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_7021736
_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         'C14 H20 Co N6 O2 S2'
_chemical_formula_sum            'C14 H20 Co N6 O2 S2'
_chemical_formula_weight         427.41
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.909(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3778(7)
_cell_length_b                   10.1202(5)
_cell_length_c                   14.0457(16)
_cell_measurement_reflns_used    6618
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      2.51
_cell_volume                     1008.55(16)
_computing_cell_refinement       '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      170(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'phi 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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6618
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.9279
_exptl_absorpt_correction_T_min  0.8566
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red32 (Stoe, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             442
_exptl_crystal_size_max          0.0893
_exptl_crystal_size_mid          0.0615
_exptl_crystal_size_min          0.0549
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.022(4)
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0638P)^2^+1.8372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                1872
_reflns_number_total             2412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51085a.txt
_cod_data_source_block           woe31a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7021736