Syntheses, crystal structures and magnetic properties of two novel layered compounds: [Fe3(C2O4)3(4,4′-bpy)4] and [Co(C2O4)(4,4′-bpy)] (4,4′-bpy = 4,4′-bipyridine) †
Zheng, Li-Min; Fang, Xia; Lii, Kwang-Hwa; Song, Hui-Hua; Xin, Xin-Quan; Fun, Hoong-Kun; Chinnakali, Kandasamy; Razak, Ibrahim Abdul; Journal of the Chemical Society, Dalton Transactions  (1999) 2311–; doi:10.1039/a809738k

data_7027227
_publ_section_title
;
 Syntheses, crystal structures and magnetic properties of two novel
 layered compounds: [Fe3(C2O4)3(4,4&#x2032;-bpy)4] and
 [Co(C2O4)(4,4&#x2032;-bpy)]
 (4,4&#x2032;-bpy&#x2005;=&#x2005;4,4&#x2032;-bipyridine)&#x200A;&#x2020;
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2311
_journal_paper_doi               10.1039/a809738k
_journal_year                    1999
_chemical_formula_sum            'C46 H32 Fe3 N8 O12'
_chemical_formula_weight         1056.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.2776(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2475(2)
_cell_length_b                   15.9840(2)
_cell_length_c                   16.38560(10)
_cell_measurement_reflns_used    7444
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.03
_cell_volume                     4243.49(8)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXL (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL (Sheldrick, 1994)'
_computing_structure_solution    'SHELXL (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device
;
Siemens SMART CCD area detector diffractometer
;
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24362
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    1.090
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   'empirical using SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       trunk
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00022(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   1.023
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_obs          0.0493
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+1.9427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1127
_refine_ls_wR_factor_obs         0.0887
_reflns_number_observed          5422
_reflns_number_total             9195
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809738Ksup1.cif
_cod_data_source_block           z9801
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+1.9427P] 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^)+(0.0336P)^2^+1.9427P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027227