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_7221135
_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
'(C36 H54 Br Cd2 N8), (Br4 Cd), (Br), 1.5(H2 O) '
_chemical_formula_sum            'C36 H57 Br6 Cd3 N8 O1.5'
_chemical_formula_weight         1442.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.2200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.67100(10)
_cell_length_b                   33.8375(4)
_cell_length_c                   14.2619(2)
_cell_measurement_temperature    150.00(10)
_cell_volume                     4659.73(10)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd.)'
_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      150.00(10)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Gemini S Ultra'
_diffrn_measurement_method       '\w and \p scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25527
_diffrn_reflns_theta_full        62.50
_diffrn_reflns_theta_max         62.50
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    17.204
_exptl_absorpt_correction_T_max  0.423
_exptl_absorpt_correction_T_min  0.224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.213
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7372
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+17.9703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                6666
_reflns_number_total             7372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00817d2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7221133--7221140.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C36 H57 Br6 Cd3 N8 O1.50'
_cod_database_code               7221135