Spiral Dinuclear Complexes of Tetradentate N4 Diazine Ligands with Mn(II), Fe(II), Fe(III), Co(III), and Ni(II) Salts
Zhiqiang Xu; Laurence K. Thompson; David O. Miller; Howard J. Clase; Judith A. K. Howard; Andrés E. Goeta; Inorganic Chemistry 37 (1998) 3620–3627; doi:10.1021/ic9715761

data_4322882
_publ_section_title
;
 Spiral Dinuclear Complexes of Tetradentate N4 Diazine Ligands with
 Mn(II), Fe(II), Fe(III), Co(III), and Ni(II) Salts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3620
_journal_page_last               3627
_journal_paper_doi               10.1021/ic9715761
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         '[Fe2 (C10 H10 N8)3]4+, 4(N O3), 5(H2 O)'
_chemical_formula_sum            'C60 H80 Fe4 N56 O34'
_chemical_formula_weight         2353.20
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 96.852(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   14.039(3)
_cell_length_b                   11.335(6)
_cell_length_c                   14.6517(15)
_cell_measurement_reflns_used    13
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      33.42
_cell_measurement_theta_min      27.64
_cell_volume                     2314.9(13)
_computing_cell_refinement       'Texray (MSC 1985)'
_computing_data_collection       'Texray (MSC 1985)'
_computing_data_reduction        'Texray (MSC 1985)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC6S 4 circle'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4102
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+2.1411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                3153
_reflns_number_total             4102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9715761_4.cif
_cod_data_source_block           x554a(5)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+2.1411P] 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^)+(0.0600P)^2^+2.1411P] 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      'P 2/n'
_cod_database_code               4322882