#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:16:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180255 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/41/7114158.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_7114158
loop_
_publ_author_name
'Barclay, Tosha M.'
'Hicks, Robin G.'
'Lemaire, Martin T.'
'Thompson, Laurence K.'
'Xu, Zhiqiang'
_publ_section_title
;
 Synthesis and coordination chemistry of a water-soluble verdazyl radical.
 structures and magnetic properties of M(H2O)2(vdCO2)2??2H2O (M = Co, Ni;
 vdCO2 = 1,5-dimethyl-6-oxo-verdazyl-3-carboxylate)
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1688
_journal_paper_doi               10.1039/b204851e
_journal_year                    2002
_chemical_formula_sum            'C10 H20 N8 Ni O10'
_chemical_formula_weight         471.05
_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-97
_cell_angle_alpha                85.450(3)
_cell_angle_beta                 84.058(3)
_cell_angle_gamma                79.127(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1957(18)
_cell_length_b                   9.4812(19)
_cell_length_c                   10.539(2)
_cell_measurement_temperature    293(2)
_cell_volume                     895.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6814
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.156
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             488
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0642P)²+0.1122P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                2369
_reflns_number_total             3146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204851e.txt
_cod_data_source_block           rhnicara
_cod_original_cell_volume        895.9(3)
_cod_database_code               7114158
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.75156(4) 0.62565(4) 0.87172(3) 0.03421(16) Uani 1 1 d .
O1 O 0.7597(3) 0.7762(2) 0.7253(2) 0.0534(6) Uani 1 1 d .
HO1A H 0.7386 0.7740 0.6477 0.080 Uiso 1 1 d R
HO1B H 0.7649 0.8639 0.7213 0.080 Uiso 1 1 d R
O2 O 0.7449(2) 0.4764(2) 1.02424(19) 0.0442(5) Uani 1 1 d .
HO2A H 0.7135 0.3954 1.0340 0.066 Uiso 1 1 d R
HO2B H 0.8068 0.4625 1.0776 0.066 Uiso 1 1 d R
O3 O 0.9758(2) 0.5615(2) 0.84215(19) 0.0425(5) Uani 1 1 d .
O4 O 1.1568(2) 0.4345(3) 0.7216(2) 0.0643(7) Uani 1 1 d .
O5 O 0.6067(2) 0.2837(3) 0.5260(2) 0.0538(6) Uani 1 1 d .
O6 O 0.5280(2) 0.6831(2) 0.9039(2) 0.0439(5) Uani 1 1 d .
O7 O 0.3431(2) 0.7926(3) 1.0310(2) 0.0548(6) Uani 1 1 d .
O8 O 0.8864(2) 0.9656(3) 1.2243(2) 0.0532(6) Uani 1 1 d .
O9 O 0.8009(3) 1.0464(2) 0.7542(2) 0.0563(6) Uani 1 1 d .
HO9A H 0.8862 1.0505 0.7632 0.084 Uiso 1 1 d R
HO9B H 0.7466 1.0839 0.8203 0.084 Uiso 1 1 d R
O10 O 0.6998(3) 0.7161(3) 0.4955(2) 0.0684(8) Uani 1 1 d .
HOA H 0.7638 0.6689 0.4368 0.103 Uiso 1 1 d R
HOB H 0.6039 0.7014 0.4730 0.103 Uiso 1 1 d R
N1 N 0.7684(2) 0.4697(2) 0.7339(2) 0.0325(5) Uani 1 1 d .
N2 N 0.9562(3) 0.3425(3) 0.5933(2) 0.0439(6) Uani 1 1 d .
N3 N 0.8482(3) 0.2967(3) 0.5373(2) 0.0440(7) Uani 1 1 d .
N4 N 0.6648(3) 0.4173(3) 0.6761(2) 0.0359(6) Uani 1 1 d .
N5 N 0.7288(3) 0.7844(2) 1.0095(2) 0.0333(5) Uani 1 1 d .
N6 N 0.5395(3) 0.9030(3) 1.1539(2) 0.0405(6) Uani 1 1 d .
N7 N 0.6464(3) 0.9468(3) 1.2131(2) 0.0402(6) Uani 1 1 d .
N8 N 0.8304(3) 0.8412(3) 1.0656(2) 0.0361(6) Uani 1 1 d .
C1 C 1.0253(3) 0.4781(3) 0.7547(3) 0.0398(7) Uani 1 1 d .
C2 C 0.9078(3) 0.4260(3) 0.6876(3) 0.0335(6) Uani 1 1 d .
C3 C 0.8977(4) 0.1997(4) 0.4355(4) 0.0718(12) Uani 1 1 d .
H3A H 1.0039 0.1873 0.4192 0.108 Uiso 1 1 calc R
H3B H 0.8523 0.2395 0.3594 0.108 Uiso 1 1 calc R
H3C H 0.8697 0.1083 0.4605 0.108 Uiso 1 1 calc R
C4 C 0.6997(3) 0.3298(3) 0.5765(3) 0.0383(7) Uani 1 1 d .
C5 C 0.5080(3) 0.4618(4) 0.7215(3) 0.0507(9) Uani 1 1 d .
H5A H 0.5003 0.5216 0.7921 0.076 Uiso 1 1 calc R
H5B H 0.4654 0.3782 0.7485 0.076 Uiso 1 1 calc R
H5C H 0.4555 0.5148 0.6535 0.076 Uiso 1 1 calc R
C6 C 0.4758(3) 0.7622(3) 0.9925(3) 0.0372(7) Uani 1 1 d .
C7 C 0.5888(3) 0.8226(3) 1.0574(3) 0.0334(6) Uani 1 1 d .
C8 C 0.5938(4) 1.0317(4) 1.3230(3) 0.0563(9) Uani 1 1 d .
H8A H 0.4879 1.0398 1.3389 0.084 Uiso 1 1 calc R
H8B H 0.6182 1.1259 1.3063 0.084 Uiso 1 1 calc R
H8C H 0.6404 0.9854 1.3966 0.084 Uiso 1 1 calc R
C10 C 0.9842(3) 0.8057(4) 1.0148(3) 0.0503(9) Uani 1 1 d .
H10A H 0.9911 0.7495 0.9418 0.075 Uiso 1 1 calc R
H10B H 1.0418 0.7513 1.0790 0.075 Uiso 1 1 calc R
H10C H 1.0216 0.8927 0.9897 0.075 Uiso 1 1 calc R
C9 C 0.7943(3) 0.9208(3) 1.1718(3) 0.0379(7) Uani 1 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
O1 Ni1 O6 92.00(9)
O1 Ni1 O3 89.72(9)
O6 Ni1 O3 178.13(8)
O1 Ni1 O2 178.36(8)
O6 Ni1 O2 88.21(9)
O3 Ni1 O2 90.09(8)
O1 Ni1 N1 88.06(9)
O6 Ni1 N1 100.91(8)
O3 Ni1 N1 78.40(8)
O2 Ni1 N1 93.50(9)
O1 Ni1 N5 91.57(9)
O6 Ni1 N5 77.68(8)
O3 Ni1 N5 103.02(8)
O2 Ni1 N5 86.88(9)
N1 Ni1 N5 178.53(8)
C1 O3 Ni1 118.02(17)
C6 O6 Ni1 118.86(18)
C2 N1 N4 114.7(2)
C2 N1 Ni1 111.99(17)
N4 N1 Ni1 132.98(18)
C2 N2 N3 114.8(2)
N2 N3 C4 124.0(2)
N2 N3 C3 116.4(3)
C4 N3 C3 119.4(3)
C4 N4 N1 123.4(2)
C4 N4 C5 118.6(2)
N1 N4 C5 117.9(2)
C7 N5 N8 115.1(2)
C7 N5 Ni1 112.02(17)
N8 N5 Ni1 132.51(18)
C7 N6 N7 115.1(2)
N6 N7 C9 124.1(2)
N6 N7 C8 115.7(2)
C9 N7 C8 120.1(2)
N5 N8 C9 123.1(2)
N5 N8 C10 117.2(2)
C9 N8 C10 119.5(2)
O4 C1 O3 125.9(3)
O4 C1 C2 118.7(3)
O3 C1 C2 115.3(2)
N2 C2 N1 128.0(3)
N2 C2 C1 116.6(3)
N1 C2 C1 115.4(2)
O5 C4 N4 122.9(3)
O5 C4 N3 122.1(3)
N4 C4 N3 115.0(2)
O7 C6 O6 125.4(3)
O7 C6 C7 119.0(3)
O6 C6 C7 115.6(2)
N6 C7 N5 127.4(3)
N6 C7 C6 117.7(2)
N5 C7 C6 114.8(2)
O8 C9 N7 122.5(3)
O8 C9 N8 122.7(3)
N7 C9 N8 114.8(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 O1 2.023(2)
Ni1 O6 2.025(2)
Ni1 O3 2.035(2)
Ni1 O2 2.060(2)
Ni1 N1 2.127(2)
Ni1 N5 2.141(2)
O3 C1 1.255(3)
O4 C1 1.225(4)
O5 C4 1.216(3)
O6 C6 1.244(3)
O7 C6 1.233(4)
O8 C9 1.213(3)
N1 C2 1.325(4)
N1 N4 1.369(3)
N2 C2 1.309(4)
N2 N3 1.360(3)
N3 C4 1.369(4)
N3 C3 1.450(4)
N4 C4 1.365(4)
N4 C5 1.464(4)
N5 C7 1.327(4)
N5 N8 1.367(3)
N6 C7 1.311(4)
N6 N7 1.361(3)
N7 C9 1.366(4)
N7 C8 1.453(4)
N8 C9 1.377(4)
N8 C10 1.446(4)
C1 C2 1.525(4)
C6 C7 1.519(4)
