#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:21:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180258 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/44/7114448.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_7114448
loop_
_publ_author_name
'Du, Miao'
'Bu, Xian-He'
'Guo, Ya-Mei'
'Zhang, Lei'
'Liao, Dai-Zheng'
'Ribas, Joan'
_publ_section_title
;
 First tetrameric NiII cluster with planar triangular topology exhibiting
 ferromagnetic pathways
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1478
_journal_paper_doi               10.1039/b203487p
_journal_year                    2002
_chemical_formula_sum            'C36 H68 Cl2 N6 Ni4 O24'
_chemical_formula_weight         1274.70
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 98.557(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.253(7)
_cell_length_b                   12.158(4)
_cell_length_c                   8.378(2)
_cell_measurement_reflns_used    3318
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.88
_cell_volume                     2442.9(12)
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5084
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.718
_exptl_absorpt_correction_T_max  0.8469
_exptl_absorpt_correction_T_min  0.7250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0576P)²+3.6917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                3197
_reflns_number_total             3350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203487p.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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_cell_volume        2443.0(12)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7114448
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni3 Ni 0.89289(2) 0.34422(5) 0.15138(7) 0.02634(15) Uani 1 1 d .
Ni1 Ni 1.0000 0.41457(7) 0.0000 0.0244(2) Uani 1 2 d S
Ni2 Ni 1.0000 0.65641(7) 0.0000 0.0279(2) Uani 1 2 d S
N2 N 0.85644(17) 0.3843(4) 0.3540(5) 0.0350(10) Uani 1 1 d .
N1 N 0.81858(16) 0.2648(4) 0.0672(5) 0.0343(10) Uani 1 1 d .
N3 N 1.0534(2) 0.7787(4) 0.0996(6) 0.0411(11) Uani 1 1 d .
O3 O 0.96641(13) 0.4403(3) 0.2205(4) 0.0277(8) Uani 1 1 d .
O4 O 0.96941(15) 0.6253(3) 0.2164(4) 0.0365(9) Uani 1 1 d .
O1 O 0.93565(13) 0.3032(3) -0.0393(4) 0.0307(8) Uani 1 1 d .
O2 O 0.95916(16) 0.1795(4) -0.2114(6) 0.0629(14) Uani 1 1 d .
O6 O 1.05742(11) 0.5322(4) 0.0866(4) 0.0270(6) Uani 1 1 d .
O5 O 0.86609(13) 0.4828(3) 0.0182(4) 0.0342(8) Uani 1 1 d .
O7 O 0.93590(16) 0.2098(4) 0.2583(6) 0.0469(11) Uani 1 1 d D
C1 C 0.8397(2) 0.2830(6) 0.4368(7) 0.0466(15) Uani 1 1 d .
H1A H 0.8225 0.3070 0.5282 0.056 Uiso 1 1 calc R
H1B H 0.8737 0.2446 0.4803 0.056 Uiso 1 1 calc R
C2 C 0.8011(2) 0.1995(5) 0.3455(8) 0.0474(15) Uani 1 1 d .
H2A H 0.7633 0.2259 0.3425 0.057 Uiso 1 1 calc R
H2B H 0.8043 0.1319 0.4076 0.057 Uiso 1 1 calc R
C3 C 0.8092(2) 0.1708(5) 0.1723(7) 0.0429(14) Uani 1 1 d .
H3A H 0.8407 0.1212 0.1770 0.051 Uiso 1 1 calc R
H3B H 0.7764 0.1312 0.1219 0.051 Uiso 1 1 calc R
C4 C 0.77023(17) 0.3442(6) 0.0485(6) 0.0396(11) Uani 1 1 d .
H4A H 0.7368 0.3028 0.0092 0.047 Uiso 1 1 calc R
H4B H 0.7758 0.3961 -0.0356 0.047 Uiso 1 1 calc R
C5 C 0.7586(2) 0.4107(6) 0.1948(7) 0.0487(14) Uani 1 1 d .
H5A H 0.7340 0.4709 0.1555 0.058 Uiso 1 1 calc R
H5B H 0.7381 0.3637 0.2589 0.058 Uiso 1 1 calc R
C6 C 0.8075(2) 0.4585(5) 0.3061(7) 0.0397(13) Uani 1 1 d .
H6A H 0.8204 0.5229 0.2543 0.048 Uiso 1 1 calc R
H6B H 0.7942 0.4832 0.4037 0.048 Uiso 1 1 calc R
C7 C 0.8994(2) 0.4409(5) 0.4710(6) 0.0398(13) Uani 1 1 d .
H7A H 0.9298 0.3899 0.5024 0.048 Uiso 1 1 calc R
H7B H 0.8830 0.4578 0.5670 0.048 Uiso 1 1 calc R
C8 C 0.9233(2) 0.5454(5) 0.4132(6) 0.0387(12) Uani 1 1 d .
H8A H 0.9477 0.5775 0.5034 0.046 Uiso 1 1 calc R
H8B H 0.8928 0.5966 0.3833 0.046 Uiso 1 1 calc R
C9 C 0.95558(17) 0.5365(6) 0.2728(5) 0.0303(10) Uani 1 1 d .
C10 C 0.8223(2) 0.2234(5) -0.1003(7) 0.0416(13) Uani 1 1 d .
H10A H 0.8218 0.2863 -0.1716 0.050 Uiso 1 1 calc R
H10B H 0.7892 0.1802 -0.1369 0.050 Uiso 1 1 calc R
C11 C 0.8728(2) 0.1543(5) -0.1182(7) 0.0411(12) Uani 1 1 d .
H11A H 0.8644 0.1115 -0.2165 0.049 Uiso 1 1 calc R
H11B H 0.8787 0.1028 -0.0288 0.049 Uiso 1 1 calc R
C12 C 0.9266(2) 0.2159(4) -0.1236(6) 0.0324(12) Uani 1 1 d .
C13 C 0.89251(17) 0.5473(4) -0.0593(5) 0.0260(10) Uani 1 1 d .
C14 C 0.8628(2) 0.6500(6) -0.1247(7) 0.0440(13) Uani 1 1 d .
H14A H 0.8489 0.6876 -0.0367 0.053 Uiso 1 1 calc R
H14B H 0.8308 0.6288 -0.2023 0.053 Uiso 1 1 calc R
C15 C 0.8979(2) 0.7308(5) -0.2060(8) 0.0471(15) Uani 1 1 d .
H15A H 0.9114 0.6935 -0.2950 0.057 Uiso 1 1 calc R
H15B H 0.8740 0.7906 -0.2511 0.057 Uiso 1 1 calc R
C16 C 0.9271(2) 0.8433(6) 0.0314(8) 0.0556(16) Uani 1 1 d .
H16A H 0.9094 0.7930 0.0980 0.067 Uiso 1 1 calc R
H16B H 0.8986 0.8940 -0.0176 0.067 Uiso 1 1 calc R
C17 C 0.9697(3) 0.9077(6) 0.1392(10) 0.0639(19) Uani 1 1 d .
H17A H 0.9524 0.9343 0.2291 0.077 Uiso 1 1 calc R
H17B H 0.9791 0.9717 0.0796 0.077 Uiso 1 1 calc R
C18 C 1.0251(2) 0.8499(6) 0.2100(8) 0.0555(16) Uani 1 1 d .
H18A H 1.0513 0.9064 0.2535 0.067 Uiso 1 1 calc R
H18B H 1.0178 0.8047 0.2999 0.067 Uiso 1 1 calc R
Cl1 Cl 0.81393(10) 0.8690(2) 0.3827(3) 0.0947(9) Uani 1 1 d .
O8 O 0.8104(4) 0.7641(8) 0.4115(18) 0.191(5) Uani 1 1 d .
O9 O 0.8363(3) 0.9066(9) 0.2514(9) 0.130(3) Uani 1 1 d .
O10 O 0.8397(4) 0.9234(9) 0.5222(10) 0.178(5) Uani 1 1 d .
O11 O 0.7565(3) 0.9174(9) 0.3497(9) 0.131(3) Uani 1 1 d .
O12 O 0.9319(2) 0.0633(4) 0.4942(5) 0.0607(12) Uani 1 1 d D
H7C H 0.933(2) 0.165(4) 0.335(5) 0.041(16) Uiso 1 1 d D
H7D H 0.9676(14) 0.187(6) 0.241(8) 0.06(2) Uiso 1 1 d D
H12A H 0.9064(18) 0.016(4) 0.500(7) 0.042(17) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
N N 0.0061 0.0033 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O5 Ni3 N1 90.48(16) . .
O5 Ni3 O7 166.66(14) . .
N1 Ni3 O7 97.82(19) . .
O5 Ni3 O1 86.21(14) . .
N1 Ni3 O1 97.68(15) . .
O7 Ni3 O1 82.35(16) . .
O5 Ni3 N2 96.41(16) . .
N1 Ni3 N2 86.19(17) . .
O7 Ni3 N2 94.57(17) . .
O1 Ni3 N2 175.33(15) . .
O5 Ni3 O3 83.33(14) . .
N1 Ni3 O3 173.78(17) . .
O7 Ni3 O3 88.15(16) . .
O1 Ni3 O3 81.31(12) . .
N2 Ni3 O3 95.13(15) . .
O6 Ni1 O6 91.6(2) . 2_755
O6 Ni1 O1 167.15(12) . .
O6 Ni1 O1 86.76(14) 2_755 .
O6 Ni1 O1 86.76(14) . 2_755
O6 Ni1 O1 167.15(12) 2_755 2_755
O1 Ni1 O1 97.6(2) . 2_755
O6 Ni1 O3 85.34(12) . .
O6 Ni1 O3 83.03(12) 2_755 .
O1 Ni1 O3 81.81(13) . .
O1 Ni1 O3 109.51(13) 2_755 .
O6 Ni1 O3 83.03(12) . 2_755
O6 Ni1 O3 85.34(12) 2_755 2_755
O1 Ni1 O3 109.51(13) . 2_755
O1 Ni1 O3 81.81(13) 2_755 2_755
O3 Ni1 O3 163.29(19) . 2_755
O6 Ni1 Ni2 45.82(10) . .
O6 Ni1 Ni2 45.82(10) 2_755 .
O1 Ni1 Ni2 131.22(10) . .
O1 Ni1 Ni2 131.22(10) 2_755 .
O3 Ni1 Ni2 81.64(10) . .
O3 Ni1 Ni2 81.64(10) 2_755 .
N3 Ni2 N3 87.9(3) . 2_755
N3 Ni2 O4 101.46(16) . 2_755
N3 Ni2 O4 93.53(16) 2_755 2_755
N3 Ni2 O4 93.53(16) . .
N3 Ni2 O4 101.46(16) 2_755 .
O4 Ni2 O4 159.2(2) 2_755 .
N3 Ni2 O6 175.81(15) . 2_755
N3 Ni2 O6 91.96(16) 2_755 2_755
O4 Ni2 O6 82.73(13) 2_755 2_755
O4 Ni2 O6 82.39(13) . 2_755
N3 Ni2 O6 91.96(16) . .
N3 Ni2 O6 175.81(15) 2_755 .
O4 Ni2 O6 82.39(13) 2_755 .
O4 Ni2 O6 82.73(13) . .
O6 Ni2 O6 88.50(19) 2_755 .
N3 Ni2 Ni1 136.06(15) . .
N3 Ni2 Ni1 136.06(15) 2_755 .
O4 Ni2 Ni1 79.59(10) 2_755 .
O4 Ni2 Ni1 79.59(10) . .
O6 Ni2 Ni1 44.25(10) 2_755 .
O6 Ni2 Ni1 44.25(10) . .
C7 N2 C6 110.3(4) . .
C7 N2 C1 106.6(4) . .
C6 N2 C1 111.1(4) . .
C7 N2 Ni3 107.7(3) . .
C6 N2 Ni3 109.7(3) . .
C1 N2 Ni3 111.2(4) . .
C3 N1 C10 109.4(4) . .
C3 N1 C4 111.7(4) . .
C10 N1 C4 105.7(4) . .
C3 N1 Ni3 111.1(3) . .
C10 N1 Ni3 107.7(3) . .
C4 N1 Ni3 111.1(3) . .
C16 N3 C15 109.7(5) 2_755 2_755
C16 N3 C18 112.0(5) 2_755 .
C15 N3 C18 104.5(5) 2_755 .
C16 N3 Ni2 109.4(4) 2_755 .
C15 N3 Ni2 110.8(4) 2_755 .
C18 N3 Ni2 110.3(3) . .
C9 O3 Ni3 112.6(3) . .
C9 O3 Ni1 123.1(3) . .
Ni3 O3 Ni1 95.47(13) . .
C9 O4 Ni2 129.5(3) . .
C12 O1 Ni1 134.4(3) . .
C12 O1 Ni3 123.9(3) . .
Ni1 O1 Ni3 99.87(14) . .
C13 O6 Ni1 130.4(3) 2_755 .
C13 O6 Ni2 115.5(3) 2_755 .
Ni1 O6 Ni2 89.93(11) . .
C13 O5 Ni3 130.1(3) . .
N2 C1 C2 120.5(5) . .
C1 C2 C3 118.4(4) . .
N1 C3 C2 116.1(5) . .
N1 C4 C5 119.2(4) . .
C6 C5 C4 118.5(4) . .
N2 C6 C5 116.8(5) . .
N2 C7 C8 116.3(4) . .
C7 C8 C9 117.3(5) . .
O4 C9 O3 125.3(4) . .
O4 C9 C8 115.7(5) . .
O3 C9 C8 119.0(5) . .
N1 C10 C11 116.1(5) . .
C10 C11 C12 116.4(5) . .
O2 C12 O1 123.7(5) . .
O2 C12 C11 118.0(5) . .
O1 C12 C11 118.2(4) . .
O5 C13 O6 125.0(5) . 2_755
O5 C13 C14 117.0(4) . .
O6 C13 C14 118.0(4) 2_755 .
C13 C14 C15 115.3(4) . .
N3 C15 C14 115.5(5) 2_755 .
N3 C16 C17 117.2(5) 2_755 .
C16 C17 C18 118.5(5) . .
N3 C18 C17 118.3(5) . .
O8 Cl1 O9 121.1(8) . .
O8 Cl1 O10 109.9(8) . .
O9 Cl1 O10 109.2(5) . .
O8 Cl1 O11 109.5(6) . .
O9 Cl1 O11 100.8(5) . .
O10 Cl1 O11 104.8(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni3 O5 2.071(4) .
Ni3 N1 2.074(4) .
Ni3 O7 2.069(4) .
Ni3 O1 2.090(3) .
Ni3 N2 2.085(4) .
Ni3 O3 2.138(3) .
Ni1 O6 2.052(4) .
Ni1 O6 2.052(4) 2_755
Ni1 O1 2.056(3) .
Ni1 O1 2.056(3) 2_755
Ni1 O3 2.150(3) .
Ni1 O3 2.150(3) 2_755
Ni1 Ni2 2.9403(14) .
Ni2 N3 2.064(5) .
Ni2 N3 2.064(5) 2_755
Ni2 O4 2.093(4) 2_755
Ni2 O4 2.093(3) .
Ni2 O6 2.109(4) 2_755
Ni2 O6 2.109(4) .
N2 C7 1.488(7) .
N2 C6 1.498(7) .
N2 C1 1.499(7) .
N1 C3 1.481(7) .
N1 C10 1.506(7) .
N1 C4 1.509(7) .
N3 C16 1.484(7) 2_755
N3 C15 1.488(8) 2_755
N3 C18 1.505(7) .
O3 C9 1.290(7) .
O4 C9 1.245(7) .
O1 C12 1.275(6) .
O2 C12 1.238(6) .
O6 C13 1.282(5) 2_755
O5 C13 1.253(6) .
C1 C2 1.509(10) .
C2 C3 1.533(9) .
C4 C5 1.529(8) .
C5 C6 1.511(8) .
C7 C8 1.506(8) .
C8 C9 1.511(6) .
C10 C11 1.510(8) .
C11 C12 1.513(7) .
C13 O6 1.282(5) 2_755
C13 C14 1.504(8) .
C14 C15 1.526(8) .
C15 N3 1.488(8) 2_755
C16 N3 1.484(7) 2_755
C16 C17 1.490(9) .
C17 C18 1.553(9) .
Cl1 O8 1.303(11) .
Cl1 O9 1.376(7) .
Cl1 O10 1.406(9) .
Cl1 O11 1.499(9) .
