Four new NiII antiferromagnetic complexes with azido bridges
Montserrat Monfort; Inmaculada Resino; Joan Ribas; Xavier Solans; Mercé Font-Bardia; Helen Stoeckli-Evans; New J. Chem. 26 (2002) 1601–1606; doi:10.1039/b205404c

data_7050963
_publ_section_title
;
 Four new NiII antiferromagnetic complexes with azido bridges
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              1601
_journal_page_last               1606
_journal_paper_doi               10.1039/b205404c
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         trans-[Ni(N-Pren)2(mu1,3-N3)]n(ClO4)n
_chemical_formula_sum            'C10 H28 Cl N7 Ni O4'
_chemical_formula_weight         404.61
_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                 95.958(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3715(7)
_cell_length_b                   18.4000(12)
_cell_length_c                   12.2042(9)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.45
_cell_volume                     1869.7(2)
_computing_cell_refinement       'CELL (Stoe & Cie GmbH, Darmstadt, 1996)'
_computing_data_collection       'EXPOSE (Stoe & Cie GmbH, Darmstadt, 1996)'
_computing_data_reduction
'INTEGRATE (Stoe & Cie GmbH, Darmstadt, 1996)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.81
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'STOE Image Plate Diffraction system'
_diffrn_measurement_method       'Phi rotation'
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14522
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.8944
_exptl_absorpt_correction_T_min  0.6277
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale purple-blus'
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0013(5)
_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   0.801
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3628
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.813
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                1986
_reflns_number_total             3628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205404c.txt
_cod_data_source_block           for_Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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^)+(0.0510P)^2^+0.0000P] 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^)+(0.0510P)^2^+0.0000P] 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(1)/c'
_cod_database_code               7050963