cd2 Cl N8), (Cd Cl4), (Cl), 4.5(H2 O)'
_chemical_formula_sum            'C36 H63 Cd3 Cl6 N8 O4.5'
_chemical_formula_weight         1229.84
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 99.012(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1322(14)
_cell_length_b                   18.536(2)
_cell_length_c                   26.333(4)
_cell_measurement_temperature    163(2)
_cell_volume                     4884.6(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      163(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            13923
_diffrn_reflns_theta_full        27.33
_diffrn_reflns_theta_max         27.33
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.668
_exptl_absorpt_correction_T_max  0.606
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2468
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.462
_refine_diff_density_min         -1.787
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         9580
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0849P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                8690
_reflns_number_total             9580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00817d2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7221133--7221140.cif.'
_cod_original_sg_symbol_Hall     'C 2y '
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C36 H63 Cd3 Cl6 N8 O4.50'
_cod_database_code               7221134