Structural analysis and magnetic properties of the 1D [Fe(dca)2bipy(H2O)]·1/2H2O and the 3D [Ni(dca)2bipy] (dca = dicyanamide; bipy = 4,4'-bipyridine)
Susana Martín; M. Gotzone Barandika; J. M. Ezpeleta; Roberto Cortés; J. I. Ruiz de Larramendi; Luis Lezama; Teófilo Rojo; J. Chem. Soc., Dalton Trans.  (2002) 4275–4280; doi:10.1039/b206069h

data_7011939
_publ_section_title
;
 Structural analysis and magnetic properties of the 1D
 [Fe(dca)2bipy(H2O)]&#x00B7;1/2H2O and the 3D
 [Ni(dca)2bipy]&#x00A0;(dca = dicyanamide; bipy = 4,4'-bipyridine)
;
_journal_issue                   22
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4275
_journal_page_last               4280
_journal_paper_doi               10.1039/b206069h
_journal_year                    2002
_chemical_formula_sum            'C14 H11 Fe N8 O1.5'
_chemical_formula_weight         371.16
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   22.366(5)
_cell_length_b                   22.366(5)
_cell_length_c                   13.311(2)
_cell_measurement_temperature    293(2)
_cell_volume                     6659(2)
_computing_cell_refinement       'STOE IPDS software (STOE, 1998)'
_computing_data_collection       'STOE IPDS software (STOE, 1998)'
_computing_data_reduction        'JANA98 (Petricek & Dusek, 1998)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SIR97 (Altomare, Cascaramo, Giacovazzo, Guagliardi, Molitemi, Burla,
Polidori, Camalli & Spagna, 1997)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.7
_diffrn_measured_fraction_theta_full 0.494
_diffrn_measured_fraction_theta_max 0.494
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method
; 
image plate with oscillating crystal geometry
;
_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  0.1280
_diffrn_reflns_av_sigmaI/netI    0.1350
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20690
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.9388
_exptl_absorpt_correction_T_min  0.9060
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       0.00132(16)
_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_ref   0.648
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3143
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.648
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                1770
_reflns_number_total             3143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206069h.txt
_cod_data_source_block           rf
_cod_original_cell_volume        6658(2)
_cod_original_formula_sum        'C14 H11 Fe N8 O1.50'
_cod_database_code               7011939