Crystal structures of [18]aneN~6~H~2~K[Co(CN)~6~].4H~2~O, [16]aneN~4~H~2~K[Co(CN)~6~] and [12]aneN~4~H~3~[Co(CN)~6~].2H~2~O. Insight into the electrostatic and hydrogen-bonding interaction in self-assembling supercomplexes
Steve C.F. Au-Yeung; Acta Crystallographica Section B 55 (1999) 389–395; doi:10.1107/S0108768198014281

data_2003056
_publ_section_title
;
 Crystal structures of [18]aneN~6~H~2~K[Co(CN)~6~].4H~2~O,
 [16]aneN~4~H~2~K[Co(CN)~6~] and [12]aneN~4~H~3~[Co(CN)~6~].2H~2~O.
 Insight into the electrostatic and hydrogen-bonding interaction in
 self-assembling supercomplexes
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              389
_journal_page_last               395
_journal_paper_doi               10.1107/S0108768198014281
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          'H3[Co(C N)6](C8 H20 N4),2(H2 O)'
_chemical_formula_moiety         'C14 H23 Co N10,2(H2 O)'
_chemical_formula_sum            'C14 H27 Co N10 O2'
_chemical_formula_weight         426.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                109.080(10)
_cell_angle_beta                 103.460(10)
_cell_angle_gamma                107.030(10)
_cell_formula_units_Z            1
_cell_length_a                   7.635(2)
_cell_length_b                   8.202(5)
_cell_length_c                   9.442(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     497.7(4)
_computing_cell_refinement       'Siemens XSCANS ver. 2.10b'
_computing_data_collection       'Siemens XSCANS ver. 2.10b'
_computing_data_reduction        'Siemens XSCANS ver. 2.10b'
_computing_molecular_graphics    'SHELXTL-PC (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXTL-PC (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_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  0.1870
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2375
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        -1.5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       Plate
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.470
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.370
_refine_ls_hydrogen_treatment
; One H atom on O2W, and the acidic H atoms of the macrocycle can not be
 located from differential map
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2015
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_obs          0.0614
_refine_ls_shift/esd_max         0.150
_refine_ls_shift/esd_mean        0.011
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(Fo)+0.002(Fo^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0820
_refine_ls_wR_factor_obs         0.0741
_reflns_number_observed          2015
_reflns_number_total             2374
_reflns_observed_criterion       >4sigma(F)
_cod_data_source_file            oa0016.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo)+0.002(Fo^2^)]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w=1/[\s^2^(Fo)+0.002(Fo^2^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2003056