Synthesis of N3−/SCN− bridged polynuclear complexes of nickel(II) using N,N,N'-trimethylethane-1,2-diamine as a blocking ligand: low temperature magnetic study and single crystal structure of [Ni(μ1,1-N3)(μ1,3-N3)(N,N,N'-Me3en)]n
Montserrat Monfort; Inmaculada Resino; Joan Ribas; Xavier Solans; Mercé Font-Bardia; New J. Chem. 25 (2001) 1577–1582; doi:10.1039/b105770g

data_7051207
_publ_section_title
;
 Synthesis of N3&#x2212;/SCN&#x2212; bridged polynuclear complexes of
 nickel(II) using N,N,N'-trimethylethane-1,2-diamine as a blocking
 ligand: low temperature magnetic study and single crystal structure of
 [Ni(\m1,1-N3)(\m1,3-N3)(N,N,N'-Me3en)]n
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              1577
_journal_page_last               1582
_journal_paper_doi               10.1039/b105770g
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C10 H28 F6 N5 Ni O2 P'
_chemical_formula_weight         454.05
_space_group_IT_number           29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.698(2)
_cell_length_b                   10.1097(14)
_cell_length_c                   15.698(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2015.2(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5326
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.108
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_F_000             944
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.0101(12)
_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_all   1.057
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2761
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.302
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_obs          0.0372
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+0.0256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1184
_refine_ls_wR_factor_obs         0.0945
_reflns_number_observed          2562
_reflns_number_total             2811
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b105770g.txt
_cod_data_source_block           ?Ni(NO2)(N,N,N'-Me3en)2?PF6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+0.0256P] 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^)+(0.0717P)^2^+0.0256P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7051207