A Novel Mixed Macrocycle Complex of Nickel: Synthesis, Structure, and Redox Chemistry of [NiII([9]aneN3)([9]aneS3)](ClO4)2.CHCl3 ([9]aneN3 = 1,4,7-Triazacyclononane and [9]aneS3 = 1,4,7-Trithiacyclononane)
A. McAuley; S. Subramanian; M. J. Zaworotko; R. Atencio; Inorganic Chemistry 37 (1998) 4607–4610; doi:10.1021/ic980099z

data_4322990
_publ_section_title
;
 A Novel Mixed Macrocycle Complex of Nickel: Synthesis, Structure, and
 Redox Chemistry of [NiII([9]aneN3)([9]aneS3)](ClO4)2.CHCl3 ([9]aneN3 =
 1,4,7-Triazacyclononane and [9]aneS3 = 1,4,7-Trithiacyclononane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4607
_journal_page_last               4610
_journal_paper_doi               10.1021/ic980099z
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C13 H28 Cl5 N3 Ni O8 S3'
_chemical_formula_weight         686.52
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.2090(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3911(8)
_cell_length_b                   14.4430(9)
_cell_length_c                   13.6116(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2514.7(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15047
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.597
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_obs          0.0278
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+1.7319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0660
_refine_ls_wR_factor_obs         0.0624
_reflns_number_observed          4916
_reflns_number_total             5765
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980099z.cif
_cod_data_source_block           p21c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+1.7319P] 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^)+(0.0259P)^2^+1.7319P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322990