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_7221138
_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 Hg2 N8, 0.5(Cl8 Hg2), Cl, 2(H2 O)'
_chemical_formula_sum            'C36 H58 Cl6 Hg3 N8 O2'
_chemical_formula_weight         1449.37
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_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                 99.587(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0947(3)
_cell_length_b                   18.4694(5)
_cell_length_c                   26.2626(7)
_cell_measurement_reflns_used    3510
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      65.0710
_cell_measurement_theta_min      3.3940
_cell_volume                     4828.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5058
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
  1 omega  -32.00   70.00   1.0000    1.2600
omega____ theta____ kappa____ phi______ frames
    -       40.5673  -57.0000   90.0000 102

  2 omega   62.00  169.00   1.0000    5.0450
omega____ theta____ kappa____ phi______ frames
    -       90.2233   15.0000  120.0000 107

  3 omega   75.00  165.00   1.0000    5.0450
omega____ theta____ kappa____ phi______ frames
    -       90.2233   45.0000    0.0000 90

  4 omega   31.00   59.00   1.0000    5.0450
omega____ theta____ kappa____ phi______ frames
    -       90.2233  -45.0000 -180.0000 28

  5 omega   13.00   60.00   1.0000    5.0450
omega____ theta____ kappa____ phi______ frames
    -       90.2233  -30.0000 -150.0000 47

  6 omega   15.00   63.00   1.0000    5.0450
omega____ theta____ kappa____ phi______ frames
    -       90.2233  -45.0000    0.0000 48

  7 omega   13.00   53.00   1.0000    5.0450
omega____ theta____ kappa____ phi______ frames
    -       90.2233  -30.0000  120.0000 40

  8 omega    2.00   73.00   1.0000    1.2600
omega____ theta____ kappa____ phi______ frames
    -       40.5673 -126.0000   60.0000 71

  9 omega -158.00 -116.00   1.0000    5.0450
omega____ theta____ kappa____ phi______ frames
    -      -83.0000 -126.0000   60.0000 42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0667410000
_diffrn_orient_matrix_UB_12      -0.0448462000
_diffrn_orient_matrix_UB_13      -0.0382287000
_diffrn_orient_matrix_UB_21      -0.1396145000
_diffrn_orient_matrix_UB_22      -0.0223565000
_diffrn_orient_matrix_UB_23      -0.0287809000
_diffrn_orient_matrix_UB_31      -0.0018644000
_diffrn_orient_matrix_UB_32      0.0666632000
_diffrn_orient_matrix_UB_33      -0.0353719000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            8346
_diffrn_reflns_theta_full        65.31
_diffrn_reflns_theta_max         65.31
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.141
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.498
_refine_diff_density_min         -2.304
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0757P)^2^+18.2227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                3345
_reflns_number_total             3993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00817d2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7221133--7221140.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7221138
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: Hg2(0.5) Cl4(0.5) Cl3(0.5) Cl5(0.5) Cl2(0.5)
3.a Free rotating group:
 O1(H1C,H1D)
3.b Ternary CH refined with riding coordinates:
 N4(H4), N3(H3), N2(H2)
3.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C3(H3A,H3B), C5(H5A,H5B), C1(H1A,H1B), C7(H7A,H7B), C4(H4A,
 H4B), C6(H6A,H6B), C9(H9A,H9B), C2(H2A,H2B)
3.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C16(H16), C15(H15), C12(H12), C11(H11)
;
_olex2_date_sample_data_collection 1427191871.14
_olex2_submission_special_instructions 'No special instructions were received'