#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/52/7205240.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_7205240
loop_
_publ_author_name
'Tian, Dan'
'Pang, Yu'
'Zhou, Yan-Hong'
'Guan, Li'
'Zhang, Hong'
_publ_section_title
;
 A series of complexes based on
 biphenyl-2,5,2′,5′-tetracarboxylic acid: syntheses,
 crystal structures, luminescent and magnetic properties
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              957
_journal_paper_doi               10.1039/c0ce00281j
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C16 H40 Ni2 O25'
_chemical_formula_sum            'C16 H40 Ni2 O25'
_chemical_formula_weight         749.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.968(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1584(5)
_cell_length_b                   17.1511(5)
_cell_length_c                   14.6293(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      4.35
_cell_volume                     3140.5(2)
_computing_cell_refinement       'SMART (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'BRUKER SMART CCD Apex II'
_diffrn_measurement_method       'omega and phi'
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6052
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.35
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2754
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0351
_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)+(0.0426P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                1901
_reflns_number_total             2754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00281J.TXT
_cod_data_source_block           complex-2
_cod_original_cell_volume        3140.53(18)
_cod_original_sg_symbol_Hall     C2/c
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7205240
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
O3 O 0.66403(17) 0.82829(12) 0.14498(17) 0.0360(6) Uani 1 1 d . . .
O7W O 0.5000 0.4108(3) 0.2500 0.133(2) Uani 1 2 d S . .
Ni1 Ni 0.75399(3) 0.73556(2) 0.15827(3) 0.02400(14) Uani 1 1 d D . .
O1 O 0.96485(17) 0.72684(12) 0.11768(17) 0.0358(6) Uani 1 1 d . . .
C3 C 1.0231(2) 0.53114(15) 0.2098(2) 0.0192(6) Uani 1 1 d . . .
C1 C 0.9397(2) 0.66167(17) 0.1422(2) 0.0243(7) Uani 1 1 d . . .
C2 C 1.0121(2) 0.59345(16) 0.1451(2) 0.0204(7) Uani 1 1 d . . .
C8 C 0.6918(3) 0.89232(18) 0.1138(2) 0.0292(8) Uani 1 1 d . . .
C4 C 1.0814(2) 0.46641(17) 0.1971(2) 0.0241(7) Uani 1 1 d . . .
H4 H 1.0863 0.4234 0.2370 0.029 Uiso 1 1 calc R . .
C7 C 1.0665(2) 0.59205(17) 0.0780(2) 0.0277(7) Uani 1 1 d . . .
H7 H 1.0620 0.6348 0.0379 0.033 Uiso 1 1 calc R . .
C6 C 1.1275(2) 0.52866(18) 0.0692(2) 0.0301(8) Uani 1 1 d . . .
H6 H 1.1651 0.5295 0.0248 0.036 Uiso 1 1 calc R . .
O5W O 0.7531(2) 0.35235(16) 0.1059(2) 0.0611(8) Uani 1 1 d . . .
O3W O 0.6625(4) 0.6604(3) 0.2311(3) 0.0833(14) Uani 1 1 d D . .
C5 C 1.1323(2) 0.46383(16) 0.1268(2) 0.0237(7) Uani 1 1 d . . .
O8W O 0.6269(3) 0.3524(2) 0.9145(3) 0.0994(12) Uani 1 1 d . . .
O4W O 0.7133(4) 0.5113(2) 0.1056(3) 0.1207(16) Uani 1 1 d . . .
O4 O 0.7619(2) 0.89762(14) 0.0746(2) 0.0524(7) Uani 1 1 d . . .
O2W O 0.66287(19) 0.69543(13) 0.03494(17) 0.0383(6) Uani 1 1 d . . .
H2WA H 0.6965 0.6637 0.0138 0.057 Uiso 1 1 calc R . .
O1W O 0.8454(2) 0.78337(16) 0.2771(2) 0.0534(8) Uani 1 1 d . . .
H1WA H 0.8887 0.7511 0.3076 0.080 Uiso 1 1 calc R . .
O9W O 0.4985(9) 0.4785(5) 0.8897(8) 0.312(6) Uani 1 1 d . . .
O6W O 0.9568(3) 0.2902(2) 0.1472(3) 0.0761(10) Uani 1 1 d . . .
O2 O 0.85291(16) 0.64911(12) 0.16127(16) 0.0300(5) Uani 1 1 d . . .
H2WB H 0.616(4) 0.729(3) -0.011(4) 0.11(2) Uiso 1 1 d . . .
H1WB H 0.811(6) 0.805(4) 0.319(5) 0.17(3) Uiso 1 1 d . . .
H6WB H 0.927(4) 0.240(3) 0.113(4) 0.088(16) Uiso 1 1 d . . .
H6WA H 1.029(8) 0.288(5) 0.160(7) 0.24(5) Uiso 1 1 d . . .
H3WA H 0.656(4) 0.653(3) 0.269(3) 0.046(16) 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'
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
C8 O3 Ni1 120.0(2) . . ?
O3 Ni1 O2W 90.83(10) . . ?
O3 Ni1 O1W 86.28(10) . . ?
O2W Ni1 O1W 175.68(12) . . ?
O3 Ni1 O2 172.89(10) . . ?
O2W Ni1 O2 88.19(9) . . ?
O1W Ni1 O2 94.28(10) . . ?
O3 Ni1 O3W 96.75(15) . . ?
O2W Ni1 O3W 88.27(15) . . ?
O1W Ni1 O3W 95.25(16) . . ?
O2 Ni1 O3W 90.26(14) . . ?
C4 C3 C2 117.6(3) . . ?
C4 C3 C3 118.9(2) . 2_755 ?
C2 C3 C3 123.6(2) . 2_755 ?
O1 C1 O2 123.3(3) . . ?
O1 C1 C2 118.9(3) . . ?
O2 C1 C2 117.8(3) . . ?
C7 C2 C3 119.8(3) . . ?
C7 C2 C1 117.2(3) . . ?
C3 C2 C1 123.0(3) . . ?
O4 C8 O3 124.4(3) . . ?
O4 C8 C5 119.7(3) . 3_455 ?
O3 C8 C5 115.9(3) . 3_455 ?
C5 C4 C3 122.3(3) . . ?
C5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C6 C7 C2 121.5(3) . . ?
C6 C7 H7 119.2 . . ?
C2 C7 H7 119.2 . . ?
C7 C6 C5 119.7(3) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
Ni1 O3W H3WA 144(5) . . ?
C6 C5 C4 118.8(3) . . ?
C6 C5 C8 120.5(3) . 3_545 ?
C4 C5 C8 120.7(3) . 3_545 ?
Ni1 O2W H2WA 109.5 . . ?
Ni1 O2W H2WB 121(3) . . ?
H2WA O2W H2WB 115.8 . . ?
Ni1 O1W H1WA 109.5 . . ?
Ni1 O1W H1WB 117(4) . . ?
H1WA O1W H1WB 108.1 . . ?
H6WB O6W H6WA 107(6) . . ?
C1 O2 Ni1 119.98(19) . . ?
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
O3 C8 1.285(4) . ?
O3 Ni1 1.956(2) . ?
Ni1 O2W 1.958(2) . ?
Ni1 O1W 1.963(2) . ?
Ni1 O2 1.965(2) . ?
Ni1 O3W 2.244(4) . ?
O1 C1 1.249(4) . ?
C3 C4 1.394(4) . ?
C3 C2 1.405(4) . ?
C3 C3 1.482(6) 2_755 ?
C1 O2 1.275(4) . ?
C1 C2 1.501(4) . ?
C2 C7 1.382(4) . ?
C8 O4 1.229(4) . ?
C8 C5 1.499(4) 3_455 ?
C4 C5 1.391(4) . ?
C4 H4 0.9300 . ?
C7 C6 1.380(4) . ?
C7 H7 0.9300 . ?
C6 C5 1.385(4) . ?
C6 H6 0.9300 . ?
O3W H3WA 0.60(5) . ?
C5 C8 1.499(4) 3_545 ?
O2W H2WA 0.8200 . ?
O2W H2WB 0.95(6) . ?
O1W H1WA 0.8200 . ?
O1W H1WB 0.94(8) . ?
O6W H6WB 1.01(5) . ?
O6W H6WA 0.91(10) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 O3 Ni1 O2W -98.4(2) . . . . ?
C8 O3 Ni1 O1W 78.4(2) . . . . ?
C8 O3 Ni1 O2 -16.4(9) . . . . ?
C8 O3 Ni1 O3W 173.3(3) . . . . ?
C4 C3 C2 C7 -6.0(4) . . . . ?
C3 C3 C2 C7 173.6(3) 2_755 . . . ?
C4 C3 C2 C1 171.5(3) . . . . ?
C3 C3 C2 C1 -8.9(5) 2_755 . . . ?
O1 C1 C2 C7 -33.4(4) . . . . ?
O2 C1 C2 C7 143.8(3) . . . . ?
O1 C1 C2 C3 149.0(3) . . . . ?
O2 C1 C2 C3 -33.8(4) . . . . ?
Ni1 O3 C8 O4 13.7(4) . . . . ?
Ni1 O3 C8 C5 -166.71(19) . . . 3_455 ?
C2 C3 C4 C5 3.3(4) . . . . ?
C3 C3 C4 C5 -176.2(3) 2_755 . . . ?
C3 C2 C7 C6 3.5(4) . . . . ?
C1 C2 C7 C6 -174.1(3) . . . . ?
C2 C7 C6 C5 1.8(5) . . . . ?
C7 C6 C5 C4 -4.4(4) . . . . ?
C7 C6 C5 C8 175.8(3) . . . 3_545 ?
C3 C4 C5 C6 1.8(4) . . . . ?
C3 C4 C5 C8 -178.3(3) . . . 3_545 ?
O1 C1 O2 Ni1 -2.7(4) . . . . ?
C2 C1 O2 Ni1 -179.75(18) . . . . ?
O3 Ni1 O2 C1 21.8(9) . . . . ?
O2W Ni1 O2 C1 104.0(2) . . . . ?
O1W Ni1 O2 C1 -72.5(2) . . . . ?
O3W Ni1 O2 C1 -167.8(2) . . . . ?
