#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013703.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_7013703
loop_
_publ_author_name
'Atencio, Reinaldo'
'Chacón, Mirbel'
'González, Teresa'
'Briceño, Alexander'
'Agrifoglio, Giuseppe'
'Sierraalta, Anibal'
_publ_section_title
;
 Robust hydrogen-bonded self-assemblies from biimidazole complexes.
 Synthesis and structural characterization of [M(biimidazole)2(OH2)2]2+
 (M = Co2+, Ni2+) complexes and carboxylate modules.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              505
_journal_page_last               513
_journal_paper_doi               10.1039/b312541f
_journal_year                    2004
_chemical_formula_moiety         'C12 H16 N8 Ni O2, 2(C7 H5 O5), 4(H2 O)'
_chemical_formula_sum            'C26 H34 N8 Ni O16'
_chemical_formula_weight         773.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '3 September 2003'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.08(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.135(5)
_cell_length_b                   9.265(4)
_cell_length_c                   13.992(4)
_cell_measurement_reflns_used    13
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.460
_cell_measurement_theta_min      20.750
_cell_volume                     1557.5(10)
_computing_cell_refinement
;
MSC/AFC, Diffractometer Control Software (Molecular
Structure Corporation, 1993a)
;
_computing_data_collection
;
MSC/AFC, Diffractometer Control Software (Molecular
Structure Corporation, 1993a)
;
_computing_data_reduction
;
TEXSAN, (Molecular Structure Corporation, 1993a)
;
_computing_molecular_graphics    'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_computing_structure_refinement  'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_computing_structure_solution    'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       'ω-2θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0862
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2874
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.8821
_exptl_absorpt_correction_T_min  0.6819
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al.,1968)'
_exptl_crystal_colour            'Pale Green'
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Laminar
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0649P)²+1.1424P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1530
_reflns_number_gt                1663
_reflns_number_total             2739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b312541f.txt
_cod_data_source_block           p21c-p
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Psi-scan' changed to
'psi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C26 H34 N8 Ni1 O16'
_cod_database_code               7013703
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.0000 0.5000 0.5000 0.0302(3) Uani 1 2 d S . .
O1W O 0.8533(3) 0.5303(4) 0.4009(2) 0.0392(10) Uani 1 1 d . . .
H1WB H 0.8227 0.6031 0.4050 0.059 Uiso 1 1 d R . .
H1WA H 0.8066 0.4771 0.3961 0.059 Uiso 1 1 d R . .
O1C O 0.5847(4) 0.3921(5) 0.5576(3) 0.0621(13) Uani 1 1 d . . .
H1CB H 0.6050 0.3570 0.5067 0.093 Uiso 1 1 d R . .
H1CA H 0.5167 0.4167 0.5530 0.093 Uiso 1 1 d R . .
O2C O 0.6824(4) 0.3222(4) 0.3888(3) 0.0557(12) Uani 1 1 d . . .
H2CB H 0.7019 0.2350 0.3825 0.084 Uiso 1 1 d R . .
H2CA H 0.6455 0.3276 0.3326 0.084 Uiso 1 1 d R . .
O1 O 0.7452(4) 0.4643(4) 0.8792(3) 0.0592(14) Uani 1 1 d . . .
O2 O 0.7568(4) 0.7011(4) 0.8731(3) 0.0474(11) Uani 1 1 d . . .
O3 O 0.5957(4) 0.8659(4) 1.1719(3) 0.0627(14) Uani 1 1 d . . .
H3O H 0.5933 0.9314 1.1322 0.094 Uiso 1 1 d R . .
O4 O 0.5410(5) 0.6150(5) 1.2571(3) 0.089(2) Uani 1 1 d . . .
H4O H 0.5149 0.6952 1.2648 0.134 Uiso 1 1 d R . .
O5 O 0.5618(4) 0.3593(4) 1.1733(3) 0.0557(13) Uani 1 1 d . . .
H5O H 0.5682 0.2882 1.1396 0.084 Uiso 1 1 d R . .
N11 N 0.9130(4) 0.3798(4) 0.5895(3) 0.0307(11) Uani 1 1 d . . .
N21 N 0.8239(4) 0.3842(5) 0.7174(3) 0.0362(12) Uani 1 1 d . . .
H21N H 0.8074 0.4044 0.7801 0.043 Uiso 1 1 d R . .
N31 N 0.8712(4) 0.7178(5) 0.7155(3) 0.0335(11) Uani 1 1 d . . .
H31N H 0.8526 0.7127 0.7780 0.040 Uiso 1 1 d R . .
N41 N 0.9547(4) 0.6672(4) 0.5885(3) 0.0301(11) Uani 1 1 d . . .
C11 C 0.8768(4) 0.4605(5) 0.6566(4) 0.0298(13) Uani 1 1 d . . .
C21 C 0.8823(5) 0.2414(6) 0.6109(4) 0.0391(14) Uani 1 1 d . . .
H21 H 0.8961 0.1593 0.5763 0.047 Uiso 1 1 d R . .
C31 C 0.8286(5) 0.2430(6) 0.6895(4) 0.0451(16) Uani 1 1 d . . .
H31 H 0.8003 0.1637 0.7188 0.054 Uiso 1 1 d R . .
C41 C 0.8993(5) 0.6145(5) 0.6553(4) 0.0301(13) Uani 1 1 d . . .
C51 C 0.9625(5) 0.8126(6) 0.6063(4) 0.0363(14) Uani 1 1 d . . .
H51 H 0.9971 0.8789 0.5705 0.044 Uiso 1 1 d R . .
C61 C 0.9119(5) 0.8454(6) 0.6847(4) 0.0360(14) Uani 1 1 d . . .
H61 H 0.9058 0.9363 0.7116 0.043 Uiso 1 1 d R . .
C1 C 0.7292(5) 0.5883(6) 0.9122(4) 0.0368(14) Uani 1 1 d . . .
C2 C 0.6746(4) 0.5979(6) 1.0011(4) 0.0319(13) Uani 1 1 d . . .
C3 C 0.6572(4) 0.7309(6) 1.0429(4) 0.0344(13) Uani 1 1 d . . .
H3 H 0.6762 0.8157 1.0136 0.041 Uiso 1 1 d R . .
C4 C 0.6123(5) 0.7368(6) 1.1280(4) 0.0404(15) Uani 1 1 d . . .
C5 C 0.5832(6) 0.6115(7) 1.1723(4) 0.0490(18) Uani 1 1 d . . .
C6 C 0.5946(5) 0.4800(6) 1.1282(4) 0.0394(14) Uani 1 1 d . . .
C7 C 0.6414(4) 0.4721(5) 1.0438(4) 0.0342(13) Uani 1 1 d . . .
H7 H 0.6505 0.3829 1.0154 0.041 Uiso 1 1 d R . .
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'
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
_geom_angle_publ_flag
N11 Ni1 N11 180.00(19) 3_766 . ?
N11 Ni1 N41 99.03(16) 3_766 . ?
N11 Ni1 N41 80.97(16) . . ?
N11 Ni1 N41 80.97(16) 3_766 3_766 ?
N11 Ni1 N41 99.03(16) . 3_766 ?
N41 Ni1 N41 180.000(1) . 3_766 ?
N11 Ni1 O1W 90.80(16) 3_766 3_766 ?
N11 Ni1 O1W 89.20(16) . 3_766 ?
N41 Ni1 O1W 88.72(16) . 3_766 ?
N41 Ni1 O1W 91.28(16) 3_766 3_766 ?
N11 Ni1 O1W 89.20(16) 3_766 . ?
N11 Ni1 O1W 90.80(16) . . ?
N41 Ni1 O1W 91.28(16) . . ?
N41 Ni1 O1W 88.72(16) 3_766 . ?
O1W Ni1 O1W 180.0 3_766 . ?
Ni1 O1W H1WB 115.8 . . ?
Ni1 O1W H1WA 122.0 . . ?
H1WB O1W H1WA 102.4 . . ?
H1CB O1C H1CA 115.6 . . ?
H2CB O2C H2CA 94.5 . . ?
C4 O3 H3O 109.6 . . ?
C5 O4 H4O 109.6 . . ?
C6 O5 H5O 109.5 . . ?
C11 N11 C21 104.1(4) . . ?
C11 N11 Ni1 111.9(3) . . ?
C21 N11 Ni1 143.8(3) . . ?
C11 N21 C31 106.3(4) . . ?
C11 N21 H21N 131.9 . . ?
C31 N21 H21N 118.5 . . ?
C41 N31 C61 106.3(4) . . ?
C41 N31 H31N 131.6 . . ?
C61 N31 H31N 118.9 . . ?
C41 N41 C51 105.3(4) . . ?
C41 N41 Ni1 110.2(3) . . ?
C51 N41 Ni1 144.5(4) . . ?
N11 C11 N21 112.9(4) . . ?
N11 C11 C41 117.6(4) . . ?
N21 C11 C41 129.4(5) . . ?
C31 C21 N11 110.0(5) . . ?
C31 C21 H21 125.1 . . ?
N11 C21 H21 124.9 . . ?
C21 C31 N21 106.6(5) . . ?
C21 C31 H31 126.8 . . ?
N21 C31 H31 126.6 . . ?
N41 C41 N31 112.3(5) . . ?
N41 C41 C11 119.2(5) . . ?
N31 C41 C11 128.6(5) . . ?
C61 C51 N41 109.8(5) . . ?
C61 C51 H51 125.1 . . ?
N41 C51 H51 125.1 . . ?
C51 C61 N31 106.5(5) . . ?
C51 C61 H61 126.7 . . ?
N31 C61 H61 126.8 . . ?
O2 C1 O1 122.5(5) . . ?
O2 C1 C2 119.6(5) . . ?
O1 C1 C2 117.9(5) . . ?
C3 C2 C7 119.3(5) . . ?
C3 C2 C1 120.9(5) . . ?
C7 C2 C1 119.8(5) . . ?
C4 C3 C2 119.9(5) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.1 . . ?
O3 C4 C3 121.5(5) . . ?
O3 C4 C5 117.9(5) . . ?
C3 C4 C5 120.7(5) . . ?
O4 C5 C6 119.1(5) . . ?
O4 C5 C4 121.5(5) . . ?
C6 C5 C4 119.4(5) . . ?
O5 C6 C5 117.4(5) . . ?
O5 C6 C7 122.1(5) . . ?
C5 C6 C7 120.5(5) . . ?
C6 C7 C2 120.0(5) . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N11 2.072(4) 3_766 ?
Ni1 N11 2.072(4) . ?
Ni1 N41 2.104(4) . ?
Ni1 N41 2.104(4) 3_766 ?
Ni1 O1W 2.115(4) 3_766 ?
Ni1 O1W 2.115(4) . ?
O1W H1WB 0.7763 . ?
O1W H1WA 0.7468 . ?
O1C H1CB 0.8501 . ?
O1C H1CA 0.8496 . ?
O2C H2CB 0.8500 . ?
O2C H2CA 0.8500 . ?
O1 C1 1.263(6) . ?
O2 C1 1.247(6) . ?
O3 C4 1.372(6) . ?
O3 H3O 0.8202 . ?
O4 C5 1.358(6) . ?
O4 H4O 0.8201 . ?
O5 C6 1.371(6) . ?
O5 H5O 0.8200 . ?
N11 C11 1.323(6) . ?
N11 C21 1.380(6) . ?
N21 C11 1.338(6) . ?
N21 C31 1.369(7) . ?
N21 H21N 0.9450 . ?
N31 C41 1.351(6) . ?
N31 C61 1.374(7) . ?
N31 H31N 0.9350 . ?
N41 C41 1.319(6) . ?
N41 C51 1.371(6) . ?
C11 C41 1.454(7) . ?
C21 C31 1.354(7) . ?
C21 H21 0.9301 . ?
C31 H31 0.9300 . ?
C51 C61 1.364(7) . ?
C51 H51 0.9300 . ?
C61 H61 0.9300 . ?
C1 C2 1.492(7) . ?
C2 C3 1.393(7) . ?
C2 C7 1.394(7) . ?
C3 C4 1.379(7) . ?
C3 H3 0.9298 . ?
C4 C5 1.385(8) . ?
C5 C6 1.382(8) . ?
C6 C7 1.382(7) . ?
C7 H7 0.9299 . ?
