#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006656.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006656
loop_
_publ_author_name
'Suzuki, H.'
'Ishiguro, S.-I.'
_publ_section_title
;
 Steric Hindrance in a Mixed Solvated Nickel(II) Complex:
 Bis(acetonitrile-<i>N</i>)tetrakis(<i>N</i>,<i>N</i>-dimethylacetamide-<i>O</i>)nickel(II)
 Bis(tetrafluoroborate)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1602
_journal_page_last               1605
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Ni(C2 H3  N)2 (C4 H9 N O)4 ] (B F4)2'
_chemical_formula_moiety         'C20 H42 N6 Ni O4,2(B F4)'
_chemical_formula_structural     '[Ni(C H3 C N)2((C H3)2N C O C H3)4](B F4)2'
_chemical_formula_sum            'C20 H42 B2 F8 N6 Ni O4'
_chemical_formula_weight         662.93
_chemical_name_systematic
;
bis(acetonitrile)tetrakis(N,N-dimethylacetamide)nickel(II) tetrafluoroborate
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.24(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.892(3)
_cell_length_b                   19.706(5)
_cell_length_c                   11.842(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      11
_cell_volume                     1603.9(9)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4880
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.459
_refine_diff_density_min         -0.663
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.152
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_hydrogen_treatment
'H atoms treated by a mixture of constrained and independent refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_obs          0.0614
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^) + (0.0731P)^2^ + 1.7845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.1825
_refine_ls_wR_factor_obs         0.1453
_reflns_number_observed          3256
_reflns_number_total             4678
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    de1060.cif
_[local]_cod_data_source_block   1
_cod_database_code               2006656
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_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni 0.0252(2) 0.0214(2) 0.0251(2) -0.0022(2) -0.0001(2) 0.0016(2)
O1 0.0394(12) 0.0258(10) 0.0309(11) 0.0013(9) -0.0011(9) 0.0062(8)
O2 0.0342(11) 0.0330(12) 0.0331(11) 0.0012(9) 0.0062(9) 0.0037(9)
N1 0.050(2) 0.0369(15) 0.0387(15) 0.0057(13) -0.0002(13) 0.0127(12)
N2 0.049(2) 0.050(2) 0.042(2) -0.0013(15) 0.0106(14) 0.0005(14)
N3 0.0300(13) 0.0325(13) 0.0356(13) -0.0040(10) -0.0015(10) 0.0004(11)
C11 0.0267(14) 0.0286(14) 0.038(2) -0.0002(11) -0.0018(11) 0.0060(12)
C12 0.055(2) 0.035(2) 0.046(2) 0.011(2) 0.001(2) -0.0017(15)
C13 0.067(3) 0.062(3) 0.034(2) 0.014(2) 0.004(2) 0.010(2)
C14 0.113(4) 0.041(2) 0.067(3) 0.016(3) -0.003(3) 0.024(2)
C21 0.0306(14) 0.039(2) 0.040(2) 0.0083(14) 0.0078(12) 0.0003(15)
C22 0.045(2) 0.052(2) 0.056(2) -0.015(2) 0.009(2) -0.004(2)
C23 0.057(2) 0.058(3) 0.055(2) -0.012(2) 0.001(2) -0.016(2)
C24 0.088(4) 0.077(3) 0.043(2) -0.003(3) 0.030(2) 0.005(2)
C31 0.034(2) 0.032(2) 0.037(2) -0.0016(13) -0.0025(13) -0.0010(13)
C32 0.053(2) 0.045(2) 0.076(3) -0.015(2) -0.011(2) -0.016(2)
B 0.047(3) 0.073(4) 0.065(3) 0.008(3) 0.006(2) 0.007(3)
F1 0.077(3) 0.228(6) 0.124(4) 0.010(3) -0.001(2) 0.013(4)
F21 0.24(2) 0.136(15) 0.104(13) 0.084(15) 0.106(13) 0.037(11)
F31 0.139(14) 0.20(2) 0.114(8) 0.137(15) -0.037(8) -0.012(11)
F41 0.148(11) 0.078(5) 0.111(7) 0.029(6) 0.003(7) -0.027(5)
F22 0.135(9) 0.082(7) 0.059(6) 0.025(6) -0.023(7) -0.005(5)
F32 0.161(11) 0.065(5) 0.084(6) 0.031(6) -0.003(6) 0.010(4)
F42 0.162(18) 0.19(2) 0.213(14) -0.137(16) -0.047(12) 0.024(13)
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Ni 0.0000 0.0000 0.0000 0.02402(15) Uani d S 1 . Ni
O1 0.0730(3) -0.06638(11) 0.1278(2) 0.0322(5) Uani d . 1 . O
O2 0.2141(3) -0.03382(11) -0.1021(2) 0.0332(5) Uani d . 1 . O
N1 0.1232(5) -0.15446(15) 0.2438(3) 0.0420(7) Uani d . 1 . N
N2 0.2566(5) -0.0271(2) -0.2868(3) 0.0464(7) Uani d . 1 . N
N3 0.1910(4) 0.06856(14) 0.0822(2) 0.0329(6) Uani d . 1 . N
C11 0.1079(4) -0.1286(2) 0.1401(3) 0.0313(6) Uani d . 1 . C
C12 0.1353(6) -0.1741(2) 0.0414(3) 0.0457(8) Uani d . 1 . C
H12A 0.022(2) -0.2039(11) 0.0288(16) 0.069 Uiso calc R 1 . H
H12B 0.253(3) -0.2016(11) 0.0571(11) 0.069 Uiso calc R 1 . H
H12C 0.149(5) -0.1464(2) -0.0264(6) 0.069 Uiso calc R 1 . H
C13 0.1024(7) -0.1118(2) 0.3429(3) 0.0544(10) Uani d . 1 . C
H13A 0.206(3) -0.1228(12) 0.4015(11) 0.082 Uiso calc R 1 . H
H13B -0.025(2) -0.1201(13) 0.3722(17) 0.082 Uiso calc R 1 . H
H13C 0.113(5) -0.0640(2) 0.3215(7) 0.082 Uiso calc R 1 . H
C14 0.1540(9) -0.2270(2) 0.2662(5) 0.074(2) Uani d . 1 . C
H14A 0.221(6) -0.2329(2) 0.3415(15) 0.111 Uiso calc R 1 . H
H14B 0.234(5) -0.2462(5) 0.209(2) 0.111 Uiso calc R 1 . H
H14C 0.0281(10) -0.2503(4) 0.263(4) 0.111 Uiso calc R 1 . H
C21 0.2869(5) -0.0040(2) -0.1824(3) 0.0362(6) Uani d . 1 . C
C22 0.4170(6) 0.0571(2) -0.1617(4) 0.0508(9) Uani d . 1 . C
H22A 0.3498(19) 0.0978(3) -0.192(2) 0.076 Uiso calc R 1 . H
H22B 0.537(2) 0.0506(7) -0.200(2) 0.076 Uiso calc R 1 . H
H22C 0.448(4) 0.0626(10) -0.0801(4) 0.076 Uiso calc R 1 . H
C23 0.1242(7) -0.0839(2) -0.3110(4) 0.0570(11) Uani d . 1 . C
H23A 0.181(2) -0.1151(9) -0.364(2) 0.086 Uiso calc R 1 . H
H23B -0.0004(18) -0.0668(3) -0.345(3) 0.086 Uiso calc R 1 . H
H23C 0.103(4) -0.1079(11) -0.2404(6) 0.086 Uiso calc R 1 . H
C24 0.3462(8) 0.0026(3) -0.3853(4) 0.0679(13) Uani d . 1 . C
H24A 0.2507(19) 0.0031(18) -0.4509(9) 0.102 Uiso calc R 1 . H
H24B 0.459(3) -0.0247(11) -0.403(2) 0.102 Uiso calc R 1 . H
H24C 0.388(5) 0.0491(7) -0.3673(12) 0.102 Uiso calc R 1 . H
C31 0.2904(5) 0.1086(2) 0.1219(3) 0.0346(7) Uani d . 1 . C
C32 0.4214(7) 0.1600(2) 0.1724(4) 0.0588(11) Uani d . 1 . C
H32A 0.443(4) 0.1518(11) 0.2540(6) 0.088 Uiso calc R 1 . H
H32B 0.364(2) 0.2051(3) 0.160(3) 0.088 Uiso calc R 1 . H
H32C 0.5460(19) 0.1579(12) 0.138(2) 0.088 Uiso calc R 1 . H
B 0.6355(8) -0.3148(3) 0.0187(5) 0.0619(13) Uani d . 1 . B
F1 0.4501(6) -0.3152(3) 0.0448(4) 0.144(2) Uani d . 1 . F
F21 0.671(4) -0.3149(14) -0.0884(17) 0.154(10) Uani d P 0.49(2) 1 F
F31 0.772(3) -0.3443(14) 0.0766(11) 0.154(10) Uani d P 0.49(2) 1 F
F41 0.635(3) -0.2450(5) 0.0552(10) 0.112(4) Uani d P 0.49(2) 1 F
F22 0.617(3) -0.3234(10) -0.0977(13) 0.094(5) Uani d P 0.51(2) 2 F
F32 0.672(3) -0.3802(5) 0.0692(10) 0.104(4) Uani d P 0.51(2) 2 F
F42 0.755(4) -0.2723(13) 0.0547(14) 0.190(11) Uani d P 0.51(2) 2 F
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 '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'
O O 0.0106 0.0060 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ni O1 . 3 180.0 no
O1 Ni O2 . . 94.54(9) yes
O1 Ni O2 . 3 85.46(9) yes
O1 Ni N3 . . 87.49(10) yes
O1 Ni N3 . 3 92.51(10) yes
O1 Ni O2 3 . 85.46(9) no
O1 Ni O2 3 3 94.54(9) no
O1 Ni N3 3 . 92.51(10) no
O1 Ni N3 3 3 87.49(10) no
O2 Ni O2 . 3 180.0 no
O2 Ni N3 . . 91.64(10) yes
O2 Ni N3 . 3 88.36(10) yes
O2 Ni N3 3 . 88.36(10) no
O2 Ni N3 3 3 91.64(10) no
N3 Ni N3 . 3 180.0 no
Ni O1 C11 . . 138.5(2) yes
Ni O2 C21 . . 129.1(2) yes
Ni N3 C31 . . 175.7(3) yes
C11 N1 C13 . . 121.2(3) no
C11 N1 C14 . . 122.8(3) no
C13 N1 C14 . . 115.9(3) no
C21 N2 C23 . . 120.1(3) no
C21 N2 C24 . . 123.7(4) no
C23 N2 C24 . . 116.2(4) no
O1 C11 N1 . . 118.9(3) no
O1 C11 C12 . . 121.8(3) no
N1 C11 C12 . . 119.2(3) no
O2 C21 N2 . . 120.3(3) no
O2 C21 C22 . . 121.1(3) no
N2 C21 C22 . . 118.5(3) no
N3 C31 C32 . . 179.1(4) no
F1 B F21 . . 118.4(14) no
F1 B F31 . . 123.9(13) no
F1 B F41 . . 85.0(8) no
F21 B F31 . . 109.7(15) no
F21 B F41 . . 107.3(14) no
F31 B F41 . . 107.2(11) no
F1 B F22 . . 102.2(10) no
F1 B F32 . . 92.1(8) no
F1 B F42 . . 123.5(16) no
F22 B F32 . . 107.7(11) no
F22 B F42 . . 116.0(12) no
F42 B F32 . . 112.1(10) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni O1 . 2.035(2) yes
Ni O2 . 2.085(2) yes
Ni N3 . 2.078(3) yes
Ni O1 3 2.035(2) no
Ni O2 3 2.085(2) no
Ni N3 3 2.078(3) no
O1 C11 . 1.256(4) no
O2 C21 . 1.253(4) no
N1 C11 . 1.326(4) no
N1 C13 . 1.459(5) no
N1 C14 . 1.466(5) no
N2 C21 . 1.320(5) no
N2 C23 . 1.458(5) no
N2 C24 . 1.480(5) no
N3 C31 . 1.124(4) no
C11 C12 . 1.496(5) no
C21 C22 . 1.511(5) no
C31 C32 . 1.457(5) no
B F1 . 1.337(7) no
B F21 . 1.31(2) no
B F22 . 1.39(2) no
B F31 . 1.264(10) no
B F32 . 1.435(11) no
B F41 . 1.441(11) no
B F42 . 1.228(12) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
C11 N3 3.432(4) 3 no
C12 O2 3.310(4) . no
C12 N3 3.322(5) 3 no
C12 F42 3.27(3) 1_455 no
C13 F21 3.45(3) 4_445 no
C22 O1 3.435(5) 3 no
C22 N3 3.388(5) . no
C23 F31 3.03(2) 4_444 no
C23 F32 3.405(17) 4_444 no
C24 F22 3.44(2) 2_654 no
C24 F32 3.171(12) 2_654 no
C24 F32 3.365(15) 4_544 no
C31 F41 3.471(12) 3_655 no
C32 F1 3.435(7) 2_655 no
C32 F21 3.26(3) 3_655 no
C32 F31 3.347(15) 2_655 no
C32 F41 3.172(13) 3_655 no
C32 F22 3.35(2) 3_655 no
C32 F32 3.269(13) 2_655 no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
_geom_torsion_publ_flag
Ni O1 C11 N1 . -169.9(2) yes
Ni O1 C11 C12 . 10.9(5) yes
Ni O2 C21 N2 . -113.4(3) yes
Ni O2 C21 C22 . 69.0(4) yes
O1 Ni O2 C21 . -159.4(3) no
O1 Ni O2 C21 3 20.6(3) no
O2 Ni O1 C11 . -48.1(3) no
O2 Ni O1 C11 3 131.9(3) no
N3 Ni O1 C11 . -139.5(3) no
N3 Ni O1 C11 3 40.5(3) no
N3 Ni O2 C21 . -71.8(3) no
N3 Ni O2 C21 3 108.2(3) no
C13 N1 C11 O1 . -0.7(5) no
C13 N1 C11 C12 . 178.5(4) no
C14 N1 C11 O1 . 176.9(4) no
C14 N1 C11 C12 . -3.9(6) no
C23 N2 C21 O2 . 5.4(5) no
C23 N2 C21 C22 . -176.9(4) no
C24 N2 C21 O2 . -176.3(4) no
C24 N2 C21 C22 . 1.3(6) no