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#$Date: 2016-03-22 11:50:55 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178919 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/48/4114846.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_4114846
loop_
_publ_author_name
'Juan C. Noveron'
'Myoung Soo Lah'
'Rico E. Del Sesto'
'Atta M. Arif'
'Joel S. Miller'
'Peter J. Stang'
_publ_section_title
;
 Engineering the Structure and Magnetic Properties of Crystalline Solids
 via the Metal-Directed Self-Assembly of a Versatile Molecular Building
 Unit
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6613
_journal_page_last               6625
_journal_paper_doi               10.1021/ja0200241
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C26 H28 N6 Ni O10'
_chemical_formula_weight         643.25
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.618(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4380(2)
_cell_length_b                   12.6144(5)
_cell_length_c                   14.7117(5)
_cell_measurement_reflns_used    12836
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.02
_cell_volume                     1368.16(8)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      200(1)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi plus Omega 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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5081
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.9262
_exptl_absorpt_correction_T_min  0.8598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & MInor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0362
_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)+(0.0361P)²+0.4700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                2373
_reflns_number_total             3122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0200241_08.cif
_cod_data_source_block           Ni_complex8
_cod_original_cell_volume        1368.15(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4114846
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
Ni1 Ni 1.0000 0.0000 0.0000 0.02045(12) Uani 1 2 d S
O1 O 0.7961(2) -0.15036(11) 0.44143(10) 0.0359(4) Uani 1 1 d .
O2 O 1.17678(19) 0.12514(12) 0.04059(10) 0.0280(3) Uani 1 1 d .
O3 O 0.77586(18) 0.09161(10) -0.05247(9) 0.0285(3) Uani 1 1 d .
O4 O 0.8917(2) 0.25079(11) -0.04384(11) 0.0376(4) Uani 1 1 d .
O5 O 0.6239(2) 0.22405(13) -0.11589(11) 0.0420(4) Uani 1 1 d .
N1 N 0.9108(2) 0.00488(12) 0.12747(11) 0.0227(3) Uani 1 1 d .
N2 N 0.7922(2) 0.02200(14) 0.39835(11) 0.0263(4) Uani 1 1 d .
N3 N 0.7637(2) 0.18938(13) -0.07095(11) 0.0264(4) Uani 1 1 d .
C1 C 0.9028(3) -0.08291(17) 0.17812(14) 0.0287(4) Uani 1 1 d .
C2 C 0.8629(3) -0.08446(16) 0.26699(14) 0.0281(4) Uani 1 1 d .
C3 C 0.8281(2) 0.01103(15) 0.30856(13) 0.0227(4) Uani 1 1 d .
C4 C 0.8299(3) 0.10261(17) 0.25487(14) 0.0290(5) Uani 1 1 d .
C5 C 0.8716(3) 0.09627(16) 0.16737(14) 0.0269(4) Uani 1 1 d .
C6 C 0.7757(2) -0.05727(16) 0.46050(13) 0.0240(4) Uani 1 1 d .
C7 C 0.7300(2) -0.02450(16) 0.55239(13) 0.0245(4) Uani 1 1 d .
C8 C 0.7289(3) -0.1041(2) 0.61787(15) 0.0377(5) Uani 1 1 d .
C9 C 0.6850(3) -0.0815(2) 0.70426(16) 0.0428(6) Uani 1 1 d .
C10 C 0.6419(3) 0.0200(2) 0.72648(15) 0.0376(6) Uani 1 1 d .
C11 C 0.6403(3) 0.1000(2) 0.66189(16) 0.0391(5) Uani 1 1 d .
C12 C 0.6836(3) 0.07743(18) 0.57494(15) 0.0339(5) Uani 1 1 d .
C13 C 1.3686(3) 0.1265(2) 0.03804(19) 0.0370(5) Uani 1 1 d .
H2N H 0.780(3) 0.082(2) 0.4135(15) 0.031(6) Uiso 1 1 d .
H2O H 1.141(4) 0.179(2) 0.0305(19) 0.051(9) Uiso 1 1 d .
H1 H 0.932(3) -0.1484(18) 0.1509(15) 0.033(6) Uiso 1 1 d .
H2 H 0.861(3) -0.1498(17) 0.2991(15) 0.031(6) Uiso 1 1 d .
H4 H 0.801(3) 0.1652(18) 0.2782(14) 0.031(6) Uiso 1 1 d .
H5 H 0.878(3) 0.1589(17) 0.1342(14) 0.025(5) Uiso 1 1 d .
H8 H 0.753(3) -0.170(2) 0.6030(17) 0.050(8) Uiso 1 1 d .
H9 H 0.684(4) -0.135(2) 0.7467(19) 0.059(8) Uiso 1 1 d .
H10 H 0.614(3) 0.0370(19) 0.7842(17) 0.038(6) Uiso 1 1 d .
H11 H 0.605(3) 0.169(2) 0.6754(17) 0.048(7) Uiso 1 1 d .
H12 H 0.682(3) 0.1330(18) 0.5298(16) 0.040(6) Uiso 1 1 d .
H13A H 1.422(4) 0.188(3) 0.060(2) 0.077(10) Uiso 1 1 d .
H13B H 1.424(4) 0.066(3) 0.072(2) 0.067(9) Uiso 1 1 d .
H13C H 1.397(4) 0.116(2) -0.021(2) 0.077(10) Uiso 1 1 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'
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
N1 Ni1 N1 180.00(8) 3_755 .
N1 Ni1 O2 89.07(6) 3_755 3_755
N1 Ni1 O2 90.93(6) . 3_755
N1 Ni1 O2 90.93(6) 3_755 .
N1 Ni1 O2 89.07(6) . .
O2 Ni1 O2 180.00(5) 3_755 .
N1 Ni1 O3 91.01(6) 3_755 .
N1 Ni1 O3 88.99(6) . .
O2 Ni1 O3 82.61(6) 3_755 .
O2 Ni1 O3 97.39(6) . .
N1 Ni1 O3 88.99(6) 3_755 3_755
N1 Ni1 O3 91.01(6) . 3_755
O2 Ni1 O3 97.39(6) 3_755 3_755
O2 Ni1 O3 82.61(6) . 3_755
O3 Ni1 O3 180.00(9) . 3_755
C13 O2 Ni1 126.34(14) . .
C13 O2 H2O 109(2) . .
Ni1 O2 H2O 116(2) . .
N3 O3 Ni1 130.54(12) . .
C1 N1 C5 115.96(16) . .
C1 N1 Ni1 121.47(12) . .
C5 N1 Ni1 122.37(13) . .
C6 N2 C3 127.37(18) . .
C6 N2 H2N 118.9(16) . .
C3 N2 H2N 113.7(16) . .
O5 N3 O4 120.15(17) . .
O5 N3 O3 119.46(17) . .
O4 N3 O3 120.39(16) . .
N1 C1 C2 124.75(19) . .
N1 C1 H1 116.8(13) . .
C2 C1 H1 118.4(13) . .
C1 C2 C3 118.74(19) . .
C1 C2 H2 120.2(13) . .
C3 C2 H2 121.1(13) . .
N2 C3 C2 125.11(17) . .
N2 C3 C4 118.14(17) . .
C2 C3 C4 116.76(17) . .
C5 C4 C3 120.23(19) . .
C5 C4 H4 120.5(14) . .
C3 C4 H4 119.3(14) . .
N1 C5 C4 123.49(19) . .
N1 C5 H5 117.9(12) . .
C4 C5 H5 118.5(12) . .
O1 C6 N2 121.53(18) . .
O1 C6 C7 121.57(17) . .
N2 C6 C7 116.90(17) . .
C12 C7 C8 118.70(19) . .
C12 C7 C6 124.59(18) . .
C8 C7 C6 116.67(18) . .
C9 C8 C7 120.7(2) . .
C9 C8 H8 120.1(16) . .
C7 C8 H8 119.2(16) . .
C10 C9 C8 120.2(2) . .
C10 C9 H9 120.3(17) . .
C8 C9 H9 119.5(17) . .
C9 C10 C11 119.9(2) . .
C9 C10 H10 121.6(15) . .
C11 C10 H10 118.6(15) . .
C10 C11 C12 120.1(2) . .
C10 C11 H11 120.5(16) . .
C12 C11 H11 119.4(16) . .
C7 C12 C11 120.4(2) . .
C7 C12 H12 119.4(14) . .
C11 C12 H12 120.2(14) . .
O2 C13 H13A 112.8(18) . .
O2 C13 H13B 109.1(16) . .
H13A C13 H13B 110(2) . .
O2 C13 H13C 112.0(19) . .
H13A C13 H13C 109(2) . .
H13B C13 H13C 104(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.0713(15) 3_755
Ni1 N1 2.0713(15) .
Ni1 O2 2.0903(14) 3_755
Ni1 O2 2.0903(14) .
Ni1 O3 2.0903(13) .
Ni1 O3 2.0903(13) 3_755
O1 C6 1.222(2) .
O2 C13 1.432(3) .
O2 H2O 0.73(3) .
O3 N3 1.264(2) .
O4 N3 1.251(2) .
O5 N3 1.236(2) .
N1 C1 1.340(2) .
N1 C5 1.343(2) .
N2 C6 1.371(3) .
N2 C3 1.389(2) .
N2 H2N 0.80(2) .
C1 C2 1.379(3) .
C1 H1 0.96(2) .
C2 C3 1.391(3) .
C2 H2 0.95(2) .
C3 C4 1.400(3) .
C4 C5 1.366(3) .
C4 H4 0.90(2) .
C5 H5 0.93(2) .
C6 C7 1.495(3) .
C7 C12 1.383(3) .
C7 C8 1.393(3) .
C8 C9 1.383(3) .
C8 H8 0.89(3) .
C9 C10 1.370(3) .
C9 H9 0.92(3) .
C10 C11 1.384(3) .
C10 H10 0.93(2) .
C11 C12 1.389(3) .
C11 H11 0.94(3) .
C12 H12 0.96(2) .
C13 H13A 0.92(3) .
C13 H13B 0.98(3) .
C13 H13C 0.93(3) .
