#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:29:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179330 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/27/4322773.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_4322773
loop_
_publ_author_name
'Victor I. Ovcharenko'
'Sergei V. Fokin'
'Vladimir A. Reznikov'
'Vladimir N. Ikorskii'
'Galina V. Romanenko'
'Renad Z. Sagdeev'
_publ_section_title
;
 Nonclassical Packing of Metal Dioximates. Superexchange through a
 Diamagnetic Metal Cation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2104
_journal_page_last               2105
_journal_paper_doi               10.1021/ic971523j
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C16 H26 N6 Ni O6'
_chemical_formula_weight         457.14
_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                 108.922(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0667(11)
_cell_length_b                   11.3119(14)
_cell_length_c                   11.8628(14)
_cell_measurement_temperature    293(2)
_cell_volume                     1024.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.0483
_diffrn_reflns_av_sigmaI/netI    0.1642
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1952
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.993
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             480
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0007(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         1818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+0.8576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                919
_reflns_number_total             1818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic971523j_1.cif
_cod_data_source_block           f66
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.8576P] 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^)+(0.0000P)^2^+0.8576P] 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               4322773
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.0000 0.5000 0.0000 0.0282(3) Uani 1 d S . .
N3 N -0.1728(5) 0.4053(3) 0.0309(3) 0.0274(10) Uani 1 d . . .
O31 O -0.3436(4) 0.4318(3) 0.0005(3) 0.0385(10) Uani 1 d . . .
C4 C -0.1086(6) 0.3128(4) 0.0922(4) 0.0269(12) Uani 1 d . . .
C3 C -0.1865(7) 0.2160(5) 0.1469(5) 0.0303(15) Uani 1 d . . .
C31 C -0.3274(10) 0.1473(7) 0.0558(7) 0.056(2) Uani 1 d . . .
H311 H -0.423(6) 0.190(4) 0.029(4) 0.05(2) Uiso 1 d . . .
H312 H -0.297(6) 0.121(5) -0.017(5) 0.06(2) Uiso 1 d . . .
H313 H -0.357(7) 0.088(5) 0.088(5) 0.06(2) Uiso 1 d . . .
C32 C -0.2487(11) 0.2610(8) 0.2469(8) 0.051(2) Uani 1 d . . .
H321 H -0.274(7) 0.195(5) 0.289(5) 0.07(2) Uiso 1 d . . .
H322 H -0.166(8) 0.294(5) 0.305(5) 0.05(2) Uiso 1 d . . .
H323 H -0.350(7) 0.316(4) 0.221(4) 0.040(16) Uiso 1 d . . .
N2 N -0.0260(6) 0.1410(4) 0.1965(4) 0.0456(12) Uani 1 d . . .
O21 O -0.0332(5) 0.0442(3) 0.2483(4) 0.0759(14) Uani 1 d . . .
C2 C 0.1434(8) 0.1891(5) 0.1929(6) 0.0361(16) Uani 1 d . . .
C21 C 0.2281(12) 0.1016(7) 0.1315(10) 0.074(3) Uani 1 d . . .
H211 H 0.330(7) 0.142(5) 0.124(5) 0.07(2) Uiso 1 d . . .
H212 H 0.156(8) 0.073(5) 0.066(5) 0.08(3) Uiso 1 d . . .
H213 H 0.268(8) 0.023(8) 0.194(6) 0.15(3) Uiso 1 d . . .
C22 C 0.2669(12) 0.2146(11) 0.3171(8) 0.081(3) Uani 1 d . . .
H221 H 0.291(9) 0.140(7) 0.370(6) 0.13(3) Uiso 1 d . . .
H222 H 0.207(10) 0.255(6) 0.351(6) 0.07(3) Uiso 1 d . . .
H223 H 0.375(7) 0.260(4) 0.311(4) 0.061(18) Uiso 1 d . . .
C1 C 0.0807(6) 0.2972(4) 0.1210(4) 0.0263(12) Uani 1 d . . .
N1 N 0.1553(5) 0.3816(4) 0.0820(3) 0.0291(10) Uani 1 d . . .
O11 O 0.3292(4) 0.3808(3) 0.1049(3) 0.0390(10) Uani 1 d . . .
H11 H 0.351(8) 0.454(6) 0.063(5) 0.10(3) Uiso 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'
O O 0.0106 0.0060 '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
N1 Ni N1 180.0 . 3_565 ?
N1 Ni N3 84.55(17) . . ?
N1 Ni N3 95.45(17) 3_565 . ?
N1 Ni N3 95.45(17) . 3_565 ?
N1 Ni N3 84.55(17) 3_565 3_565 ?
N3 Ni N3 180.0 . 3_565 ?
C4 N3 O31 121.6(4) . . ?
C4 N3 Ni 112.7(3) . . ?
O31 N3 Ni 125.5(3) . . ?
N3 C4 C1 115.4(5) . . ?
N3 C4 C3 133.4(5) . . ?
C1 C4 C3 111.1(4) . . ?
N2 C3 C31 110.2(5) . . ?
N2 C3 C4 98.7(4) . . ?
C31 C3 C4 112.9(5) . . ?
N2 C3 C32 110.2(5) . . ?
C31 C3 C32 111.7(6) . . ?
C4 C3 C32 112.4(5) . . ?
C3 C31 H311 110(3) . . ?
C3 C31 H312 115(3) . . ?
H311 C31 H312 107(5) . . ?
C3 C31 H313 110(4) . . ?
H311 C31 H313 105(5) . . ?
H312 C31 H313 109(5) . . ?
C3 C32 H321 109(3) . . ?
C3 C32 H322 113(4) . . ?
H321 C32 H322 99(5) . . ?
C3 C32 H323 115(3) . . ?
H321 C32 H323 111(4) . . ?
H322 C32 H323 109(5) . . ?
O21 N2 C2 121.2(4) . . ?
O21 N2 C3 120.7(4) . . ?
C2 N2 C3 117.9(4) . . ?
C1 C2 N2 100.0(4) . . ?
C1 C2 C22 113.4(7) . . ?
N2 C2 C22 111.3(5) . . ?
C1 C2 C21 112.7(5) . . ?
N2 C2 C21 109.7(5) . . ?
C22 C2 C21 109.6(7) . . ?
C2 C21 H211 106(3) . . ?
C2 C21 H212 113(4) . . ?
H211 C21 H212 115(6) . . ?
C2 C21 H213 106(4) . . ?
H211 C21 H213 111(5) . . ?
H212 C21 H213 105(6) . . ?
C2 C22 H221 111(4) . . ?
C2 C22 H222 105(5) . . ?
H221 C22 H222 101(6) . . ?
C2 C22 H223 109(3) . . ?
H221 C22 H223 117(5) . . ?
H222 C22 H223 113(7) . . ?
N1 C1 C4 113.5(4) . . ?
N1 C1 C2 134.7(5) . . ?
C4 C1 C2 111.7(5) . . ?
C1 N1 O11 120.1(4) . . ?
C1 N1 Ni 113.8(3) . . ?
O11 N1 Ni 126.1(3) . . ?
N1 O11 H11 103(4) . . ?
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
Ni N1 1.876(4) . ?
Ni N1 1.876(4) 3_565 ?
Ni N3 1.886(4) . ?
Ni N3 1.886(4) 3_565 ?
N3 C4 1.283(5) . ?
N3 O31 1.340(4) . ?
C4 C1 1.464(6) . ?
C4 C3 1.510(7) . ?
C3 N2 1.499(6) . ?
C3 C31 1.505(8) . ?
C3 C32 1.518(8) . ?
C31 H311 0.88(4) . ?
C31 H312 1.01(5) . ?
C31 H313 0.85(5) . ?
C32 H321 0.96(5) . ?
C32 H322 0.87(5) . ?
C32 H323 0.99(5) . ?
N2 O21 1.266(5) . ?
N2 C2 1.485(7) . ?
C2 C1 1.482(7) . ?
C2 C22 1.515(10) . ?
C2 C21 1.516(9) . ?
C21 H211 0.97(6) . ?
C21 H212 0.87(5) . ?
C21 H213 1.14(8) . ?
C22 H221 1.03(7) . ?
C22 H222 0.85(6) . ?
C22 H223 1.03(5) . ?
C1 N1 1.292(5) . ?
N1 O11 1.340(5) . ?
O11 H11 1.01(7) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O11 H11 O31 1.01(7) 1.49(7) 2.483(5) 168(6) 3_565
