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_4322883
_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_sum            'C8.33 H10.67 Cl0.67 N5.33 Ni0.67 O5.33'
_chemical_formula_weight         333.66
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            27
_cell_length_a                   17.373(3)
_cell_length_b                   17.373(3)
_cell_length_c                   33.235(6)
_cell_measurement_reflns_used    462
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.64
_cell_measurement_theta_min      13.73
_cell_volume                     8687(3)
_computing_cell_refinement       'SMART (Siemens, 1996a)'
_computing_data_collection       'SMART (Siemens, 1996a)'
_computing_data_reduction        'SAINT (Siemens, 1996b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1995)'
_computing_publication_material  'SHELXTL (Sheldrick, 1995)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1995)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1995)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Siemens SMART-CCD'
_diffrn_measurement_method       \w
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            25184
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.863022
_exptl_absorpt_correction_type   'multi-scans (SADABS)'
_exptl_absorpt_process_details   '(Sheldrick, G., 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         1706
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_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_obs          0.0404
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+69.7768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1269
_refine_ls_wR_factor_obs         0.1124
_reflns_number_observed          1467
_reflns_number_total             1714
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715761_5.cif
_cod_data_source_block           x271yn(7)
_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^)+(0.0564P)^2^+69.7768P] 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^)+(0.0564P)^2^+69.7768P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8685(5)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4322883