#------------------------------------------------------------------------------
#$Date: 2017-02-04 15:49:48 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191595 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/12/7041296.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_7041296
loop_
_publ_author_name
'Zhou, Xinhui'
'Chen, Qianqian'
'Liu, Baolin'
'Li, Liang'
'Yang, Tao'
'Huang, Wei'
_publ_section_title
;
 Syntheses, structures and magnetic properties of nine coordination
 polymers based on terphenyl-tetracarboxylic acid ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              430
_journal_page_last               444
_journal_paper_doi               10.1039/c6dt04270h
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C46 H28 N4 Ni2 O9'
_chemical_formula_weight         898.14
_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
_audit_update_record
;
2016-04-19 deposited with the CCDC.
2016-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.257(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8839(15)
_cell_length_b                   15.7369(18)
_cell_length_c                   19.059(2)
_cell_measurement_reflns_used    1936
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.3
_cell_measurement_theta_min      2.0
_cell_volume                     4053.2(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_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    0.0417
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11989
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.9073
_exptl_absorpt_correction_T_min  0.8902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3457
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0708
_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)+(0.0744P)²+26.9418P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1887
_reflns_number_gt                2822
_reflns_number_total             3457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt04270h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7041290--7041299.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7041296
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
Ni1 Ni 0.12927(5) 0.85221(5) 0.77361(3) 0.0276(3) Uani 1 1 d .
C1 C 0.1743(8) 0.7040(7) 0.8864(6) 0.096(3) Uani 1 1 d U
H1 H 0.1084 0.6878 0.8707 0.115 Uiso 1 1 calc R
C2 C 0.2371(11) 0.6527(8) 0.9393(7) 0.125(4) Uani 1 1 d U
H2 H 0.2125 0.6052 0.9584 0.150 Uiso 1 1 calc R
C3 C 0.3342(10) 0.6750(9) 0.9613(7) 0.124(4) Uani 1 1 d U
H3 H 0.3773 0.6428 0.9957 0.149 Uiso 1 1 calc R
C4 C 0.3681(8) 0.7475(8) 0.9313(6) 0.097(3) Uani 1 1 d U
C5 C 0.4699(9) 0.7745(10) 0.9497(7) 0.120(4) Uani 1 1 d U
H5 H 0.5158 0.7439 0.9835 0.144 Uiso 1 1 calc R
C6 C 0.5001(9) 0.8451(10) 0.9177(7) 0.123(4) Uani 1 1 d U
H6 H 0.5663 0.8612 0.9297 0.147 Uiso 1 1 calc R
C7 C 0.4322(7) 0.8929(8) 0.8674(6) 0.094(3) Uani 1 1 d U
C8 C 0.4576(9) 0.9680(9) 0.8349(7) 0.115(4) Uani 1 1 d U
H8 H 0.5221 0.9884 0.8473 0.138 Uiso 1 1 calc R
C9 C 0.3877(8) 1.0105(8) 0.7855(7) 0.104(3) Uani 1 1 d U
H9 H 0.4042 1.0592 0.7633 0.125 Uiso 1 1 calc R
C10 C 0.2895(6) 0.9791(6) 0.7685(5) 0.077(2) Uani 1 1 d U
H10 H 0.2424 1.0071 0.7335 0.092 Uiso 1 1 calc R
C11 C 0.3320(6) 0.8684(6) 0.8471(4) 0.066(2) Uani 1 1 d U
C12 C 0.3002(6) 0.7933(6) 0.8791(5) 0.072(2) Uani 1 1 d U
C13 C 0.0015(4) 0.9420(3) 0.6448(3) 0.0245(11) Uani 1 1 d U
C14 C 0.0022(4) 0.9784(3) 0.5715(3) 0.0225(11) Uani 1 1 d U
C15 C -0.0694(4) 1.0352(3) 0.5356(3) 0.0254(11) Uani 1 1 d U
C16 C -0.0710(4) 1.0551(3) 0.4638(3) 0.0253(11) Uani 1 1 d U
H16 H -0.1195 1.0917 0.4389 0.030 Uiso 1 1 calc R
C17 C -0.1410(4) 1.0791(4) 0.5709(3) 0.0293(12) Uani 1 1 d U
C18 C -0.1078(5) 1.1244(5) 0.6341(4) 0.0499(17) Uani 1 1 d U
H18 H -0.0409 1.1236 0.6566 0.060 Uiso 1 1 calc R
C19 C -0.1725(5) 1.1709(5) 0.6644(4) 0.0545(18) Uani 1 1 d U
H19 H -0.1484 1.2031 0.7056 0.065 Uiso 1 1 calc R
C20 C -0.2406(5) 1.0773(5) 0.5419(4) 0.0531(18) Uani 1 1 d U
H20 H -0.2650 1.0468 0.4998 0.064 Uiso 1 1 calc R
C21 C -0.3058(5) 1.1206(5) 0.5746(4) 0.059(2) Uani 1 1 d U
H21 H -0.3735 1.1160 0.5554 0.071 Uiso 1 1 calc R
C22 C -0.2729(5) 1.1695(4) 0.6339(3) 0.0423(15) Uani 1 1 d U
C23 C -0.3435(5) 1.2188(4) 0.6680(4) 0.0452(16) Uani 1 1 d U
N1 N 0.2036(4) 0.7727(4) 0.8583(3) 0.0568(16) Uani 1 1 d .
N2 N 0.2630(4) 0.9142(4) 0.7990(3) 0.0510(15) Uani 1 1 d .
O1 O 0.0826(3) 0.9313(3) 0.6883(2) 0.0375(10) Uani 1 1 d .
O2 O -0.0824(3) 0.9212(3) 0.6523(2) 0.0407(10) Uani 1 1 d .
O3 O -0.3064(4) 1.2761(3) 0.7099(3) 0.0621(14) Uani 1 1 d .
O4 O -0.4324(4) 1.1994(4) 0.6537(3) 0.0800(19) Uani 1 1 d .
O5 O 0.0000 0.7795(3) 0.7500 0.0331(12) Uani 1 2 d S
H5A H -0.0558 0.7940 0.7239 0.040 Uiso 0.50 1 d PR
H5B H 0.0091 0.7274 0.7417 0.040 Uiso 0.50 1 d PR
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
O2 Ni1 O1 97.81(18) 2_556 .
O2 Ni1 O3 171.7(2) 2_556 3_545
O1 Ni1 O3 89.2(2) . 3_545
O2 Ni1 N2 89.9(2) 2_556 .
O1 Ni1 N2 90.1(2) . .
O3 Ni1 N2 85.7(2) 3_545 .
O2 Ni1 O5 92.69(14) 2_556 .
O1 Ni1 O5 93.59(14) . .
O3 Ni1 O5 91.25(18) 3_545 .
N2 Ni1 O5 175.1(2) . .
O2 Ni1 N1 87.9(2) 2_556 .
O1 Ni1 N1 169.6(2) . .
O3 Ni1 N1 84.5(2) 3_545 .
N2 Ni1 N1 81.1(2) . .
O5 Ni1 N1 94.9(2) . .
N1 C1 C2 124.1(11) . .
N1 C1 H1 118.0 . .
C2 C1 H1 118.0 . .
C3 C2 C1 118.3(13) . .
C3 C2 H2 120.9 . .
C1 C2 H2 120.9 . .
C2 C3 C4 118.9(12) . .
C2 C3 H3 120.5 . .
C4 C3 H3 120.5 . .
C12 C4 C3 118.2(11) . .
C12 C4 C5 118.9(12) . .
C3 C4 C5 122.8(11) . .
C6 C5 C4 120.8(11) . .
C6 C5 H5 119.6 . .
C4 C5 H5 119.6 . .
C5 C6 C7 120.7(12) . .
C5 C6 H6 119.7 . .
C7 C6 H6 119.7 . .
C6 C7 C11 120.5(12) . .
C6 C7 C8 123.5(11) . .
C11 C7 C8 116.0(10) . .
C9 C8 C7 120.2(11) . .
C9 C8 H8 119.9 . .
C7 C8 H8 119.9 . .
C8 C9 C10 118.9(12) . .
C8 C9 H9 120.6 . .
C10 C9 H9 120.6 . .
N2 C10 C9 122.7(10) . .
N2 C10 H10 118.7 . .
C9 C10 H10 118.7 . .
N2 C11 C7 122.2(9) . .
N2 C11 C12 118.6(7) . .
C7 C11 C12 119.1(8) . .
N1 C12 C4 123.1(10) . .
N1 C12 C11 116.9(7) . .
C4 C12 C11 119.9(9) . .
O1 C13 O2 127.7(5) . .
O1 C13 C14 118.0(4) . .
O2 C13 C14 114.1(4) . .
C16 C14 C15 119.7(4) 5_576 .
C16 C14 C13 116.9(4) 5_576 .
C15 C14 C13 122.9(4) . .
C14 C15 C16 118.3(4) . .
C14 C15 C17 123.3(4) . .
C16 C15 C17 118.3(5) . .
C14 C16 C15 121.9(5) 5_576 .
C14 C16 H16 119.0 5_576 .
C15 C16 H16 119.0 . .
C20 C17 C18 117.8(5) . .
C20 C17 C15 121.7(5) . .
C18 C17 C15 120.5(5) . .
C19 C18 C17 121.1(6) . .
C19 C18 H18 119.4 . .
C17 C18 H18 119.4 . .
C22 C19 C18 120.3(6) . .
C22 C19 H19 119.8 . .
C18 C19 H19 119.8 . .
C17 C20 C21 120.7(6) . .
C17 C20 H20 119.6 . .
C21 C20 H20 119.6 . .
C22 C21 C20 121.5(6) . .
C22 C21 H21 119.3 . .
C20 C21 H21 119.3 . .
C21 C22 C19 118.3(5) . .
C21 C22 C23 121.5(6) . .
C19 C22 C23 120.2(6) . .
O3 C23 O4 124.6(6) . .
O3 C23 C22 115.9(6) . .
O4 C23 C22 119.5(6) . .
C1 N1 C12 117.3(7) . .
C1 N1 Ni1 131.0(6) . .
C12 N1 Ni1 111.1(5) . .
C10 N2 C11 119.9(7) . .
C10 N2 Ni1 127.9(6) . .
C11 N2 Ni1 111.3(5) . .
C13 O1 Ni1 133.5(3) . .
C13 O2 Ni1 133.2(4) . 2_556
C23 O3 Ni1 129.5(4) . 3_455
Ni1 O5 Ni1 113.6(2) . 2_556
Ni1 O5 H5A 127.0 . .
Ni1 O5 H5B 114.3 . .
Ni1 O5 H5B 130.2 2_556 .
H5A O5 H5B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.004(4) 2_556
Ni1 O1 2.031(4) .
Ni1 O3 2.050(4) 3_545
Ni1 N2 2.054(6) .
Ni1 O5 2.088(3) .
Ni1 N1 2.115(5) .
C1 N1 1.311(12) .
C1 C2 1.423(14) .
C1 H1 0.9300 .
C2 C3 1.363(17) .
C2 H2 0.9300 .
C3 C4 1.405(17) .
C3 H3 0.9300 .
C4 C12 1.402(13) .
C4 C5 1.441(16) .
C5 C6 1.378(18) .
C5 H5 0.9300 .
C6 C7 1.400(16) .
C6 H6 0.9300 .
C7 C11 1.409(12) .
C7 C8 1.416(17) .
C8 C9 1.362(16) .
C8 H8 0.9300 .
C9 C10 1.417(13) .
C9 H9 0.9300 .
C10 N2 1.270(11) .
C10 H10 0.9300 .
C11 N2 1.370(10) .
C11 C12 1.444(13) .
C12 N1 1.348(10) .
C13 O1 1.247(6) .
C13 O2 1.250(6) .
C13 C14 1.512(6) .
C14 C16 1.393(7) 5_576
C14 C15 1.394(7) .
C15 C16 1.399(7) .
C15 C17 1.492(7) .
C16 C14 1.393(7) 5_576
C16 H16 0.9300 .
C17 C20 1.367(8) .
C17 C18 1.386(9) .
C18 C19 1.383(9) .
C18 H18 0.9300 .
C19 C22 1.381(9) .
C19 H19 0.9300 .
C20 C21 1.389(9) .
C20 H20 0.9300 .
C21 C22 1.357(10) .
C21 H21 0.9300 .
C22 C23 1.509(8) .
C23 O3 1.236(8) .
C23 O4 1.239(8) .
O2 Ni1 2.004(4) 2_556
O3 Ni1 2.050(4) 3_455
O5 Ni1 2.088(3) 2_556
O5 H5A 0.8501 .
O5 H5B 0.8499 .
