#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/26/4322684.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_4322684
loop_
_publ_author_name
'Takeichiro Koga'
'Hideki Furutachi'
'Takako Nakamura'
'Nobuo Fukita'
'Masaaki Ohba'
'Kazuhiro Takahashi'
'Hisashi Ōkawa'
_publ_section_title
;
 Dinuclear Nickel(II) Complexes of Phenol-Based "End-Off" Compartmental
 Ligands and Their Urea Adducts Relevant to the Urease Active Site
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              989
_journal_page_last               996
_journal_paper_doi               10.1021/ic971209p
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C46 H57 B N4 Ni2 O6'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Mon Aug 25 19:59:24 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                99.90(2)
_cell_angle_beta                 104.16(2)
_cell_angle_gamma                109.01(2)
_cell_formula_units_Z            2.00
_cell_length_a                   13.613(3)
_cell_length_b                   16.475(4)
_cell_length_c                   11.307(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      29.33
_cell_volume                     2235.4(12)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_diffrn_ambient_temperature      20.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.07548
_diffrn_orient_matrix_UB_12      -0.01929
_diffrn_orient_matrix_UB_13      0.00714
_diffrn_orient_matrix_UB_21      0.03202
_diffrn_orient_matrix_UB_22      0.02774
_diffrn_orient_matrix_UB_23      0.09375
_diffrn_orient_matrix_UB_31      -0.00406
_diffrn_orient_matrix_UB_32      0.05758
_diffrn_orient_matrix_UB_33      -0.01259
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  2.30
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7878
_diffrn_reflns_theta_max         25.0016
_diffrn_standards_decay_%        -7.22
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 8.934
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             940.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         -0.98800
_refine_diff_density_min         1.00330
_refine_ls_extinction_coef       2.39820
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   3.080
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         5266
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0550
_refine_ls_shift/esd_max         0.1900
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0470
_cod_data_source_file            ic971209p_1.cif
_cod_data_source_block           '[Ni2(L1)(AcO)2(MeOH)](BPh4)(complex2)'
_cod_original_cell_volume        2235(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C46 H57 N4 O6 B Ni2'
_cod_database_code               4322684
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   -y,   -z'
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_calc_attached_atom
Ni1 -0.17321(5) -0.35323(4) -0.11235(6) 0.0468(2) Uij ? ?
Ni2 0.09344(5) -0.23339(4) 0.01930(6) 0.0439(2) Uij ? ?
O1 -0.0497(2) -0.2404(2) -0.1019(3) 0.048(1) Uij ? ?
O2 -0.1074(3) -0.4405(2) -0.1564(3) 0.053(1) Uij ? ?
O3 0.0661(3) -0.3637(2) -0.0289(3) 0.049(1) Uij ? ?
O4 -0.1439(3) -0.3329(2) 0.0722(3) 0.054(1) Uij ? ?
O5 0.0293(3) -0.2353(2) 0.1643(3) 0.058(1) Uij ? ?
O6 0.1532(3) -0.2317(2) -0.1513(3) 0.064(1) Uij ? ?
N1 -0.2491(3) -0.3571(3) -0.2882(4) 0.057(1) Uij ? ?
N2 -0.3267(3) -0.4580(3) -0.1414(4) 0.058(2) Uij ? ?
N3 0.1519(3) -0.1001(3) 0.0589(4) 0.055(1) Uij ? ?
N4 0.2490(3) -0.2047(3) 0.1554(4) 0.055(1) Uij ? ?
C1 -0.0547(4) -0.1825(3) -0.1694(5) 0.047(2) Uij ? ?
C2 -0.1378(4) -0.2071(3) -0.2869(5) 0.052(2) Uij ? ?
C3 -0.1435(5) -0.1433(4) -0.3541(5) 0.062(2) Uij ? ?
C4 -0.0717(5) -0.0558(4) -0.3091(6) 0.062(2) Uij ? ?
C5 0.0088(4) -0.0319(3) -0.1951(6) 0.060(2) Uij ? ?
C6 0.0216(4) -0.0919(3) -0.1243(5) 0.050(2) Uij ? ?
C7 -0.2263(5) -0.2944(4) -0.3423(5) 0.061(2) Uij ? ?
C8 -0.3520(5) -0.4368(4) -0.3524(6) 0.084(2) Uij ? ?
C9 -0.3664(7) -0.4972(6) -0.2732(8) 0.157(4) Uij ? ?
C10 -0.3144(6) -0.5285(5) -0.0816(9) 0.126(3) Uij ? ?
C11 -0.3999(5) -0.4270(4) -0.0929(7) 0.092(3) Uij ? ?
C12 -0.0828(5) 0.0121(4) -0.3808(6) 0.087(3) Uij ? ?
C13 0.1157(4) -0.0563(3) -0.0102(5) 0.060(2) Uij ? ?
C14 0.2542(5) -0.0537(4) 0.1642(6) 0.074(2) Uij ? ?
C15 0.2817(7) -0.1151(5) 0.228(1) 0.217(5) Uij ? ?
C16 0.3259(6) -0.2143(8) 0.1001(7) 0.193(5) Uij ? ?
C17 0.2469(5) -0.2564(6) 0.2451(6) 0.116(3) Uij ? ?
C18 -0.0090(4) -0.4307(3) -0.1106(5) 0.044(2) Uij ? ?
C19 0.0215(4) -0.5072(3) -0.1597(5) 0.059(2) Uij ? ?
C20 -0.0625(5) -0.2820(3) 0.1663(5) 0.051(2) Uij ? ?
C21 -0.0776(5) -0.2780(4) 0.2949(6) 0.083(2) Uij ? ?
C22 0.0953(6) -0.2993(5) -0.2705(6) 0.093(3) Uij ? ?
C23 0.4663(4) 0.2127(3) 0.1797(4) 0.044(2) Uij ? ?
C24 0.3573(4) 0.1944(3) 0.1698(4) 0.046(2) Uij ? ?
C25 0.2787(4) 0.1859(3) 0.0585(5) 0.055(2) Uij ? ?
C26 0.3064(5) 0.1937(4) -0.0494(5) 0.062(2) Uij ? ?
C27 0.4128(5) 0.2114(4) -0.0439(5) 0.070(2) Uij ? ?
C28 0.4904(4) 0.2197(4) 0.0670(5) 0.063(2) Uij ? ?
C29 0.6516(4) 0.3337(3) 0.3574(4) 0.044(2) Uij ? ?
C30 0.6550(5) 0.3931(4) 0.2829(5) 0.069(2) Uij ? ?
C31 0.7327(6) 0.4797(4) 0.3216(6) 0.089(2) Uij ? ?
C32 0.8109(6) 0.5124(4) 0.4370(6) 0.086(2) Uij ? ?
C33 0.8091(5) 0.4575(4) 0.5155(5) 0.089(2) Uij ? ?
C34 0.7306(5) 0.3717(4) 0.4762(5) 0.068(2) Uij ? ?
C35 0.6286(4) 0.1605(3) 0.2879(5) 0.045(2) Uij ? ?
C36 0.7204(5) 0.1663(4) 0.3817(5) 0.061(2) Uij ? ?
C37 0.7730(5) 0.1074(4) 0.3691(6) 0.069(2) Uij ? ?
C38 0.7363(5) 0.0397(4) 0.2605(6) 0.068(2) Uij ? ?
C39 0.6460(6) 0.0303(4) 0.1674(6) 0.081(2) Uij ? ?
C40 0.5940(5) 0.0902(4) 0.1805(5) 0.071(2) Uij ? ?
C41 0.5083(4) 0.2043(3) 0.4205(4) 0.045(2) Uij ? ?
C42 0.4877(4) 0.2663(3) 0.5022(5) 0.053(2) Uij ? ?
C43 0.4357(5) 0.2442(4) 0.5909(5) 0.062(2) Uij ? ?
C44 0.4021(5) 0.1576(4) 0.5997(5) 0.066(2) Uij ? ?
C45 0.4205(5) 0.0944(4) 0.5226(5) 0.064(2) Uij ? ?
C46 0.4728(4) 0.1179(3) 0.4355(5) 0.053(2) Uij ? ?
B 0.5635(5) 0.2284(4) 0.3106(5) 0.044(2) Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 92 0.003 0.002 'International Tables'
H 0 114 0.000 0.000 'International Tables'
N 0 8 0.006 0.003 'International Tables'
O 0 12 0.011 0.006 'International Tables'
B 0 2 0.001 0.001 'International Tables'
Ni 0 4 0.339 1.112 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) Ni(1) O(2) 98.8(1) ? ? ? yes
O(1) Ni(1) O(4) 96.2(1) ? ? ? yes
O(1) Ni(1) N(1) 89.2(2) ? ? ? yes
O(1) Ni(1) N(2) 167.1(2) ? ? ? yes
O(2) Ni(1) O(4) 103.9(1) ? ? ? yes
O(2) Ni(1) N(1) 97.3(2) ? ? ? yes
O(2) Ni(1) N(2) 91.5(2) ? ? ? yes
O(4) Ni(1) N(1) 157.0(2) ? ? ? yes
O(4) Ni(1) N(2) 88.7(2) ? ? ? yes
N(1) Ni(1) N(2) 81.8(2) ? ? ? yes
O(1) Ni(2) O(3) 97.8(1) ? ? ? yes
O(1) Ni(2) O(5) 91.1(1) ? ? ? yes
O(1) Ni(2) O(6) 84.8(1) ? ? ? yes
O(1) Ni(2) N(3) 89.8(2) ? ? ? yes
O(1) Ni(2) N(4) 171.3(2) ? ? ? yes
O(3) Ni(2) O(5) 96.8(1) ? ? ? yes
O(3) Ni(2) O(6) 83.9(1) ? ? ? yes
O(3) Ni(2) N(3) 167.2(2) ? ? ? yes
O(3) Ni(2) N(4) 90.9(1) ? ? ? yes
O(5) Ni(2) O(6) 175.9(1) ? ? ? yes
O(5) Ni(2) N(3) 93.3(2) ? ? ? yes
O(5) Ni(2) N(4) 87.8(2) ? ? ? yes
O(6) Ni(2) N(3) 86.6(2) ? ? ? yes
O(6) Ni(2) N(4) 96.3(2) ? ? ? yes
N(3) Ni(2) N(4) 81.6(2) ? ? ? yes
Ni(1) O(1) Ni(2) 109.1(1) ? ? ? yes
Ni(1) O(1) C(1) 127.3(3) ? ? ? yes
Ni(2) O(1) C(1) 123.4(3) ? ? ? yes
Ni(1) O(2) C(18) 126.5(3) ? ? ? yes
Ni(2) O(3) C(18) 133.7(3) ? ? ? yes
Ni(1) O(4) C(20) 132.8(4) ? ? ? yes
Ni(2) O(5) C(20) 130.5(3) ? ? ? yes
Ni(2) O(6) C(22) 122.7(3) ? ? ? yes
Ni(1) N(1) C(7) 127.0(4) ? ? ? yes
Ni(1) N(1) C(8) 113.7(4) ? ? ? yes
C(7) N(1) C(8) 118.6(5) ? ? ? yes
Ni(1) N(2) C(9) 103.6(4) ? ? ? yes
Ni(1) N(2) C(10) 112.9(4) ? ? ? yes
Ni(1) N(2) C(11) 113.0(3) ? ? ? yes
C(9) N(2) C(10) 106.5(6) ? ? ? yes
C(9) N(2) C(11) 114.2(6) ? ? ? yes
C(10) N(2) C(11) 106.5(5) ? ? ? yes
Ni(2) N(3) C(13) 124.9(4) ? ? ? yes
Ni(2) N(3) C(14) 115.0(3) ? ? ? yes
C(13) N(3) C(14) 119.3(5) ? ? ? yes
Ni(2) N(4) C(15) 104.6(4) ? ? ? yes
Ni(2) N(4) C(16) 112.9(4) ? ? ? yes
Ni(2) N(4) C(17) 115.5(4) ? ? ? yes
C(15) N(4) C(16) 111.6(7) ? ? ? yes
C(15) N(4) C(17) 105.4(7) ? ? ? yes
C(16) N(4) C(17) 106.7(6) ? ? ? yes
O(1) C(1) C(2) 121.5(5) ? ? ? yes
O(1) C(1) C(6) 121.4(5) ? ? ? yes
C(2) C(1) C(6) 117.0(5) ? ? ? yes
C(1) C(2) C(3) 120.2(5) ? ? ? yes
C(1) C(2) C(7) 124.3(5) ? ? ? yes
C(3) C(2) C(7) 115.4(5) ? ? ? yes
C(2) C(3) C(4) 122.7(5) ? ? ? yes
C(3) C(4) C(5) 117.1(5) ? ? ? yes
C(3) C(4) C(12) 121.5(6) ? ? ? yes
C(5) C(4) C(12) 121.3(6) ? ? ? yes
C(4) C(5) C(6) 123.6(5) ? ? ? yes
C(1) C(6) C(5) 119.3(5) ? ? ? yes
C(1) C(6) C(13) 124.6(5) ? ? ? yes
C(5) C(6) C(13) 116.0(5) ? ? ? yes
N(1) C(7) C(2) 126.3(5) ? ? ? yes
N(1) C(8) C(9) 110.3(5) ? ? ? yes
N(2) C(9) C(8) 116.5(7) ? ? ? yes
N(3) C(13) C(6) 127.0(5) ? ? ? yes
N(3) C(14) C(15) 110.6(5) ? ? ? yes
N(4) C(15) C(14) 118.1(8) ? ? ? yes
O(2) C(18) O(3) 126.5(5) ? ? ? yes
O(2) C(18) C(19) 116.6(5) ? ? ? yes
O(3) C(18) C(19) 116.9(5) ? ? ? yes
O(4) C(20) O(5) 126.5(5) ? ? ? yes
O(4) C(20) C(21) 116.4(5) ? ? ? yes
O(5) C(20) C(21) 117.0(5) ? ? ? yes
C(24) C(23) C(28) 114.5(5) ? ? ? yes
C(24) C(23) B 124.7(4) ? ? ? yes
C(28) C(23) B 120.7(5) ? ? ? yes
C(23) C(24) C(25) 122.8(5) ? ? ? yes
C(24) C(25) C(26) 120.5(5) ? ? ? yes
C(25) C(26) C(27) 118.6(5) ? ? ? yes
C(26) C(27) C(28) 120.6(5) ? ? ? yes
C(23) C(28) C(27) 123.0(5) ? ? ? yes
C(30) C(29) C(34) 112.9(5) ? ? ? yes
C(30) C(29) B 124.3(5) ? ? ? yes
C(34) C(29) B 122.8(4) ? ? ? yes
C(29) C(30) C(31) 123.4(5) ? ? ? yes
C(30) C(31) C(32) 121.2(6) ? ? ? yes
C(31) C(32) C(33) 117.7(6) ? ? ? yes
C(32) C(33) C(34) 120.5(6) ? ? ? yes
C(29) C(34) C(33) 124.3(5) ? ? ? yes
C(36) C(35) C(40) 113.8(5) ? ? ? yes
C(36) C(35) B 121.7(5) ? ? ? yes
C(40) C(35) B 124.4(5) ? ? ? yes
C(35) C(36) C(37) 123.3(5) ? ? ? yes
C(36) C(37) C(38) 120.6(5) ? ? ? yes
C(37) C(38) C(39) 118.3(5) ? ? ? yes
C(38) C(39) C(40) 120.8(6) ? ? ? yes
C(35) C(40) C(39) 123.3(5) ? ? ? yes
C(42) C(41) C(46) 114.5(5) ? ? ? yes
C(42) C(41) B 123.4(5) ? ? ? yes
C(46) C(41) B 122.0(5) ? ? ? yes
C(41) C(42) C(43) 123.0(5) ? ? ? yes
C(42) C(43) C(44) 119.3(5) ? ? ? yes
C(43) C(44) C(45) 120.1(5) ? ? ? yes
C(44) C(45) C(46) 119.7(5) ? ? ? yes
C(41) C(46) C(45) 123.4(5) ? ? ? yes
C(23) B C(29) 109.3(4) ? ? ? yes
C(23) B C(35) 110.8(4) ? ? ? yes
C(23) B C(41) 109.3(4) ? ? ? yes
C(29) B C(35) 109.9(4) ? ? ? yes
C(29) B C(41) 110.5(4) ? ? ? yes
C(35) B C(41) 106.9(4) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni(1) O(1) 2.022(3) ? ? yes
Ni(1) O(2) 1.982(3) ? ? yes
Ni(1) O(4) 1.973(3) ? ? yes
Ni(1) N(1) 1.983(4) ? ? yes
Ni(1) N(2) 2.138(4) ? ? yes
Ni(2) O(1) 2.044(3) ? ? yes
Ni(2) O(3) 2.006(3) ? ? yes
Ni(2) O(5) 2.037(3) ? ? yes
Ni(2) O(6) 2.270(4) ? ? yes
Ni(2) N(3) 2.002(4) ? ? yes
Ni(2) N(4) 2.141(4) ? ? yes
O(1) C(1) 1.328(5) ? ? yes
O(2) C(18) 1.257(5) ? ? yes
O(3) C(18) 1.252(5) ? ? yes
O(4) C(20) 1.255(6) ? ? yes
O(5) C(20) 1.244(6) ? ? yes
O(6) C(22) 1.439(7) ? ? yes
N(1) C(7) 1.280(6) ? ? yes
N(1) C(8) 1.480(6) ? ? yes
N(2) C(9) 1.406(8) ? ? yes
N(2) C(10) 1.476(8) ? ? yes
N(2) C(11) 1.435(7) ? ? yes
N(3) C(13) 1.269(6) ? ? yes
N(3) C(14) 1.457(6) ? ? yes
N(4) C(15) 1.424(9) ? ? yes
N(4) C(16) 1.380(8) ? ? yes
N(4) C(17) 1.431(7) ? ? yes
C(1) C(2) 1.411(6) ? ? yes
C(1) C(6) 1.428(6) ? ? yes
C(2) C(3) 1.409(7) ? ? yes
C(2) C(7) 1.451(7) ? ? yes
C(3) C(4) 1.371(7) ? ? yes
C(4) C(5) 1.368(7) ? ? yes
C(4) C(12) 1.514(7) ? ? yes
C(5) C(6) 1.401(7) ? ? yes
C(6) C(13) 1.446(7) ? ? yes
C(8) C(9) 1.449(10) ? ? yes
C(14) C(15) 1.431(10) ? ? yes
C(18) C(19) 1.511(6) ? ? yes
C(20) C(21) 1.510(7) ? ? yes
C(23) C(24) 1.386(6) ? ? yes
C(23) C(28) 1.406(6) ? ? yes
C(23) B 1.641(7) ? ? yes
C(24) C(25) 1.390(6) ? ? yes
C(25) C(26) 1.376(7) ? ? yes
C(26) C(27) 1.365(8) ? ? yes
C(27) C(28) 1.380(7) ? ? yes
C(29) C(30) 1.394(7) ? ? yes
C(29) C(34) 1.385(6) ? ? yes
C(29) B 1.658(7) ? ? yes
C(30) C(31) 1.387(7) ? ? yes
C(31) C(32) 1.353(8) ? ? yes
C(32) C(33) 1.371(8) ? ? yes
C(33) C(34) 1.380(7) ? ? yes
C(35) C(36) 1.391(6) ? ? yes
C(35) C(40) 1.386(7) ? ? yes
C(35) B 1.661(7) ? ? yes
C(36) C(37) 1.390(7) ? ? yes
C(37) C(38) 1.367(8) ? ? yes
C(38) C(39) 1.352(8) ? ? yes
C(39) C(40) 1.398(7) ? ? yes
C(41) C(42) 1.402(7) ? ? yes
C(41) C(46) 1.401(6) ? ? yes
C(41) B 1.643(7) ? ? yes
C(42) C(43) 1.394(7) ? ? yes
C(43) C(44) 1.379(8) ? ? yes
C(44) C(45) 1.367(8) ? ? yes
C(45) C(46) 1.386(7) ? ? yes
