#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/73/4327385.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_4327385
loop_
_publ_author_name
'Hideki Ohtsu'
'Koji Tanaka'
_publ_section_title
;
 Equilibrium of Low- and High-Spin States of Ni(II) Complexes Controlled
 by the Donor Ability of the Bidentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3024
_journal_page_last               3030
_journal_paper_doi               10.1021/ic035486+
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C32 H41 N3 Ni O5'
_chemical_formula_weight         606.39
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 96.583(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.774(2)
_cell_length_b                   9.712(2)
_cell_length_c                   16.132(3)
_cell_measurement_reflns_used    5371
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1521.2(5)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.9637
_diffrn_measured_fraction_theta_max 0.9637
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11097
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Light Blue'
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     371
_refine_ls_number_reflns         3562
_refine_ls_R_factor_gt           0.034(>2.0sigma(I))
_refine_ls_shift/su_max          0.0150
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00063|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.048(>2.0sigma(I))
_reflns_number_gt                3460
_reflns_number_total             3568
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic0354862Bsi20031229_015759_3.cif
_cod_data_source_block           '[Ni(MePy(Bz)2)(tBuacac)(NO3)]'
_cod_original_cell_volume        1521.2(4)
_cod_original_formula_sum        'C32 H41 N3 O5 Ni '
_cod_database_code               4327385
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+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_calc_flag
Ni(1) Ni 0.77144(3) 0.4662(8) 0.20713(2) 0.01813(7) Uani 1.00 d
O(1) O 0.6717(2) 0.3039(8) 0.2445(1) 0.0217(4) Uani 1.00 d
O(2) O 0.5961(2) 0.5531(8) 0.1608(1) 0.0224(4) Uani 1.00 d
O(3) O 0.9546(2) 0.3475(8) 0.2239(1) 0.0265(4) Uani 1.00 d
O(4) O 0.8290(2) 0.3398(8) 0.1048(1) 0.0340(5) Uani 1.00 d
O(5) O 1.0155(3) 0.2137(8) 0.1251(2) 0.0553(8) Uani 1.00 d
N(1) N 0.8817(2) 0.6372(8) 0.1735(1) 0.0198(5) Uani 1.00 d
N(2) N 0.8148(2) 0.5625(8) 0.3297(1) 0.0194(4) Uani 1.00 d
N(3) N 0.9350(3) 0.2978(8) 0.1500(2) 0.0301(6) Uani 1.00 d
C(1) C 0.7934(3) 0.6379(9) 0.0249(2) 0.0339(7) Uani 1.00 d
C(2) C 0.8788(3) 0.7000(8) 0.0989(2) 0.0246(6) Uani 1.00 d
C(3) C 0.9527(3) 0.8220(8) 0.0911(2) 0.0306(6) Uani 1.00 d
C(4) C 1.0308(3) 0.8782(9) 0.1601(2) 0.0338(7) Uani 1.00 d
C(5) C 1.0337(3) 0.8122(9) 0.2366(2) 0.0281(6) Uani 1.00 d
C(6) C 0.9583(2) 0.6920(8) 0.2405(2) 0.0202(5) Uani 1.00 d
C(7) C 0.9561(2) 0.6124(8) 0.3206(1) 0.0215(5) Uani 1.00 d
C(8) C 0.5009(3) 0.5601(9) 0.3465(2) 0.0317(7) Uani 1.00 d
C(9) C 0.3680(3) 0.5571(9) 0.3717(2) 0.0406(8) Uani 1.00 d
C(10) C 0.3254(3) 0.6607(9) 0.4206(2) 0.0411(8) Uani 1.00 d
C(11) C 0.4112(3) 0.7679(9) 0.4452(2) 0.0393(8) Uani 1.00 d
C(12) C 0.5441(3) 0.7710(8) 0.4222(2) 0.0296(7) Uani 1.00 d
C(13) C 0.5914(3) 0.6680(8) 0.3718(2) 0.0253(6) Uani 1.00 d
C(14) C 0.7328(3) 0.6867(8) 0.3450(2) 0.0247(6) Uani 1.00 d
C(15) C 1.0314(2) 0.4754(9) 0.5043(1) 0.0260(5) Uani 1.00 d
C(16) C 1.1003(3) 0.5247(8) 0.5789(2) 0.0295(6) Uani 1.00 d
C(17) C 1.0317(3) 0.6019(9) 0.6331(2) 0.0291(6) Uani 1.00 d
C(18) C 0.8929(3) 0.6295(8) 0.6126(2) 0.0316(7) Uani 1.00 d
C(19) C 0.8240(3) 0.5818(9) 0.5381(2) 0.0277(6) Uani 1.00 d
C(20) C 0.8929(3) 0.5054(8) 0.4820(1) 0.0219(5) Uani 1.00 d
C(21) C 0.8215(2) 0.4573(8) 0.3983(1) 0.0207(5) Uani 1.00 d
C(22) C 0.3597(3) 0.0843(9) 0.2080(2) 0.0338(7) Uani 1.00 d
C(23) C 0.4996(3) 0.1478(9) 0.3423(2) 0.0330(7) Uani 1.00 d
C(24) C 0.6091(3) 0.0203(8) 0.2323(2) 0.0294(6) Uani 1.00 d
C(25) C 0.5026(3) 0.1305(8) 0.2477(2) 0.0243(5) Uani 1.00 d
C(26) C 0.5491(2) 0.2702(8) 0.2157(1) 0.0194(5) Uani 1.00 d
C(27) C 0.4578(3) 0.3521(8) 0.1640(2) 0.0233(6) Uani 1.00 d
C(28) C 0.4824(2) 0.4905(8) 0.1428(1) 0.0203(5) Uani 1.00 d
C(29) C 0.3675(3) 0.5740(8) 0.0935(2) 0.0259(6) Uani 1.00 d
C(30) C 0.3902(4) 0.7284(9) 0.1103(3) 0.0524(10) Uani 1.00 d
C(31) C 0.2249(3) 0.5348(9) 0.1152(2) 0.0391(8) Uani 1.00 d
C(32) C 0.3734(4) 0.5444(9) 0.0009(2) 0.0447(9) Uani 1.00 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Ni Ni 0.339 1.112
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(1) Ni(1) O(2) 91.10(8) yes
O(1) Ni(1) O(3) 88.1(1) yes
O(1) Ni(1) O(4) 87.8(1) yes
O(1) Ni(1) N(1) 177.23(9) yes
O(1) Ni(1) N(2) 96.67(9) yes
O(2) Ni(1) O(3) 164.22(9) yes
O(2) Ni(1) O(4) 103.99(9) yes
O(2) Ni(1) N(1) 90.7(1) yes
O(2) Ni(1) N(2) 103.20(10) yes
O(3) Ni(1) O(4) 60.23(9) yes
O(3) Ni(1) N(1) 90.70(9) yes
O(3) Ni(1) N(2) 92.55(9) yes
O(4) Ni(1) N(1) 93.75(10) yes
O(4) Ni(1) N(2) 152.34(10) yes
N(1) Ni(1) N(2) 80.9(1) yes
Ni(1) O(1) C(26) 124.5(2) yes
Ni(1) O(2) C(28) 125.3(2) yes
Ni(1) O(3) N(3) 93.0(2) yes
Ni(1) O(4) N(3) 90.6(2) yes
Ni(1) N(1) C(2) 129.4(2) yes
Ni(1) N(1) C(6) 111.2(2) yes
C(2) N(1) C(6) 119.3(3) yes
Ni(1) N(2) C(7) 97.9(2) yes
Ni(1) N(2) C(14) 116.5(2) yes
Ni(1) N(2) C(21) 111.3(2) yes
C(7) N(2) C(14) 106.1(2) yes
C(7) N(2) C(21) 109.3(2) yes
C(14) N(2) C(21) 114.2(2) yes
O(3) N(3) O(4) 116.2(3) yes
O(3) N(3) O(5) 121.4(3) yes
O(4) N(3) O(5) 122.4(3) yes
N(1) C(2) C(1) 118.8(3) yes
N(1) C(2) C(3) 120.3(3) yes
C(1) C(2) C(3) 120.8(3) yes
C(2) C(3) C(4) 120.2(3) yes
C(3) C(4) C(5) 119.0(3) yes
C(4) C(5) C(6) 118.2(3) yes
N(1) C(6) C(5) 122.9(3) yes
N(1) C(6) C(7) 115.0(2) yes
C(5) C(6) C(7) 122.0(3) yes
N(2) C(7) C(6) 110.9(2) yes
C(9) C(8) C(13) 120.3(3) yes
C(8) C(9) C(10) 120.2(4) yes
C(9) C(10) C(11) 120.6(3) yes
C(10) C(11) C(12) 120.0(3) yes
C(11) C(12) C(13) 121.3(3) yes
C(8) C(13) C(12) 117.7(3) yes
C(8) C(13) C(14) 125.2(3) yes
C(12) C(13) C(14) 117.1(3) yes
N(2) C(14) C(13) 118.7(2) yes
C(16) C(15) C(20) 120.7(3) yes
C(15) C(16) C(17) 120.7(3) yes
C(16) C(17) C(18) 119.1(3) yes
C(17) C(18) C(19) 120.5(3) yes
C(18) C(19) C(20) 121.0(3) yes
C(15) C(20) C(19) 118.0(3) yes
C(15) C(20) C(21) 119.9(3) yes
C(19) C(20) C(21) 122.1(3) yes
N(2) C(21) C(20) 114.9(3) yes
C(22) C(25) C(23) 109.1(3) yes
C(22) C(25) C(24) 109.3(3) yes
C(22) C(25) C(26) 114.0(3) yes
C(23) C(25) C(24) 109.1(3) yes
C(23) C(25) C(26) 106.1(2) yes
C(24) C(25) C(26) 109.2(2) yes
O(1) C(26) C(25) 113.9(2) yes
O(1) C(26) C(27) 125.4(3) yes
C(25) C(26) C(27) 120.6(3) yes
C(26) C(27) C(28) 124.8(3) yes
O(2) C(28) C(27) 124.6(3) yes
O(2) C(28) C(29) 115.8(2) yes
C(27) C(28) C(29) 119.6(2) yes
C(28) C(29) C(30) 110.1(3) yes
C(28) C(29) C(31) 112.6(3) yes
C(28) C(29) C(32) 107.5(3) yes
C(30) C(29) C(31) 108.7(3) yes
C(30) C(29) C(32) 109.6(3) yes
C(31) C(29) C(32) 108.4(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni(1) O(1) 1.983(2) yes
Ni(1) O(2) 1.979(2) yes
Ni(1) O(3) 2.120(2) yes
Ni(1) O(4) 2.182(3) yes
Ni(1) N(1) 2.086(3) yes
Ni(1) N(2) 2.184(2) yes
O(1) C(26) 1.277(3) yes
O(2) C(28) 1.271(3) yes
O(3) N(3) 1.279(4) yes
O(4) N(3) 1.265(4) yes
O(5) N(3) 1.233(4) yes
N(1) C(2) 1.346(4) yes
N(1) C(6) 1.351(4) yes
N(2) C(7) 1.487(3) yes
N(2) C(14) 1.484(4) yes
N(2) C(21) 1.503(4) yes
C(1) C(2) 1.503(4) yes
C(2) C(3) 1.401(4) yes
C(3) C(4) 1.387(5) yes
C(4) C(5) 1.388(5) yes
C(5) C(6) 1.386(4) yes
C(6) C(7) 1.508(4) yes
C(8) C(9) 1.406(4) yes
C(8) C(13) 1.401(5) yes
C(9) C(10) 1.372(6) yes
C(10) C(11) 1.367(6) yes
C(11) C(12) 1.392(5) yes
C(12) C(13) 1.400(4) yes
C(13) C(14) 1.506(4) yes
C(15) C(16) 1.395(4) yes
C(15) C(20) 1.391(4) yes
C(16) C(17) 1.383(5) yes
C(17) C(18) 1.386(5) yes
C(18) C(19) 1.388(4) yes
C(19) C(20) 1.401(4) yes
C(20) C(21) 1.520(4) yes
C(22) C(25) 1.536(4) yes
C(23) C(25) 1.538(4) yes
C(24) C(25) 1.534(4) yes
C(25) C(26) 1.539(4) yes
C(26) C(27) 1.398(4) yes
C(27) C(28) 1.414(4) yes
C(28) C(29) 1.532(4) yes
C(29) C(30) 1.535(5) yes
C(29) C(31) 1.524(4) yes
C(29) C(32) 1.529(5) yes
