#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:23:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179479 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/76/4337615.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_4337615
loop_
_publ_author_name
'Esteban, Jordi'
'Font-Bardia, Mercè'
'Costa, José Sánchez'
'Teat, Simon J.'
'Escuer, Albert'
_publ_section_title
;
 New topologies in pentanuclear nickel/oximato clusters: structural and
 magnetic characterization.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3194
_journal_page_last               3203
_journal_paper_doi               10.1021/ic500057j
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '2(C31 H45 Br3 N9 Ni5 O13), 3(C H4 O), H2 O'
_chemical_formula_sum            'C65 H104 Br6 N18 Ni10 O30'
_chemical_formula_weight         2684.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.210(7)
_cell_length_b                   15.210(7)
_cell_length_c                   40.38(2)
_cell_measurement_reflns_used    4872
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     8090(7)
_computing_cell_refinement       AUTOMAR
_computing_data_collection       MARXDS
_computing_data_reduction        MARSCALE
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      105(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_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  0.0928
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            27340
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.25
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    3.999
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4050
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.00089(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         5531
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0517
_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)+(0.0668P)²+10.4331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                4439
_reflns_number_total             5531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500057j_si_001.cif
_cod_data_source_block           joom65a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4337615
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Br1 Br 0.39891(4) 0.92497(3) -0.118967(10) 0.07363(16) Uani 1 1 d U
Ni2 Ni 0.3333 0.6667 0.065550(16) 0.04764(17) Uani 1 3 d S
Ni1 Ni 0.3333 0.6667 -0.022564(15) 0.04480(17) Uani 1 3 d S
Ni3 Ni 0.42819(3) 0.79847(3) -0.084496(10) 0.05278(14) Uani 1 1 d U
O1 O 0.36679(16) 0.57158(16) 0.00532(5) 0.0488(5) Uani 1 1 d .
O2 O 0.30219(17) 0.75062(17) -0.05524(5) 0.0485(5) Uani 1 1 d .
O3 O 0.3333 0.6667 -0.11012(9) 0.0492(8) Uani 1 3 d S
O4 O 0.5153(2) 0.9123(2) -0.05034(7) 0.0723(7) Uani 1 1 d U
H4O H 0.4975 0.8946 -0.0283 0.108 Uiso 1 1 calc R
O5 O 0.5553(2) 0.8259(2) -0.11123(7) 0.0693(7) Uani 1 1 d D
H5O H 0.549(4) 0.7628(16) -0.1119(12) 0.083 Uiso 1 1 d D
N1 N 0.2456(2) 0.5340(2) 0.09401(7) 0.0546(6) Uani 1 1 d .
N2 N 0.3336(2) 0.55785(19) 0.03593(6) 0.0484(5) Uani 1 1 d .
N3 N 0.2696(3) 0.3105(3) 0.01516(10) 0.0840(10) Uani 1 1 d .
C1 C 0.2029(3) 0.5258(3) 0.12375(9) 0.0612(8) Uani 1 1 d .
H1 H 0.2035 0.5824 0.1328 0.073 Uiso 1 1 calc R
C2 C 0.1577(3) 0.4354(3) 0.14153(10) 0.0651(9) Uani 1 1 d .
H2 H 0.1264 0.4313 0.1617 0.078 Uiso 1 1 calc R
C3 C 0.1595(3) 0.3520(3) 0.12913(10) 0.0712(10) Uani 1 1 d .
H3 H 0.1310 0.2913 0.1409 0.085 Uiso 1 1 calc R
C4 C 0.2041(3) 0.3605(3) 0.09928(10) 0.0664(9) Uani 1 1 d .
H4 H 0.2069 0.3054 0.0905 0.080 Uiso 1 1 calc R
C5 C 0.2464(3) 0.4530(3) 0.08135(8) 0.0535(7) Uani 1 1 d .
C6 C 0.2914(3) 0.4660(3) 0.04849(8) 0.0547(7) Uani 1 1 d .
C7 C 0.2807(3) 0.3822(3) 0.03018(10) 0.0628(8) Uani 1 1 d .
C8 C 0.2780(3) 0.8223(3) -0.04234(9) 0.0621(8) Uani 1 1 d .
H8A H 0.2652 0.8559 -0.0602 0.093 Uiso 1 1 calc R
H8B H 0.3338 0.8715 -0.0293 0.093 Uiso 1 1 calc R
H8C H 0.2186 0.7882 -0.0287 0.093 Uiso 1 1 calc R
C9 C 0.3333 0.6667 -0.14561(15) 0.0656(15) Uani 1 3 d S
H9A H 0.2854 0.6001 -0.1535 0.098 Uiso 0.33 1 calc PR
H9B H 0.3999 0.6853 -0.1535 0.098 Uiso 0.33 1 calc PR
H9C H 0.3147 0.7146 -0.1535 0.098 Uiso 0.33 1 calc PR
C10 C 0.5954(4) 1.0102(3) -0.05518(12) 0.0788(11) Uani 1 1 d .
H10A H 0.6190 1.0431 -0.0341 0.118 Uiso 1 1 calc R
H10B H 0.5729 1.0477 -0.0684 0.118 Uiso 1 1 calc R
H10C H 0.6497 1.0075 -0.0664 0.118 Uiso 1 1 calc R
C11 C 0.5920(4) 0.8799(4) -0.14193(14) 0.0908(14) Uani 1 1 d .
H11A H 0.6530 0.8803 -0.1483 0.136 Uiso 1 1 calc R
H11B H 0.6061 0.9484 -0.1392 0.136 Uiso 1 1 calc R
H11C H 0.5414 0.8469 -0.1588 0.136 Uiso 1 1 calc R
O1W O 0.1862(8) 0.0988(9) 0.0912(3) 0.151(4) Uani 0.50 1 d PD
C1W C 0.1005(12) 0.1061(16) 0.1022(4) 0.172(8) Uani 0.50 1 d PD
O2W O 0.0000 0.0000 0.0000 0.084(2) Uani 1 6 d S
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'
Br Br -0.2901 2.4595 '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'
Ni Ni 0.3393 1.1124 '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'
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_3
N2 Ni2 N2 89.20(10) 3_565 2_665
N2 Ni2 N2 89.20(10) 3_565 .
N2 Ni2 N2 89.20(10) 2_665 .
N2 Ni2 N1 78.53(11) 3_565 3_565
N2 Ni2 N1 101.06(11) 2_665 3_565
N2 Ni2 N1 163.79(11) . 3_565
N2 Ni2 N1 163.79(11) 3_565 2_665
N2 Ni2 N1 78.53(11) 2_665 2_665
N2 Ni2 N1 101.06(11) . 2_665
N1 Ni2 N1 93.32(11) 3_565 2_665
N2 Ni2 N1 101.06(11) 3_565 .
N2 Ni2 N1 163.79(11) 2_665 .
N2 Ni2 N1 78.53(11) . .
N1 Ni2 N1 93.32(11) 3_565 .
N1 Ni2 N1 93.32(11) 2_665 .
O2 Ni1 O2 83.01(10) . 2_665
O2 Ni1 O2 83.01(10) . 3_565
O2 Ni1 O2 83.01(10) 2_665 3_565
O2 Ni1 O1 91.10(9) . 3_565
O2 Ni1 O1 91.81(9) 2_665 3_565
O2 Ni1 O1 172.56(9) 3_565 3_565
O2 Ni1 O1 91.81(9) . 2_665
O2 Ni1 O1 172.56(9) 2_665 2_665
O2 Ni1 O1 91.10(9) 3_565 2_665
O1 Ni1 O1 93.62(8) 3_565 2_665
O2 Ni1 O1 172.56(9) . .
O2 Ni1 O1 91.10(9) 2_665 .
O2 Ni1 O1 91.81(9) 3_565 .
O1 Ni1 O1 93.62(8) 3_565 .
O1 Ni1 O1 93.62(8) 2_665 .
O2 Ni3 O5 170.67(10) . .
O2 Ni3 O3 82.46(10) . .
O5 Ni3 O3 93.62(11) . .
O2 Ni3 O2 82.37(12) . 3_565
O5 Ni3 O2 88.71(10) . 3_565
O3 Ni3 O2 81.87(9) . 3_565
O2 Ni3 O4 90.38(10) . .
O5 Ni3 O4 92.07(12) . .
O3 Ni3 O4 168.46(12) . .
O2 Ni3 O4 88.25(10) 3_565 .
O2 Ni3 Br1 95.51(7) . .
O5 Ni3 Br1 93.45(8) . .
O3 Ni3 Br1 98.95(7) . .
O2 Ni3 Br1 177.63(6) 3_565 .
O4 Ni3 Br1 90.70(9) . .
N2 O1 Ni1 114.25(17) . .
C8 O2 Ni1 118.3(2) . .
C8 O2 Ni3 119.8(2) . .
Ni1 O2 Ni3 97.23(10) . .
C8 O2 Ni3 122.2(2) . 2_665
Ni1 O2 Ni3 96.45(9) . 2_665
Ni3 O2 Ni3 97.54(9) . 2_665
C9 O3 Ni3 120.01(9) . 2_665
C9 O3 Ni3 120.01(9) . .
Ni3 O3 Ni3 97.17(12) 2_665 .
C9 O3 Ni3 120.01(9) . 3_565
Ni3 O3 Ni3 97.17(12) 2_665 3_565
Ni3 O3 Ni3 97.17(12) . 3_565
C10 O4 Ni3 130.5(3) . .
C10 O4 H4O 114.8 . .
Ni3 O4 H4O 114.8 . .
C11 O5 Ni3 128.6(3) . .
C11 O5 H5O 112(3) . .
Ni3 O5 H5O 102(3) . .
C5 N1 C1 118.9(3) . .
C5 N1 Ni2 112.2(2) . .
C1 N1 Ni2 128.3(3) . .
O1 N2 C6 118.5(3) . .
O1 N2 Ni2 125.38(19) . .
C6 N2 Ni2 116.0(2) . .
N1 C1 C2 122.1(4) . .
N1 C1 H1 119.0 . .
C2 C1 H1 119.0 . .
C3 C2 C1 119.7(4) . .
C3 C2 H2 120.1 . .
C1 C2 H2 120.1 . .
C4 C3 C2 118.3(4) . .
C4 C3 H3 120.9 . .
C2 C3 H3 120.9 . .
C3 C4 C5 120.4(4) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
N1 C5 C4 120.6(3) . .
N1 C5 C6 116.2(3) . .
C4 C5 C6 123.2(3) . .
N2 C6 C7 122.2(3) . .
N2 C6 C5 116.2(3) . .
C7 C6 C5 121.3(3) . .
N3 C7 C6 178.4(5) . .
O2 C8 H8A 109.5 . .
O2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
O2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O3 C9 H9A 109.5 . .
O3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
O3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
O4 C10 H10A 109.5 . .
O4 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O4 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O5 C11 H11A 109.5 . .
O5 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
O5 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Ni3 2.5873(11) .
Ni2 N2 2.044(3) 3_565
Ni2 N2 2.044(3) 2_665
Ni2 N2 2.044(3) .
Ni2 N1 2.117(3) 3_565
Ni2 N1 2.117(3) 2_665
Ni2 N1 2.117(3) .
Ni1 O2 2.050(2) .
Ni1 O2 2.050(2) 2_665
Ni1 O2 2.050(2) 3_565
Ni1 O1 2.087(2) 3_565
Ni1 O1 2.087(2) 2_665
Ni1 O1 2.087(2) .
Ni3 O2 2.050(2) .
Ni3 O5 2.066(3) .
Ni3 O3 2.068(2) .
Ni3 O2 2.075(2) 3_565
Ni3 O4 2.089(3) .
O1 N2 1.312(3) .
O2 C8 1.413(4) .
O2 Ni3 2.075(2) 2_665
O3 C9 1.433(7) .
O3 Ni3 2.068(2) 2_665
O3 Ni3 2.068(2) 3_565
O4 C10 1.387(5) .
O4 H4O 0.9300 .
O5 C11 1.437(6) .
O5 H5O 0.917(8) .
N1 C5 1.339(4) .
N1 C1 1.341(4) .
N2 C6 1.314(4) .
N3 C7 1.184(5) .
C1 C2 1.390(5) .
C1 H1 0.9300 .
C2 C3 1.378(6) .
C2 H2 0.9300 .
C3 C4 1.357(6) .
C3 H3 0.9300 .
C4 C5 1.419(5) .
C4 H4 0.9300 .
C5 C6 1.461(5) .
C6 C7 1.410(5) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
O1W C1W 1.433(10) .
