Synthesis, structures and magnetic properties of Fe(ii) and Co(ii) thiocyanato coordination compounds: on the importance of the diamagnetic counterparts for structure determination.
Wöhlert, Susanne; Peters, Lars; Näther, Christian; Dalton transactions (Cambridge, England : 2003) 42 (2013) 10746–10758; doi:10.1039/c3dt51085a

data_7021735
_publ_section_title
;
 Synthesis, structures and magnetic properties of Fe(ii) and Co(ii)
 thiocyanato coordination compounds: on the importance of the diamagnetic
 counterparts for structure determination.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10746
_journal_page_last               10758
_journal_paper_doi               10.1039/c3dt51085a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C12 H16 Fe N6 O2 S2'
_chemical_formula_sum            'C12 H16 Fe N6 O2 S2'
_chemical_formula_weight         396.28
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.530(10)
_cell_angle_beta                 111.800(10)
_cell_angle_gamma                99.190(10)
_cell_formula_units_Z            1
_cell_length_a                   6.9323(5)
_cell_length_b                   8.1273(6)
_cell_length_c                   9.2839(6)
_cell_measurement_reflns_used    6806
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.59
_cell_volume                     436.96(8)
_computing_cell_refinement       'X-Area (Stoe, 2008)'
_computing_data_collection       'X-Area (Stoe, 2008)'
_computing_data_reduction        'X-Area (Stoe, 2008)'
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and Diamond (Brandenburg, 2011)
;
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'omega scan'
_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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6806
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  0.8706
_exptl_absorpt_correction_T_min  0.8078
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red32 (Stoe, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.1240
_exptl_crystal_size_mid          0.0964
_exptl_crystal_size_min          0.0854
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.0709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                1700
_reflns_number_total             1886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51085a.txt
_cod_data_source_block           woe6
_cod_original_cell_volume        436.96(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7021735