Synthesis, crystal structure and metamagnetic properties of a two-dimensional honeycomb network based on ferricyanide and (3,10-dimethyl-1,3,5,8,10,12-hexaazacyclotetradecane)nickel(II) building blocks †
Kou, Hui-Zhong; Gao, Song; Bu, Wei-Ming; Liao, Dai-Zheng; Ma, Bao-Qing; Jiang, Zong-Hui; Yan, Shi-Ping; Fan, Yu-Guo; Wang, Geng-Lin; Journal of the Chemical Society, Dalton Transactions  (1999) 2477–; doi:10.1039/a902228g

data_7027406
_publ_section_title
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 Synthesis, crystal structure and metamagnetic properties of a
 two-dimensional honeycomb network based on ferricyanide and
 (3,10-dimethyl-1,3,5,8,10,12-hexaazacyclotetradecane)nickel(II) building
 blocks&#x200A;&#x2020;
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_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2477
_journal_paper_doi               10.1039/a902228g
_journal_year                    1999
_chemical_formula_sum            'C42 H96 Fe2 N30 Ni3 O9'
_chemical_formula_weight         1453.32
_chemical_name_systematic
; 
 ? 
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_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                   14.809(3)
_cell_length_b                   14.809(3)
_cell_length_c                   18.390(3)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.71
_cell_measurement_theta_min      4.74
_cell_volume                     3492.7(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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6176
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        8.58%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.344
_exptl_absorpt_correction_type   'semi-empirical from psi-scan'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.0010(5)
_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   0.991
_refine_ls_goodness_of_fit_obs   1.134
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_obs          0.0485
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1255
_refine_ls_wR_factor_obs         0.1090
_reflns_number_observed          1974
_reflns_number_total             2688
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902228gsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1200P)^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^)+(0.1200P)^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 
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_cod_original_sg_symbol_H-M      P-3c1
_cod_database_code               7027406