Directed synthesis of μ-1,3,5 bridged dicyanamides by thermal decomposition of μ-1,5 bridged precursor compounds.
Wriedt, Mario; Näther, Christian; Dalton transactions (Cambridge, England : 2003) 40 (2011) 886–898; doi:10.1039/c0dt00864h

data_7014446
_publ_section_title
;
 Directed synthesis of \m-1,3,5 bridged dicyanamides by thermal
 decomposition of \m-1,5 bridged precursor compounds.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              886
_journal_page_last               898
_journal_paper_doi               10.1039/c0dt00864h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C8 H4 Fe N8'
_chemical_formula_sum            'C8 H4 Fe N8'
_chemical_formula_weight         268.04
_chemical_name_systematic
;
catena[(\m2-dicyanamido-N,N'')-(\m3-dicyanamido-N,N',N'')-(pyridazine-N)-iron(II)]
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   23.235(2)
_cell_length_b                   7.4044(7)
_cell_length_c                   6.3484(4)
_cell_measurement_reflns_used    6920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      3.33
_cell_volume                     1092.19(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'Phi 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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6920
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         3.33
_diffrn_standards_decay_%        NONE
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.007(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_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.1841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                925
_reflns_number_total             1114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00864H.TXT
_cod_data_source_block           2-Fe
_cod_original_sg_symbol_H-M      'P nma'
_cod_database_code               7014446