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#$Date: 2016-03-23 00:57:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179137 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/99/4309937.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_4309937
loop_
_publ_author_name
'Yong Bok Go'
'Xiqu Wang'
'Ekaterina V. Anokhina'
'Allan J. Jacobson'
_publ_section_title
;
Influence of the Reaction Temperature and pH on the Coordination Modes of
the 1,4-Benzenedicarboxylate (BDC) Ligand: A Case Study of the
NiII(BDC)/2,2'-Bipyridine System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8265
_journal_page_last               8271
_journal_paper_doi               10.1021/ic050644d
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C28 H24 N4 Ni O6'
_chemical_formula_weight         571.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.266(2)
_cell_length_b                   10.6915(15)
_cell_length_c                   17.171(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2619.0(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15699
_diffrn_reflns_theta_full        28.73
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedra
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0430P)²+1.0206P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                2619
_reflns_number_total             3189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050644dsi20050426_020950_1.cif
_cod_data_source_block           5
_cod_original_cell_volume        2618.9(6)
_cod_database_code               4309937
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.96980(14) 0.45922(18) 0.11854(11) 0.0491(4) Uani 1 1 d . . .
H1 H 0.9076 0.4853 0.1196 0.059 Uiso 1 1 calc R . .
C2 C 0.99512(16) 0.3661(2) 0.06717(16) 0.0697(7) Uani 1 1 d . . .
H2 H 0.9512 0.3312 0.0335 0.084 Uiso 1 1 calc R . .
C3 C 1.08603(18) 0.3261(2) 0.06666(16) 0.0790(8) Uani 1 1 d . . .
H3 H 1.1044 0.2618 0.0335 0.095 Uiso 1 1 calc R . .
C4 C 1.15028(16) 0.3815(2) 0.11537(14) 0.0642(6) Uani 1 1 d . . .
H4 H 1.2125 0.3554 0.1155 0.077 Uiso 1 1 calc R . .
C5 C 1.12069(12) 0.47689(15) 0.16433(9) 0.0406(4) Uani 1 1 d . . .
C6 C 1.18562(11) 0.54664(15) 0.21587(9) 0.0396(3) Uani 1 1 d . . .
C7 C 1.28148(14) 0.5270(2) 0.21639(13) 0.0609(5) Uani 1 1 d . . .
H7 H 1.3080 0.4653 0.1852 0.073 Uiso 1 1 calc R . .
C8 C 1.33723(15) 0.5999(3) 0.26364(14) 0.0735(7) Uani 1 1 d . . .
H8 H 1.4019 0.5887 0.2641 0.088 Uiso 1 1 calc R . .
C9 C 1.29646(15) 0.6891(2) 0.31007(14) 0.0660(6) Uani 1 1 d . . .
H9 H 1.3328 0.7394 0.3424 0.079 Uiso 1 1 calc R . .
C10 C 1.20018(13) 0.70254(18) 0.30757(11) 0.0485(4) Uani 1 1 d . . .
H10 H 1.1724 0.7624 0.3394 0.058 Uiso 1 1 calc R . .
C11 C 1.05715(11) 0.81132(14) 0.11337(8) 0.0334(3) Uani 1 1 d . . .
C12 C 1.08541(11) 0.94029(15) -0.00745(10) 0.0397(3) Uani 1 1 d . . .
H12 H 1.1430 0.9005 -0.0128 0.048 Uiso 1 1 calc R . .
C13 C 1.02756(11) 0.91058(14) 0.05524(8) 0.0322(3) Uani 1 1 d . . .
C14 C 0.94219(12) 0.97149(15) 0.06172(9) 0.0397(4) Uani 1 1 d . . .
H14 H 0.9028 0.9527 0.1032 0.048 Uiso 1 1 calc R . .
O1 O 1.13377(8) 0.75915(12) 0.10377(7) 0.0498(3) Uani 1 1 d . . .
O2 O 0.99937(8) 0.79003(12) 0.16749(7) 0.0416(3) Uani 1 1 d . . .
O1W O 1.23013(16) 0.6454(2) -0.01508(14) 0.1140(8) Uani 1 1 d . . .
Ni1 Ni 1.0000 0.65248(2) 0.2500 0.02896(10) Uani 1 2 d S . .
N1 N 1.03071(10) 0.51366(12) 0.16695(7) 0.0364(3) Uani 1 1 d . . .
N2 N 1.14529(10) 0.63360(13) 0.26168(7) 0.0354(3) Uani 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'
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'
N N 0.0061 0.0033 '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'
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
N1 C1 C2 122.86(19) . . ?
C3 C2 C1 118.6(2) . . ?
C2 C3 C4 119.6(2) . . ?
C3 C4 C5 118.8(2) . . ?
N1 C5 C4 121.74(17) . . ?
N1 C5 C6 115.47(14) . . ?
C4 C5 C6 122.78(17) . . ?
N2 C6 C7 121.55(17) . . ?
N2 C6 C5 115.40(14) . . ?
C7 C6 C5 123.04(17) . . ?
C8 C7 C6 119.2(2) . . ?
C9 C8 C7 119.4(2) . . ?
C8 C9 C10 118.4(2) . . ?
N2 C10 C9 123.02(19) . . ?
O1 C11 O2 126.37(14) . . ?
O1 C11 C13 118.25(13) . . ?
O2 C11 C13 115.38(14) . . ?
C14 C12 C13 120.50(15) 5_775 . ?
C14 C13 C12 118.39(14) . . ?
C14 C13 C11 121.38(13) . . ?
C12 C13 C11 120.21(14) . . ?
C12 C14 C13 121.11(14) 5_775 . ?
C11 O2 Ni1 129.60(10) . . ?
O2 Ni1 O2 87.86(7) 3_755 . ?
O2 Ni1 N2 98.07(5) 3_755 3_755 ?
O2 Ni1 N2 89.92(5) . 3_755 ?
O2 Ni1 N2 89.92(5) 3_755 . ?
O2 Ni1 N2 98.07(5) . . ?
N2 Ni1 N2 168.93(8) 3_755 . ?
O2 Ni1 N1 167.73(5) 3_755 . ?
O2 Ni1 N1 92.22(5) . . ?
N2 Ni1 N1 94.20(5) 3_755 . ?
N2 Ni1 N1 77.92(5) . . ?
O2 Ni1 N1 92.22(5) 3_755 3_755 ?
O2 Ni1 N1 167.73(5) . 3_755 ?
N2 Ni1 N1 77.92(5) 3_755 3_755 ?
N2 Ni1 N1 94.20(5) . 3_755 ?
N1 Ni1 N1 90.30(7) . 3_755 ?
C1 N1 C5 118.24(15) . . ?
C1 N1 Ni1 126.41(12) . . ?
C5 N1 Ni1 115.34(10) . . ?
C10 N2 C6 118.42(16) . . ?
C10 N2 Ni1 125.82(12) . . ?
C6 N2 Ni1 115.71(11) . . ?
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
C1 N1 1.336(2) . ?
C1 C2 1.378(3) . ?
C2 C3 1.366(3) . ?
C3 C4 1.375(3) . ?
C4 C5 1.388(2) . ?
C5 N1 1.343(2) . ?
C5 C6 1.482(2) . ?
C6 N2 1.347(2) . ?
C6 C7 1.384(2) . ?
C7 C8 1.378(3) . ?
C8 C9 1.373(3) . ?
C9 C10 1.382(3) . ?
C10 N2 1.333(2) . ?
C11 O1 1.2381(19) . ?
C11 O2 1.2629(18) . ?
C11 C13 1.517(2) . ?
C12 C14 1.383(2) 5_775 ?
C12 C13 1.393(2) . ?
C13 C14 1.386(2) . ?
C14 C12 1.383(2) 5_775 ?
O2 Ni1 2.0421(11) . ?
Ni1 O2 2.0421(11) 3_755 ?
Ni1 N2 2.0921(15) 3_755 ?
Ni1 N2 2.0921(15) . ?
Ni1 N1 2.1043(13) . ?
Ni1 N1 2.1043(13) 3_755 ?
