Reactions between macrocyclic nickel(II) complexes and ferricyanide. Metamagnetic properties of a two-dimensional honeycomb assembly [NiL3]3[Fe(CN)6]2·8H2O (L3 = 3,10-dihydroxyethyl-1,3,6,8,10,12-hexaazacyclotetradecane) †
Kou, Hui-Zhong; Bu, Wei-Ming; Gao, Song; Liao, Dai-Zheng; Jiang, Zong-Hui; Yan, Shi-Ping; Fan, Yu-Guo; Wang, Geng-Lin; Journal of the Chemical Society, Dalton Transactions  (2000) 2996–; doi:10.1039/b003289l

data_7009741
_publ_section_title
;
 Reactions between macrocyclic nickel(II) complexes and ferricyanide.
 Metamagnetic properties of a two-dimensional honeycomb assembly
 [NiL3]3[Fe(CN)6]2&#x00B7;8H2O
 (L3&#x2005;=&#x2005;3,10-dihydroxyethyl-1,3,6,8,10,12-hexaazacyclotetradecane)&#x200A;&#x2020;
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2996
_journal_paper_doi               10.1039/b003289l
_journal_year                    2000
_chemical_formula_sum            'C48 H106 Fe2 N30 Ni3 O14'
_chemical_formula_weight         1615.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   14.993(3)
_cell_length_b                   14.993(3)
_cell_length_c                   18.450(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.35
_cell_measurement_theta_min      4.72
_cell_volume                     3591.7(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4951
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.57
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  0.9534
_exptl_absorpt_correction_T_min  0.7332
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.169
_refine_ls_goodness_of_fit_obs   1.455
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_restrained_S_obs      1.455
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_obs          0.0456
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0721
_refine_ls_wR_factor_obs         0.0652
_reflns_number_observed          1875
_reflns_number_total             2113
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b003289l.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^2^)+(0.0732P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3591.8(12)
_cod_original_sg_symbol_H-M      P-3c1
_cod_database_code               7009741