#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/26/4322685.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_4322685
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            'C22 H35 Br N6 Ni2 O4 S2'
_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 21:32:28 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                103.53(2)
_cell_angle_beta                 100.91(1)
_cell_angle_gamma                85.62(1)
_cell_formula_units_Z            2.00
_cell_length_a                   10.167(1)
_cell_length_b                   16.119(2)
_cell_length_c                   9.472(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      29.49
_cell_volume                     1481.1(5)
_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)'
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      20.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.08443
_diffrn_orient_matrix_UB_12      -0.03028
_diffrn_orient_matrix_UB_13      -0.00877
_diffrn_orient_matrix_UB_21      0.05073
_diffrn_orient_matrix_UB_22      -0.05607
_diffrn_orient_matrix_UB_23      -0.01577
_diffrn_orient_matrix_UB_31      0.01850
_diffrn_orient_matrix_UB_32      0.00395
_diffrn_orient_matrix_UB_33      0.10884
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  1.98
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5532
_diffrn_reflns_theta_max         24.9959
_diffrn_standards_decay_%        1.35
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 28.028
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             728.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_min          0.150
_refine_diff_density_max         -1.04930
_refine_diff_density_min         0.65070
_refine_ls_extinction_coef       19.72937
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.940
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4160
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0500
_refine_ls_shift/esd_max         0.1060
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0540
_cod_data_source_file            ic971209p_2.cif
_cod_data_source_block           '[Ni(L2)(AcO)(NCS)2(MeOH)](complex3)'
_cod_original_cell_volume        1481.2(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C22 H35 N6 O4 S2 Br Ni2'
_cod_database_code               4322685
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
Br1 0.34689(7) -0.07661(5) -0.29603(9) 0.0606(2) Uij ? ?
Ni1 0.28251(8) 0.34193(5) 0.22023(8) 0.0381(2) Uij ? ?
Ni2 0.18201(7) 0.22380(5) 0.37424(8) 0.0371(2) Uij ? ?
S1 0.6230(2) 0.2066(2) 0.6727(2) 0.0708(7) Uij ? ?
S2 0.1920(3) 0.4958(1) 0.6596(2) 0.0795(7) Uij ? ?
O1 0.3042(4) 0.2163(2) 0.2233(4) 0.040(1) Uij ? ?
O2 0.0960(4) 0.3241(3) 0.0957(5) 0.050(1) Uij ? ?
O3 0.0189(4) 0.2416(3) 0.2216(5) 0.049(1) Uij ? ?
O4 0.4723(4) 0.3530(3) 0.3745(5) 0.050(1) Uij ? ?
N1 0.3711(5) 0.3194(3) 0.0442(6) 0.045(2) Uij ? ?
N2 0.2745(6) 0.4718(3) 0.1990(6) 0.047(2) Uij ? ?
N3 0.1549(5) 0.0907(3) 0.3124(6) 0.043(1) Uij ? ?
N4 0.0594(5) 0.2232(3) 0.5379(6) 0.046(2) Uij ? ?
N5 0.3612(6) 0.2144(4) 0.5238(6) 0.052(2) Uij ? ?
N6 0.2094(5) 0.3605(3) 0.4223(6) 0.045(2) Uij ? ?
C1 0.3193(6) 0.1520(4) 0.1114(7) 0.039(2) Uij ? ?
C2 0.3602(6) 0.1650(4) -0.0173(6) 0.038(2) Uij ? ?
C3 0.3719(6) 0.0942(4) -0.1358(7) 0.045(2) Uij ? ?
C4 0.3419(6) 0.0148(4) -0.1282(8) 0.050(2) Uij ? ?
C5 0.3083(6) 0.0004(4) -0.0010(8) 0.048(2) Uij ? ?
C6 0.2996(6) 0.0675(4) 0.1205(7) 0.041(2) Uij ? ?
C7 0.3914(6) 0.2467(4) -0.0400(7) 0.046(2) Uij ? ?
C8 0.4021(8) 0.3984(4) 0.0046(8) 0.056(2) Uij ? ?
C9 0.2909(8) 0.4638(4) 0.0439(8) 0.057(2) Uij ? ?
C10 0.3807(9) 0.5237(5) 0.3030(9) 0.067(2) Uij ? ?
C11 0.1417(8) 0.5150(5) 0.2183(10) 0.068(3) Uij ? ?
C12 0.2779(7) 0.0486(4) 0.2634(8) 0.052(2) Uij ? ?
C13 0.0374(7) 0.0600(5) 0.1969(8) 0.061(2) Uij ? ?
C14 0.1398(8) 0.0735(4) 0.4547(8) 0.057(2) Uij ? ?
C15 0.0328(7) 0.1314(5) 0.5213(9) 0.060(2) Uij ? ?
C16 -0.0672(7) 0.2730(5) 0.5116(9) 0.066(3) Uij ? ?
C17 0.1283(8) 0.2576(5) 0.6893(8) 0.061(2) Uij ? ?
C18 0.0070(7) 0.2828(4) 0.1222(7) 0.050(2) Uij ? ?
C19 -0.1281(8) 0.2828(7) 0.025(1) 0.088(3) Uij ? ?
C20 0.4703(6) 0.2110(4) 0.5835(7) 0.044(2) Uij ? ?
C21 0.2029(7) 0.4181(4) 0.5232(7) 0.047(2) Uij ? ?
C22 0.5944(7) 0.3145(5) 0.3312(9) 0.067(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 44 0.003 0.002 'International Tables'
H 0 70 0.000 0.000 'International Tables'
O 0 8 0.011 0.006 'International Tables'
N 0 12 0.006 0.003 'International Tables'
S 0 4 0.125 0.123 'International Tables'
Br 0 2 -0.290 2.459 '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) 91.1(2) ? ? ? yes
O(1) Ni(1) O(4) 84.4(2) ? ? ? yes
O(1) Ni(1) N(1) 89.7(2) ? ? ? yes
O(1) Ni(1) N(2) 173.5(2) ? ? ? yes
O(1) Ni(1) N(6) 86.9(2) ? ? ? yes
O(2) Ni(1) O(4) 172.2(2) ? ? ? yes
O(2) Ni(1) N(1) 93.0(2) ? ? ? yes
O(2) Ni(1) N(2) 90.5(2) ? ? ? yes
O(2) Ni(1) N(6) 93.0(2) ? ? ? yes
O(4) Ni(1) N(1) 93.3(2) ? ? ? yes
O(4) Ni(1) N(2) 94.7(2) ? ? ? yes
O(4) Ni(1) N(6) 80.4(2) ? ? ? yes
N(1) Ni(1) N(2) 83.9(2) ? ? ? yes
N(1) Ni(1) N(6) 173.1(2) ? ? ? yes
N(2) Ni(1) N(6) 99.3(2) ? ? ? yes
O(1) Ni(2) O(3) 90.5(2) ? ? ? yes
O(1) Ni(2) N(3) 91.6(2) ? ? ? yes
O(1) Ni(2) N(4) 175.8(2) ? ? ? yes
O(1) Ni(2) N(5) 85.0(2) ? ? ? yes
O(1) Ni(2) N(6) 85.4(2) ? ? ? yes
O(3) Ni(2) N(3) 89.9(2) ? ? ? yes
O(3) Ni(2) N(4) 92.1(2) ? ? ? yes
O(3) Ni(2) N(5) 173.9(2) ? ? ? yes
O(3) Ni(2) N(6) 87.7(2) ? ? ? yes
N(3) Ni(2) N(4) 85.3(2) ? ? ? yes
N(3) Ni(2) N(5) 94.3(2) ? ? ? yes
N(3) Ni(2) N(6) 176.2(2) ? ? ? yes
N(4) Ni(2) N(5) 92.6(2) ? ? ? yes
N(4) Ni(2) N(6) 97.9(2) ? ? ? yes
N(5) Ni(2) N(6) 87.8(2) ? ? ? yes
Ni(1) O(1) Ni(2) 94.7(2) ? ? ? yes
Ni(1) O(1) C(1) 127.0(4) ? ? ? yes
Ni(2) O(1) C(1) 127.6(4) ? ? ? yes
Ni(1) O(2) C(18) 124.5(4) ? ? ? yes
Ni(2) O(3) C(18) 129.5(4) ? ? ? yes
Ni(1) O(4) C(22) 121.8(4) ? ? ? yes
Ni(1) N(1) C(7) 127.0(4) ? ? ? yes
Ni(1) N(1) C(8) 113.0(4) ? ? ? yes
C(7) N(1) C(8) 119.7(6) ? ? ? yes
Ni(1) N(2) C(9) 103.4(4) ? ? ? yes
Ni(1) N(2) C(10) 113.1(4) ? ? ? yes
Ni(1) N(2) C(11) 112.1(4) ? ? ? yes
C(9) N(2) C(10) 111.1(6) ? ? ? yes
C(9) N(2) C(11) 108.3(6) ? ? ? yes
C(10) N(2) C(11) 108.7(6) ? ? ? yes
Ni(2) N(3) C(12) 108.3(4) ? ? ? yes
Ni(2) N(3) C(13) 117.1(4) ? ? ? yes
Ni(2) N(3) C(14) 100.5(4) ? ? ? yes
C(12) N(3) C(13) 108.9(5) ? ? ? yes
C(12) N(3) C(14) 111.4(5) ? ? ? yes
C(13) N(3) C(14) 110.5(5) ? ? ? yes
Ni(2) N(4) C(15) 104.8(4) ? ? ? yes
Ni(2) N(4) C(16) 111.3(4) ? ? ? yes
Ni(2) N(4) C(17) 112.6(4) ? ? ? yes
C(15) N(4) C(16) 110.7(5) ? ? ? yes
C(15) N(4) C(17) 109.0(5) ? ? ? yes
C(16) N(4) C(17) 108.3(6) ? ? ? yes
Ni(2) N(5) C(20) 166.8(6) ? ? ? yes
Ni(1) N(6) Ni(2) 88.1(2) ? ? ? yes
Ni(1) N(6) C(21) 135.3(5) ? ? ? yes
Ni(2) N(6) C(21) 136.0(5) ? ? ? yes
O(1) C(1) C(2) 121.5(5) ? ? ? yes
O(1) C(1) C(6) 119.8(5) ? ? ? yes
C(2) C(1) C(6) 118.6(5) ? ? ? yes
C(1) C(2) C(3) 119.3(6) ? ? ? yes
C(1) C(2) C(7) 125.3(5) ? ? ? yes
C(3) C(2) C(7) 115.3(6) ? ? ? yes
C(2) C(3) C(4) 120.4(6) ? ? ? yes
Br(1) C(4) C(3) 118.6(5) ? ? ? yes
Br(1) C(4) C(5) 120.5(5) ? ? ? yes
C(3) C(4) C(5) 120.8(6) ? ? ? yes
C(4) C(5) C(6) 121.0(6) ? ? ? yes
C(1) C(6) C(5) 119.5(6) ? ? ? yes
C(1) C(6) C(12) 120.8(5) ? ? ? yes
C(5) C(6) C(12) 119.6(6) ? ? ? yes
N(1) C(7) C(2) 125.2(6) ? ? ? yes
N(1) C(8) C(9) 106.5(5) ? ? ? yes
N(2) C(9) C(8) 110.7(6) ? ? ? yes
N(3) C(12) C(6) 112.9(5) ? ? ? yes
N(3) C(14) C(15) 111.4(6) ? ? ? yes
N(4) C(15) C(14) 111.6(5) ? ? ? yes
O(2) C(18) O(3) 126.9(6) ? ? ? yes
O(2) C(18) C(19) 116.6(6) ? ? ? yes
O(3) C(18) C(19) 116.5(6) ? ? ? yes
S(1) C(20) N(5) 178.2(6) ? ? ? yes
S(2) C(21) N(6) 179.2(6) ? ? ? 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
Br(1) C(4) 1.904(7) ? ? yes
Ni(1) O(1) 2.027(4) ? ? yes
Ni(1) O(2) 2.036(4) ? ? yes
Ni(1) O(4) 2.180(4) ? ? yes
Ni(1) N(1) 1.990(5) ? ? yes
Ni(1) N(2) 2.143(5) ? ? yes
Ni(1) N(6) 2.131(5) ? ? yes
Ni(2) O(1) 2.042(4) ? ? yes
Ni(2) O(3) 2.034(4) ? ? yes
Ni(2) N(3) 2.113(5) ? ? yes
Ni(2) N(4) 2.167(5) ? ? yes
Ni(2) N(5) 2.105(6) ? ? yes
Ni(2) N(6) 2.172(5) ? ? yes
S(1) C(20) 1.626(6) ? ? yes
S(2) C(21) 1.589(7) ? ? yes
O(1) C(1) 1.321(7) ? ? yes
O(2) C(18) 1.258(8) ? ? yes
O(3) C(18) 1.257(8) ? ? yes
O(4) C(22) 1.432(9) ? ? yes
N(1) C(7) 1.281(8) ? ? yes
N(1) C(8) 1.481(8) ? ? yes
N(2) C(9) 1.485(8) ? ? yes
N(2) C(10) 1.478(9) ? ? yes
N(2) C(11) 1.494(9) ? ? yes
N(3) C(12) 1.478(9) ? ? yes
N(3) C(13) 1.487(8) ? ? yes
N(3) C(14) 1.476(8) ? ? yes
N(4) C(15) 1.492(9) ? ? yes
N(4) C(16) 1.475(9) ? ? yes
N(4) C(17) 1.470(8) ? ? yes
N(5) C(20) 1.150(8) ? ? yes
N(6) C(21) 1.174(8) ? ? yes
C(1) C(2) 1.425(8) ? ? yes
C(1) C(6) 1.416(8) ? ? yes
C(2) C(3) 1.417(8) ? ? yes
C(2) C(7) 1.450(8) ? ? yes
C(3) C(4) 1.359(9) ? ? yes
C(4) C(5) 1.385(10) ? ? yes
C(5) C(6) 1.394(9) ? ? yes
C(6) C(12) 1.513(9) ? ? yes
C(8) C(9) 1.52(1) ? ? yes
C(14) C(15) 1.51(1) ? ? yes
C(18) C(19) 1.503(9) ? ? yes
