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_7221136
_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 Cl N8 Zn2, 3(Cl O4), 3(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C42 H67 Cl4 N11 O14 Zn2'
_chemical_formula_weight         1222.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                87.296(7)
_cell_angle_beta                 66.076(7)
_cell_angle_gamma                81.938(6)
_cell_formula_units_Z            2
_cell_length_a                   13.149(5)
_cell_length_b                   14.006(5)
_cell_length_c                   15.694(6)
_cell_measurement_reflns_used    930
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2615.7(17)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20172
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         11058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0855P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1651
_reflns_number_gt                6326
_reflns_number_total             11058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00817d2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7221133--7221140.cif.
;
_cod_original_cell_volume        2615.6(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7221136