#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/95/7009510.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_7009510
loop_
_publ_author_name
'Yaroslaw D. Lampeka'
'Sergey P. Gavrish'
'Robert W. Hay'
'Tanja Eisenblätter'
'Philip Lightfoot'
_publ_section_title
;
 The crystal and molecular structures of the nickel(II) complexes of
 malonamide-derived unsubstituted 14- and 13-membered
 tetraazamacrocycles and NMR study of the complexes in aqueous solution
;
_journal_issue                   13
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              2023
_journal_page_last               2029
_journal_paper_doi               10.1039/b001510p
_journal_year                    2000
_chemical_formula_sum            'C10 H30 N4 Ni O8'
_chemical_formula_weight         393.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Mon Jan 31 15:25:26 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 92.17(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.247(2)
_cell_length_b                   24.982(4)
_cell_length_c                   9.436(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    473.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      25.0
_cell_volume                     1707.1(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      473.2
_diffrn_measurement_device       AFC7S
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.11940
_diffrn_orient_matrix_UB_12      0.01944
_diffrn_orient_matrix_UB_13      -0.00918
_diffrn_orient_matrix_UB_21      0.06855
_diffrn_orient_matrix_UB_22      -0.03453
_diffrn_orient_matrix_UB_23      0.01079
_diffrn_orient_matrix_UB_31      -0.00874
_diffrn_orient_matrix_UB_32      -0.00527
_diffrn_orient_matrix_UB_33      -0.10459
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.92
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3141
_diffrn_reflns_theta_max         25.00
_diffrn_standards_decay_%        -0.15
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             840.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.60
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.464
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2286
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0476
_refine_ls_shift/esd_max         0.6660
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0541
_reflns_number_observed          2286
_reflns_number_total             2888
_reflns_observed_criterion       3.00
_cod_data_source_file            b001510p.txt
_cod_data_source_block           Ya
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 53 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1707.1(7)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C10 H30 N4 O8 Ni '
_cod_database_code               7009510
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
1/2-x,1/2+y,1/2-z
'   -x,   -y,   -z'
1/2+x,1/2-y,1/2+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
Ni(1) 0.46470(10) 0.19939(3) 0.64487(7) 0.0180(2) Uani ? ?
O(1) 0.5286(5) 0.3318(2) 0.8984(4) 0.024(1) Uani ? ?
O(2) 0.5407(5) 0.3322(2) 0.4006(4) 0.024(1) Uani ? ?
O(3) 0.8373(7) 0.1511(3) 0.6491(5) 0.053(2) Uani ? ?
O(4) 0.1902(8) 0.4417(2) 0.6394(5) 0.050(2) Uani ? ?
O(5) -0.1866(9) 0.4539(3) 0.6211(6) 0.064(2) Uani ? ?
O(6) 0.4951(8) 0.4397(2) 0.4339(6) 0.043(2) Uani ? ?
O(7) 0.3989(7) 0.4370(2) 0.8918(5) 0.038(1) Uani ? ?
O(8) 0.3606(9) 0.4827(2) 0.1715(6) 0.040(1) Uani ? ?
N(1) 0.5010(6) 0.2497(2) 0.7936(4) 0.020(1) Uani ? ?
N(2) 0.4169(6) 0.1487(2) 0.7957(4) 0.021(1) Uani ? ?
N(3) 0.4121(6) 0.1502(2) 0.4902(5) 0.022(1) Uani ? ?
N(4) 0.5026(6) 0.2498(2) 0.5007(4) 0.019(1) Uani ? ?
C(1) 0.5139(8) 0.3303(2) 0.6490(6) 0.025(2) Uani ? ?
C(2) 0.5149(7) 0.3016(2) 0.7871(5) 0.019(1) Uani ? ?
C(3) 0.5009(8) 0.2265(2) 0.9377(5) 0.024(2) Uani ? ?
C(4) 0.5278(8) 0.1673(2) 0.9211(6) 0.026(2) Uani ? ?
C(5) 0.4408(9) 0.0908(2) 0.7735(6) 0.029(2) Uani ? ?
C(6) 0.3398(9) 0.0710(2) 0.6384(6) 0.033(2) Uani ? ?
C(7) 0.4321(9) 0.0913(2) 0.5090(6) 0.031(2) Uani ? ?
C(8) 0.5204(8) 0.1681(2) 0.3691(6) 0.025(2) Uani ? ?
C(9) 0.4999(8) 0.2276(2) 0.3557(5) 0.023(2) Uani ? ?
C(10) 0.5203(7) 0.3019(2) 0.5078(5) 0.020(1) Uani ? ?
H(1) 0.4041 0.3511 0.6449 0.0295 Uani ? ?
H(2) 0.6182 0.3534 0.6536 0.0295 Uani ? ?
H(3) 0.5989 0.2412 0.9950 0.0281 Uani ? ?
H(4) 0.3866 0.2335 0.9801 0.0281 Uani ? ?
H(5) 0.4886 0.1494 1.0035 0.0316 Uani ? ?
H(6) 0.6546 0.1599 0.9083 0.0316 Uani ? ?
H(7) 0.5687 0.0834 0.7670 0.0352 Uani ? ?
H(8) 0.3940 0.0722 0.8523 0.0352 Uani ? ?
H(9) 0.3405 0.0329 0.6375 0.0397 Uani ? ?
H(10) 0.2158 0.0834 0.6369 0.0397 Uani ? ?
H(11) 0.3787 0.0740 0.4279 0.0373 Uani ? ?
H(12) 0.5599 0.0829 0.5176 0.0373 Uani ? ?
H(13) 0.6467 0.1591 0.3854 0.0300 Uani ? ?
H(14) 0.4749 0.1513 0.2845 0.0300 Uani ? ?
H(15) 0.3861 0.2361 0.3074 0.0278 Uani ? ?
H(16) 0.5991 0.2420 0.3049 0.0278 Uani ? ?
H(17) 0.2912 0.1535 0.8181 0.0253 Uani ? ?
H(18) 0.2863 0.1560 0.4624 0.0268 Uani ? ?
H(19) 0.515(9) 0.412(3) 0.427(7) 0.0399 Uani ? ?
H(20) 0.406(9) 0.441(3) 0.433(9) 0.0399 Uani ? ?
H(21) 0.404(8) 0.434(3) 0.807(6) 0.0328 Uani ? ?
H(22) 0.440(8) 0.407(2) 0.900(6) 0.0328 Uani ? ?
H(23) 0.888(8) 0.160(3) 0.715(6) 0.0328 Uani ? ?
H(24) 0.895(9) 0.159(3) 0.588(6) 0.0328 Uani ? ?
H(25) 0.436(8) 0.508(2) 0.129(6) 0.0328 Uani ? ?
H(26) 0.36(1) 0.460(3) 0.184(8) 0.0328 Uani ? ?
H(27) 0.019(8) 0.450(2) 0.624(6) 0.0328 Uani ? ?
H(28) 0.245(10) 0.458(3) 0.598(7) 0.0328 Uani ? ?
H(29) -0.219(9) 0.471(3) 0.681(6) 0.0328 Uani ? ?
H(30) -0.25(1) 0.456(3) 0.570(7) 0.0328 Uani ? ?
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 40 0.003 0.002 'International Tables'
H 0 120 0.000 0.000 'International Tables'
N 0 16 0.006 0.003 'International Tables'
O 0 32 0.011 0.006 '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
1 -1 -1
1 1 -1
1 3 0
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
N(1) Ni(1) N(2) 85.0(2) ? ? ? yes
N(1) Ni(1) N(3) 176.2(2) ? ? ? yes
N(1) Ni(1) N(4) 94.1(2) ? ? ? yes
N(2) Ni(1) N(3) 95.9(2) ? ? ? yes
N(2) Ni(1) N(4) 177.8(2) ? ? ? yes
N(3) Ni(1) N(4) 84.8(2) ? ? ? yes
Ni(1) N(1) C(2) 129.4(4) ? ? ? yes
Ni(1) N(1) C(3) 114.6(4) ? ? ? yes
C(2) N(1) C(3) 115.9(4) ? ? ? yes
Ni(1) N(2) C(4) 105.8(3) ? ? ? yes
Ni(1) N(2) C(5) 120.7(3) ? ? ? yes
C(4) N(2) C(5) 111.1(4) ? ? ? yes
Ni(1) N(3) C(7) 121.5(3) ? ? ? yes
Ni(1) N(3) C(8) 107.2(3) ? ? ? yes
C(7) N(3) C(8) 109.8(4) ? ? ? yes
Ni(1) N(4) C(9) 114.9(4) ? ? ? yes
Ni(1) N(4) C(10) 130.1(4) ? ? ? yes
C(9) N(4) C(10) 114.8(4) ? ? ? yes
C(2) C(1) C(10) 123.0(5) ? ? ? yes
O(1) C(2) N(1) 123.2(5) ? ? ? yes
O(1) C(2) C(1) 115.2(5) ? ? ? yes
N(1) C(2) C(1) 121.6(5) ? ? ? yes
N(1) C(3) C(4) 106.6(4) ? ? ? yes
N(2) C(4) C(3) 109.0(5) ? ? ? yes
N(2) C(5) C(6) 112.4(5) ? ? ? yes
C(5) C(6) C(7) 110.8(5) ? ? ? yes
N(3) C(7) C(6) 112.7(5) ? ? ? yes
N(3) C(8) C(9) 108.1(5) ? ? ? yes
N(4) C(9) C(8) 107.3(4) ? ? ? yes
O(2) C(10) N(4) 124.3(5) ? ? ? yes
O(2) C(10) C(1) 115.3(5) ? ? ? yes
N(4) C(10) C(1) 120.4(5) ? ? ? 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) N(1) 1.895(4) ? ? yes
Ni(1) N(2) 1.947(4) ? ? yes
Ni(1) N(3) 1.935(4) ? ? yes
Ni(1) N(4) 1.882(4) ? ? yes
O(1) C(2) 1.294(6) ? ? yes
O(2) C(10) 1.277(6) ? ? yes
N(1) C(2) 1.301(7) ? ? yes
N(1) C(3) 1.478(6) ? ? yes
N(2) C(4) 1.480(7) ? ? yes
N(2) C(5) 1.473(7) ? ? yes
N(3) C(7) 1.489(7) ? ? yes
N(3) C(8) 1.480(7) ? ? yes
N(4) C(9) 1.475(6) ? ? yes
N(4) C(10) 1.308(7) ? ? yes
C(1) C(2) 1.488(7) ? ? yes
C(1) C(10) 1.512(7) ? ? yes
C(3) C(4) 1.499(8) ? ? yes
C(5) C(6) 1.528(8) ? ? yes
C(6) C(7) 1.502(8) ? ? yes
C(8) C(9) 1.499(8) ? ? yes
