#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:09:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180063 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/09/7050964.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050964
loop_
_publ_author_name
'Montserrat Monfort'
'Inmaculada Resino'
'Joan Ribas'
'Xavier Solans'
'Mercé Font-Bardia'
'Helen Stoeckli-Evans'
_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,N-Me2en)2(mu1,3-N3)]n(PF6)n'
_chemical_formula_sum            'C8 H24 F6 N7 Ni P'
_chemical_formula_weight         422.02
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                116.77(22)
_cell_angle_beta                 91.86(19)
_cell_angle_gamma                109.07(27)
_cell_formula_units_Z            1
_cell_length_a                   6.385(21)
_cell_length_b                   8.841(36)
_cell_length_c                   9.102(7)
_cell_measurement_temperature    293(2)
_cell_volume                     424(3)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1770
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    1.306
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_F_000             218
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.0000(142)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.984
_refine_ls_goodness_of_fit_obs   1.028
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.269
_refine_ls_restrained_S_obs      1.028
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_obs          0.0542
_refine_ls_shift/esd_max         -8.520
_refine_ls_shift/esd_mean        0.079
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0695P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1599
_refine_ls_wR_factor_obs         0.1262
_reflns_number_observed          1566
_reflns_number_total             1770
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b205404c.txt
_cod_data_source_block           for_compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0695P)^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^)+(0.0695P)^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_cell_volume        423.6(22)
_cod_database_code               7050964
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni 0.0000 0.0000 0.0000 0.0197(3) Uani 1 d S .
N1 N 0.1802(6) 0.2952(5) 0.1669(5) 0.0396(8) Uani 1 d . .
N2 N 0.0410(7) 0.0703(6) -0.1905(5) 0.0528(10) Uani 1 d . .
H1N H 0.1198(7) 0.0120(6) -0.2594(5) 0.649(67) Uiso 1 calc R .
H1NA H -0.0952(7) 0.0373(6) -0.2519(5) 0.649(67) Uiso 1 calc R .
N3 N 0.3034(6) -0.0506(6) -0.0197(5) 0.0482(9) Uani 1 d . .
N4 N 0.5000 0.0000 0.0000 0.0337(10) Uani 1 d S .
C1 C 0.1338(9) 0.3758(7) 0.0670(7) 0.0572(13) Uani 1 d . .
H1 H 0.2325(9) 0.5045(7) 0.1210(7) 0.649(67) Uiso 1 calc R .
H1A H -0.0219(9) 0.3674(7) 0.0612(7) 0.649(67) Uiso 1 calc R .
C2 C 0.1706(10) 0.2799(8) -0.1065(7) 0.0651(15) Uani 1 d . .
H2 H 0.3314(10) 0.3070(8) -0.1019(7) 0.649(67) Uiso 1 calc R .
H3A H 0.1203(10) 0.3254(8) -0.1743(7) 0.649(67) Uiso 1 calc R .
C3 C 0.0941(9) 0.3672(8) 0.3251(7) 0.0619(14) Uani 1 d . .
H3 H 0.1242(9) 0.3150(8) 0.3918(7) 0.649(67) Uiso 1 calc R .
H3A' H -0.0664(9) 0.3346(8) 0.2972(7) 0.649(67) Uiso 1 calc R .
H3B H 0.1691(9) 0.4983(8) 0.3879(7) 0.649(67) Uiso 1 calc R .
C4 C 0.4293(9) 0.3602(8) 0.2307(7) 0.0647(15) Uani 1 d . .
H4 H 0.4539(9) 0.3049(8) 0.2959(7) 0.649(67) Uiso 1 calc R .
H4A H 0.4913(9) 0.4911(8) 0.3000(7) 0.649(67) Uiso 1 calc R .
H4B H 0.5025(9) 0.3262(8) 0.1371(7) 0.649(67) Uiso 1 calc R .
P1 P 0.5000 0.0000 0.5000 0.0466(4) Uani 1 d S .
F1 F 0.2665(9) -0.1288(8) 0.4997(8) 0.146(2) Uani 1 d . .
F2 F 0.3755(9) 0.1406(7) 0.5140(6) 0.121(2) Uani 1 d . .
F3 F 0.4268(8) -0.1156(7) 0.3014(5) 0.114(2) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N2 180.0 . 2 ?
N2 Ni1 N3 90.0(2) . . ?
N2 Ni1 N3 90.0(2) 2 . ?
N2 Ni1 N3 90.0(2) . 2 ?
N2 Ni1 N3 90.0(2) 2 2 ?
N3 Ni1 N3 180.0 . 2 ?
N2 Ni1 N1 96.2(3) . 2 ?
N2 Ni1 N1 83.8(3) 2 2 ?
N3 Ni1 N1 86.7(4) . 2 ?
N3 Ni1 N1 93.3(4) 2 2 ?
N2 Ni1 N1 83.8(3) . . ?
N2 Ni1 N1 96.2(3) 2 . ?
N3 Ni1 N1 93.3(4) . . ?
N3 Ni1 N1 86.7(4) 2 . ?
N1 Ni1 N1 180.0 2 . ?
C1 N1 C4 111.6(4) . . ?
C1 N1 C3 108.9(4) . . ?
C4 N1 C3 103.0(5) . . ?
C1 N1 Ni1 103.6(4) . . ?
C4 N1 Ni1 116.5(5) . . ?
C3 N1 Ni1 113.2(4) . . ?
C2 N2 Ni1 107.9(4) . . ?
C2 N2 H1N 110.1(4) . . ?
Ni1 N2 H1N 110.1(2) . . ?
C2 N2 H1NA 110.1(4) . . ?
Ni1 N2 H1NA 110.1(2) . . ?
H1N N2 H1NA 108.4 . . ?
N4 N3 Ni1 151.4(4) . . ?
N3 N4 N3 180.0 2_655 . ?
N1 C1 C2 111.0(5) . . ?
N1 C1 H1 109.4(4) . . ?
C2 C1 H1 109.4(4) . . ?
N1 C1 H1A 109.4(3) . . ?
C2 C1 H1A 109.4(4) . . ?
H1 C1 H1A 108.0 . . ?
C1 C2 N2 111.7(5) . . ?
C1 C2 H2 109.3(4) . . ?
N2 C2 H2 109.3(4) . . ?
C1 C2 H3A 109.3(4) . . ?
N2 C2 H3A 109.3(4) . . ?
H2 C2 H3A 107.9 . . ?
N1 C3 H3 109.5(3) . . ?
N1 C3 H3A 109.5(4) . . ?
H3 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5(4) . . ?
H3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C4 H4 109.5(3) . . ?
N1 C4 H4A 109.5(4) . . ?
H4 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5(4) . . ?
H4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
F1 P1 F1 180.0 2_656 . ?
F1 P1 F3 94.1(5) 2_656 . ?
F1 P1 F3 85.9(5) . . ?
F1 P1 F3 85.9(5) 2_656 2_656 ?
F1 P1 F3 94.1(5) . 2_656 ?
F3 P1 F3 180.000(1) . 2_656 ?
F1 P1 F2 93.4(4) 2_656 . ?
F1 P1 F2 86.6(4) . . ?
F3 P1 F2 93.9(3) . . ?
F3 P1 F2 86.1(4) 2_656 . ?
F1 P1 F2 86.6(4) 2_656 2_656 ?
F1 P1 F2 93.4(4) . 2_656 ?
F3 P1 F2 86.1(4) . 2_656 ?
F3 P1 F2 93.9(3) 2_656 2_656 ?
F2 P1 F2 180.000(1) . 2_656 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.087(5) . ?
Ni1 N2 2.087(5) 2 ?
Ni1 N3 2.122(8) . ?
Ni1 N3 2.122(8) 2 ?
Ni1 N1 2.190(12) 2 ?
Ni1 N1 2.190(12) . ?
N1 C1 1.459(7) . ?
N1 C4 1.496(9) . ?
N1 C3 1.495(7) . ?
N2 C2 1.544(11) . ?
N2 H1N 0.90 . ?
N2 H1NA 0.90 . ?
N3 N4 1.164(6) . ?
N4 N3 1.164(6) 2_655 ?
C1 C2 1.489(8) . ?
C1 H1 0.97 . ?
C1 H1A 0.97 . ?
C2 H2 0.97 . ?
C2 H3A 0.97 . ?
C3 H3 0.96 . ?
C3 H3A 0.96 . ?
C3 H3B 0.96 . ?
C4 H4 0.96 . ?
C4 H4A 0.96 . ?
C4 H4B 0.96 . ?
P1 F1 1.551(8) 2_656 ?
P1 F1 1.551(8) . ?
P1 F3 1.581(6) . ?
P1 F3 1.581(6) 2_656 ?
P1 F2 1.644(8) . ?
P1 F2 1.644(8) 2_656 ?
