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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/48/4114849.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_4114849
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 Co0.5 N6 Ni0.5 O10'
_chemical_formula_weight         643.36
_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                 97.8068(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4425(3)
_cell_length_b                   12.6362(5)
_cell_length_c                   14.7425(8)
_cell_measurement_reflns_used    3090
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     1373.61(11)
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0953
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5869
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.99
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.9301
_exptl_absorpt_correction_T_min  0.8669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red-green
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       prism
_exptl_crystal_F_000             667
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0481
_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)+(0.0340P)²+0.0406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                1975
_reflns_number_total             3162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0200241_11.cif
_cod_data_source_block           Co_Ni_Complex11
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C26 H28 Co0.50 N6 Ni0.50 O10'
_cod_database_code               4114849
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 0.01794(17) Uani 0.4840(12) 2 d SP
Co1 Co 1.0000 0.0000 0.0000 0.01794(17) Uani 0.4840(12) 2 d SP
O1 O 0.7719(2) 0.09256(11) -0.05231(11) 0.0279(5) Uani 1 1 d .
O2 O 0.8884(3) 0.25142(12) -0.04467(13) 0.0382(5) Uani 1 1 d .
O3 O 0.6208(3) 0.22471(14) -0.11715(14) 0.0426(6) Uani 1 1 d .
O4 O 0.8229(2) -0.12644(13) -0.03953(12) 0.0273(5) Uani 1 1 d .
O5 O 0.7971(3) -0.15024(12) 0.44196(12) 0.0347(5) Uani 1 1 d .
N1 N 0.7598(3) 0.19011(16) -0.07182(14) 0.0266(5) Uani 1 1 d .
N2 N 0.9093(3) 0.00467(14) 0.12835(13) 0.0230(5) Uani 1 1 d .
N3 N 0.7924(3) 0.02213(15) 0.39882(14) 0.0240(5) Uani 1 1 d .
C1 C 0.6307(4) -0.1274(2) -0.0386(3) 0.0375(8) Uani 1 1 d .
C2 C 0.9039(4) -0.08259(19) 0.17976(17) 0.0277(6) Uani 1 1 d .
C3 C 0.8639(4) -0.08430(19) 0.26776(17) 0.0279(6) Uani 1 1 d .
C4 C 0.8275(3) 0.01100(16) 0.30913(16) 0.0207(5) Uani 1 1 d .
C5 C 0.8274(4) 0.10225(18) 0.25526(18) 0.0283(7) Uani 1 1 d .
C6 C 0.8684(4) 0.09561(18) 0.16841(17) 0.0253(6) Uani 1 1 d .
C7 C 0.7758(3) -0.05748(18) 0.46094(16) 0.0230(6) Uani 1 1 d .
C8 C 0.7310(3) -0.02503(17) 0.55258(17) 0.0225(6) Uani 1 1 d .
C9 C 0.7293(4) -0.1039(2) 0.61818(19) 0.0348(7) Uani 1 1 d .
C10 C 0.6867(4) -0.0818(2) 0.7039(2) 0.0404(8) Uani 1 1 d .
C11 C 0.6422(4) 0.0197(2) 0.7261(2) 0.0367(7) Uani 1 1 d .
C12 C 0.6414(4) 0.0992(2) 0.66156(19) 0.0370(7) Uani 1 1 d .
C13 C 0.6833(4) 0.0772(2) 0.57507(19) 0.0323(7) Uani 1 1 d .
H1A H 0.576(4) -0.188(3) -0.066(2) 0.073(11) Uiso 1 1 d .
H1B H 0.576(4) -0.057(3) -0.066(2) 0.073(10) Uiso 1 1 d .
H1C H 0.606(6) -0.127(3) 0.027(3) 0.134(18) Uiso 1 1 d .
H2 H 0.932(4) -0.147(2) 0.1528(18) 0.048(8) Uiso 1 1 d .
H3 H 0.866(3) -0.1507(17) 0.3000(16) 0.031(7) Uiso 1 1 d .
H3N H 0.779(4) 0.088(2) 0.4193(19) 0.045(8) Uiso 1 1 d .
H4 H 0.862(4) -0.186(3) -0.034(2) 0.065(12) Uiso 1 1 d .
H5 H 0.797(3) 0.1652(19) 0.2789(16) 0.032(7) Uiso 1 1 d .
H6 H 0.874(3) 0.1606(18) 0.1323(16) 0.029(7) Uiso 1 1 d .
H9 H 0.760(4) -0.170(2) 0.6017(18) 0.050(9) Uiso 1 1 d .
H10 H 0.685(4) -0.139(2) 0.749(2) 0.059(9) Uiso 1 1 d .
H11 H 0.612(3) 0.0378(16) 0.7835(16) 0.014(6) Uiso 1 1 d .
H12 H 0.607(4) 0.172(2) 0.6738(19) 0.052(9) Uiso 1 1 d .
H13 H 0.684(3) 0.1310(18) 0.5274(18) 0.034(7) 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'
Co Co 0.3494 0.9721 '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
N2 Ni1 N2 180.00(10) 3_755 .
N2 Ni1 O4 89.71(7) 3_755 .
N2 Ni1 O4 90.29(7) . .
N2 Ni1 O4 90.29(7) 3_755 3_755
N2 Ni1 O4 89.71(7) . 3_755
O4 Ni1 O4 180.00(11) . 3_755
N2 Ni1 O1 88.44(7) 3_755 3_755
N2 Ni1 O1 91.56(7) . 3_755
O4 Ni1 O1 97.04(7) . 3_755
O4 Ni1 O1 82.96(7) 3_755 3_755
N2 Ni1 O1 91.56(7) 3_755 .
N2 Ni1 O1 88.44(7) . .
O4 Ni1 O1 82.96(7) . .
O4 Ni1 O1 97.04(7) 3_755 .
O1 Ni1 O1 180.00(12) 3_755 .
N1 O1 Ni1 130.47(15) . .
C1 O4 Ni1 126.37(16) . .
C1 O4 H4 110(2) . .
Ni1 O4 H4 118(2) . .
O3 N1 O2 120.1(2) . .
O3 N1 O1 119.8(2) . .
O2 N1 O1 120.1(2) . .
C2 N2 C6 115.3(2) . .
C2 N2 Ni1 121.69(15) . .
C6 N2 Ni1 122.71(16) . .
C7 N3 C4 127.19(19) . .
C7 N3 H3N 115.5(18) . .
C4 N3 H3N 117.3(18) . .
O4 C1 H1A 112(2) . .
O4 C1 H1B 109.0(17) . .
H1A C1 H1B 114(3) . .
O4 C1 H1C 109(3) . .
H1A C1 H1C 107(3) . .
H1B C1 H1C 106(3) . .
N2 C2 C3 125.1(2) . .
N2 C2 H2 116.7(16) . .
C3 C2 H2 118.2(16) . .
C2 C3 C4 118.8(2) . .
C2 C3 H3 119.2(14) . .
C4 C3 H3 121.9(14) . .
N3 C4 C3 125.2(2) . .
N3 C4 C5 118.1(2) . .
C3 C4 C5 116.7(2) . .
C6 C5 C4 120.1(2) . .
C6 C5 H5 121.0(15) . .
C4 C5 H5 119.0(15) . .
N2 C6 C5 124.0(2) . .
N2 C6 H6 116.6(14) . .
C5 C6 H6 119.3(14) . .
O5 C7 N3 121.5(2) . .
O5 C7 C8 121.6(2) . .
N3 C7 C8 116.9(2) . .
C9 C8 C13 118.2(2) . .
C9 C8 C7 117.2(2) . .
C13 C8 C7 124.5(2) . .
C10 C9 C8 121.3(3) . .
C10 C9 H9 122.3(18) . .
C8 C9 H9 116.4(18) . .
C9 C10 C11 120.2(3) . .
C9 C10 H10 119.8(17) . .
C11 C10 H10 120.0(17) . .
C10 C11 C12 119.5(3) . .
C10 C11 H11 122.7(13) . .
C12 C11 H11 117.9(13) . .
C13 C12 C11 120.6(3) . .
C13 C12 H12 117.3(17) . .
C11 C12 H12 122.1(17) . .
C12 C13 C8 120.2(2) . .
C12 C13 H13 123.2(14) . .
C8 C13 H13 116.5(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 2.0944(19) 3_755
Ni1 N2 2.0944(19) .
Ni1 O4 2.1027(16) .
Ni1 O4 2.1027(16) 3_755
Ni1 O1 2.1185(16) 3_755
Ni1 O1 2.1185(16) .
O1 N1 1.266(2) .
O2 N1 1.254(3) .
O3 N1 1.232(3) .
O4 C1 1.432(3) .
O4 H4 0.80(3) .
O5 C7 1.220(3) .
N2 C2 1.342(3) .
N2 C6 1.346(3) .
N3 C7 1.377(3) .
N3 C4 1.389(3) .
N3 H3N 0.89(3) .
C1 H1A 0.94(3) .
C1 H1B 1.04(3) .
C1 H1C 1.01(5) .
C2 C3 1.370(3) .
C2 H2 0.95(3) .
C3 C4 1.393(3) .
C3 H3 0.96(2) .
C4 C5 1.400(3) .
C5 C6 1.359(3) .
C5 H5 0.91(2) .
C6 H6 0.98(2) .
C7 C8 1.492(3) .
C8 C9 1.390(3) .
C8 C13 1.392(3) .
C9 C10 1.373(4) .
C9 H9 0.90(3) .
C10 C11 1.375(4) .
C10 H10 0.99(3) .
C11 C12 1.383(4) .
C11 H11 0.93(2) .
C12 C13 1.381(4) .
C12 H12 0.97(3) .
C13 H13 0.98(2) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3N O2 0.89(3) 2.22(3) 3.038(3) 151(2) 4_566
O4 H4 O5 0.80(3) 2.15(3) 2.839(2) 144(3) 4
