#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:47:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180518 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/87/7218785.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_7218785
loop_
_publ_author_name
'Qiao, Jin-Zhong'
'Zhan, Mao-Sheng'
'Hu, Tuo-Ping'
_publ_section_title
;
 Syntheses, crystal structures, photoluminescent/magnetic properties of
 four new coordination polymers based on
 2,3′,4,5′-biphenyltetracarboxylic acid
;
_journal_issue                   107
_journal_name_full               'RSC Adv.'
_journal_page_first              62285
_journal_paper_doi               10.1039/C4RA09505G
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C44 H48 Co3 N4 O30'
_chemical_formula_weight         1289.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.721(5)
_cell_angle_beta                 101.817(5)
_cell_angle_gamma                98.064(5)
_cell_formula_units_Z            1
_cell_length_a                   7.3730(4)
_cell_length_b                   13.0724(7)
_cell_length_c                   13.8570(8)
_cell_measurement_reflns_used    2680
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4650
_cell_measurement_theta_min      3.2280
_cell_volume                     1262.17(13)
_computing_cell_refinement       'SMART (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Apex II CCD diffractometer'
_diffrn_measurement_method       'ω 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  0.0359
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8246
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             661
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.772
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         4417
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0626
_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)+(0.0739P)²+5.2301P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                3331
_reflns_number_total             4417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra09505g2.cif
_cod_data_source_block           htp-21
_cod_original_cell_volume        1262.16(12)
_cod_database_code               7218785
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Co1 Co 1.0000 0.5000 0.5000 0.0180(3) Uani 1 2 d S . .
Co2 Co 0.28302(13) 0.17519(6) 0.66141(6) 0.0357(3) Uani 1 1 d . . .
O1 O 0.3306(6) 0.3375(3) 0.6939(3) 0.0259(9) Uani 1 1 d . . .
O12W O 0.8147(6) 0.3653(3) 0.4035(3) 0.0273(9) Uani 1 1 d D . .
O3 O 0.5694(5) 0.6867(3) 0.6000(3) 0.0284(9) Uani 1 1 d . . .
O8 O 0.9303(6) 1.1684(3) 1.1068(3) 0.0311(10) Uani 1 1 d D . .
O4 O 0.8284(6) 0.7613(3) 0.7192(3) 0.0330(10) Uani 1 1 d . . .
O2 O 0.3142(7) 0.3485(3) 0.8549(3) 0.0430(12) Uani 1 1 d . . .
O7 O 0.9264(6) 1.0207(3) 1.1647(3) 0.0373(11) Uani 1 1 d . . .
N2 N 1.0853(6) 0.5508(3) 0.2128(3) 0.0228(10) Uani 1 1 d . . .
O5 O 0.3497(6) 1.0189(3) 0.6819(3) 0.0361(10) Uani 1 1 d . . .
O13W O 0.7879(6) 0.5904(3) 0.4771(3) 0.0325(10) Uani 1 1 d D . .
O14W O -0.0810(7) 0.1672(3) 0.3797(3) 0.0404(11) Uani 1 1 d D . .
O6 O 0.5248(6) 1.1664(3) 0.7751(3) 0.0417(11) Uani 1 1 d . . .
N1 N 1.0816(6) 0.5402(3) 0.3696(3) 0.0239(10) Uani 1 1 d . . .
C1 C 0.5768(7) 0.6623(4) 0.7663(4) 0.0167(10) Uani 1 1 d . . .
O9W O 0.1061(8) 0.1642(4) 0.7679(4) 0.0461(12) Uani 1 1 d D . .
O10W O 0.4161(8) 0.1663(4) 0.5349(4) 0.0599(15) Uani 1 1 d . . .
H10A H 0.4146 0.2239 0.5098 0.090 Uiso 1 1 d R . .
H10B H 0.3573 0.1113 0.4850 0.090 Uiso 1 1 d R . .
C14 C 0.6659(8) 0.7083(4) 0.6902(4) 0.0226(12) Uani 1 1 d . . .
C6 C 0.5605(7) 0.7243(4) 0.8570(4) 0.0200(11) Uani 1 1 d . . .
C16 C 0.8785(8) 1.0660(4) 1.0979(4) 0.0230(12) Uani 1 1 d . . .
C2 C 0.5128(8) 0.5539(4) 0.7436(4) 0.0210(11) Uani 1 1 d . . .
H2 H 0.533(8) 0.518(4) 0.686(5) 0.025 Uiso 1 1 d . . .
C9 C 0.7552(8) 1.0099(4) 0.9961(4) 0.0219(11) Uani 1 1 d . . .
C8 C 0.7156(8) 0.8997(4) 0.9737(4) 0.0206(11) Uani 1 1 d . . .
H8A H 0.759(8) 0.870(5) 1.015(5) 0.025 Uiso 1 1 d . . .
C19 C 1.0217(8) 0.4919(4) 0.2744(4) 0.0210(11) Uani 1 1 d . . .
H19 H 0.943(9) 0.439(5) 0.252(4) 0.025 Uiso 1 1 d . . .
C21 C 1.0433(8) 0.5236(4) 0.1040(4) 0.0220(11) Uani 1 1 d . . .
C7 C 0.6072(7) 0.8436(4) 0.8799(4) 0.0201(11) Uani 1 1 d . . .
C13 C 0.3569(8) 0.3886(4) 0.7851(4) 0.0263(13) Uani 1 1 d . . .
C5 C 0.4886(8) 0.6747(4) 0.9246(4) 0.0231(12) Uani 1 1 d . . .
H5 H 0.4805 0.7151 0.9858 0.028 Uiso 1 1 calc R . .
C3 C 0.4365(8) 0.5043(4) 0.8100(4) 0.0219(12) Uani 1 1 d . . .
C22 C 1.0173(8) 0.4209(4) 0.0529(4) 0.0275(13) Uani 1 1 d . . .
H22 H 1.0303 0.3677 0.0886 0.033 Uiso 1 1 calc R . .
C11 C 0.5706(7) 1.0090(4) 0.8322(4) 0.0220(11) Uani 1 1 d . . .
C4 C 0.4286(8) 0.5661(4) 0.9027(4) 0.0246(12) Uani 1 1 d . . .
H4 H 0.379(8) 0.537(4) 0.950(5) 0.029 Uiso 1 1 d . . .
C18 C 1.1925(9) 0.6430(5) 0.2742(4) 0.0311(14) Uani 1 1 d . . .
H18 H 1.250(9) 0.691(5) 0.249(5) 0.037 Uiso 1 1 d . . .
C10 C 0.6842(8) 1.0649(4) 0.9248(4) 0.0223(12) Uani 1 1 d . . .
H10 H 0.703(8) 1.134(5) 0.941(4) 0.027 Uiso 1 1 d . . .
C15 C 0.4778(8) 1.0688(4) 0.7586(4) 0.0285(13) Uani 1 1 d . . .
C12 C 0.5341(8) 0.8988(4) 0.8096(4) 0.0226(12) Uani 1 1 d . . .
H12 H 0.4599 0.8619 0.7468 0.027 Uiso 1 1 calc R . .
C20 C 1.0284(9) 0.6048(4) 0.0519(4) 0.0305(13) Uani 1 1 d . . .
H20 H 1.050(9) 0.679(5) 0.085(5) 0.037 Uiso 1 1 d . . .
C17 C 1.1882(9) 0.6357(5) 0.3691(4) 0.0326(14) Uani 1 1 d . . .
H17 H 1.2487 0.6878 0.4266 0.039 Uiso 1 1 calc R . .
H14A H -0.161(8) 0.112(4) 0.354(5) 0.07(3) Uiso 1 1 d D . .
H14B H 0.000(9) 0.188(6) 0.350(5) 0.07(3) Uiso 1 1 d D . .
O11W O 0.0413(8) 0.1285(5) 0.5578(4) 0.083(2) Uani 1 1 d D . .
H11A H -0.0509 0.0920 0.5712 0.100 Uiso 1 1 d RD . .
H11B H 0.0501 0.1399 0.5018 0.100 Uiso 1 1 d RD . .
H13A H 0.732(7) 0.611(4) 0.520(3) 0.019(15) Uiso 1 1 d D . .
H12A H 0.842(8) 0.305(3) 0.399(5) 0.04(2) Uiso 1 1 d D . .
H13B H 0.767(9) 0.604(5) 0.420(2) 0.04(2) Uiso 1 1 d D . .
H12B H 0.706(5) 0.376(5) 0.402(7) 0.07(3) Uiso 1 1 d D . .
H8 H 1.007(7) 1.190(5) 1.160(3) 0.036(19) Uiso 1 1 d D . .
H9WA H 0.025(7) 0.163(5) 0.800(4) 0.026(18) Uiso 1 1 d D . .
H9WB H 0.171(14) 0.219(5) 0.803(7) 0.12(5) Uiso 1 1 d D . .
O15W O -0.278(2) 0.0564(17) 0.5933(17) 0.112(6) Uani 0.61(4) 1 d PU A 2
O16W O -0.234(3) -0.002(3) 0.6288(18) 0.082(10) Uani 0.39(4) 1 d PU A 1
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'
Co Co 0.3494 0.9721 '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'
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
O13W Co1 O13W 180.0(2) 2_766 .
O13W Co1 O12W 89.90(17) 2_766 .
O13W Co1 O12W 90.10(17) . .
O13W Co1 O12W 90.10(17) 2_766 2_766
O13W Co1 O12W 89.90(17) . 2_766
O12W Co1 O12W 180.00(16) . 2_766
O13W Co1 N1 92.01(17) 2_766 .
O13W Co1 N1 87.99(17) . .
O12W Co1 N1 88.54(16) . .
O12W Co1 N1 91.46(16) 2_766 .
O13W Co1 N1 87.99(17) 2_766 2_766
O13W Co1 N1 92.01(17) . 2_766
O12W Co1 N1 91.46(16) . 2_766
O12W Co1 N1 88.54(16) 2_766 2_766
N1 Co1 N1 180.000(1) . 2_766
O11W Co2 O1 106.0(2) . .
O11W Co2 O6 159.3(2) . 1_545
O1 Co2 O6 94.19(15) . 1_545
O11W Co2 O10W 85.9(2) . .
O1 Co2 O10W 93.12(17) . .
O6 Co2 O10W 97.8(2) 1_545 .
O11W Co2 O9W 84.2(2) . .
O1 Co2 O9W 93.33(17) . .
O6 Co2 O9W 90.2(2) 1_545 .
O10W Co2 O9W 169.4(2) . .
O11W Co2 O5 100.1(2) . 1_545
O1 Co2 O5 153.86(16) . 1_545
O6 Co2 O5 59.66(15) 1_545 1_545
O10W Co2 O5 90.35(18) . 1_545
O9W Co2 O5 87.57(18) . 1_545
O11W Co2 C15 129.7(2) . 1_545
O1 Co2 C15 123.64(17) . 1_545
O6 Co2 C15 29.64(16) 1_545 1_545
O10W Co2 C15 98.0(2) . 1_545
O9W Co2 C15 85.5(2) . 1_545
O5 Co2 C15 30.34(16) 1_545 1_545
C13 O1 Co2 119.8(3) . .
C19 N2 C18 106.6(4) . .
C19 N2 C21 126.9(4) . .
C18 N2 C21 126.5(4) . .
C15 O5 Co2 87.3(3) . 1_565
C15 O6 Co2 91.0(4) . 1_565
C19 N1 C17 104.8(4) . .
C19 N1 Co1 129.6(4) . .
C17 N1 Co1 124.8(4) . .
C2 C1 C6 119.8(5) . .
C2 C1 C14 117.2(5) . .
C6 C1 C14 122.9(4) . .
O4 C14 O3 124.4(5) . .
O4 C14 C1 118.8(4) . .
O3 C14 C1 116.8(5) . .
C5 C6 C1 118.8(4) . .
C5 C6 C7 119.1(5) . .
C1 C6 C7 121.9(5) . .
O7 C16 O8 123.5(5) . .
O7 C16 C9 122.9(5) . .
O8 C16 C9 113.7(5) . .
C1 C2 C3 121.4(5) . .
C10 C9 C8 120.1(5) . .
C10 C9 C16 121.8(5) . .
C8 C9 C16 118.1(5) . .
C7 C8 C9 120.6(5) . .
N1 C19 N2 111.8(5) . .
C22 C21 C20 120.6(5) . .
C22 C21 N2 120.9(5) . .
C20 C21 N2 118.5(5) . .
C12 C7 C8 119.0(5) . .
C12 C7 C6 120.5(4) . .
C8 C7 C6 120.4(5) . .
O2 C13 O1 124.2(5) . .
O2 C13 C3 117.5(5) . .
O1 C13 C3 118.2(5) . .
C6 C5 C4 121.1(5) . .
C2 C3 C4 118.5(5) . .
C2 C3 C13 122.5(5) . .
C4 C3 C13 119.0(5) . .
C21 C22 C20 120.5(5) . 2_765
C10 C11 C12 120.2(5) . .
C10 C11 C15 119.4(5) . .
C12 C11 C15 120.3(5) . .
C5 C4 C3 120.2(5) . .
C17 C18 N2 106.1(5) . .
C11 C10 C9 119.3(5) . .
O6 C15 O5 120.8(5) . .
O6 C15 C11 119.6(5) . .
O5 C15 C11 119.6(5) . .
O6 C15 Co2 59.4(3) . 1_565
O5 C15 Co2 62.4(3) . 1_565
C11 C15 Co2 168.3(4) . 1_565
C7 C12 C11 120.5(5) . .
C22 C20 C21 118.9(5) 2_765 .
C18 C17 N1 110.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O13W 2.097(4) 2_766
Co1 O13W 2.097(4) .
Co1 O12W 2.111(4) .
Co1 O12W 2.111(4) 2_766
Co1 N1 2.147(4) .
Co1 N1 2.147(4) 2_766
Co2 O11W 1.983(6) .
Co2 O1 2.049(3) .
Co2 O6 2.155(4) 1_545
Co2 O10W 2.170(5) .
Co2 O9W 2.172(6) .
Co2 O5 2.222(4) 1_545
Co2 C15 2.505(6) 1_545
O1 C13 1.277(6) .
O3 C14 1.263(6) .
O8 C16 1.315(6) .
O4 C14 1.242(6) .
O2 C13 1.256(7) .
O7 C16 1.210(6) .
N2 C19 1.359(7) .
N2 C18 1.370(7) .
N2 C21 1.440(7) .
O5 C15 1.267(7) .
O5 Co2 2.222(4) 1_565
O6 C15 1.239(6) .
O6 Co2 2.155(4) 1_565
N1 C19 1.308(7) .
N1 C17 1.381(7) .
C1 C2 1.383(7) .
C1 C6 1.401(7) .
C1 C14 1.521(7) .
C6 C5 1.382(7) .
C6 C7 1.507(7) .
C16 C9 1.502(7) .
C2 C3 1.384(7) .
C9 C10 1.387(7) .
C9 C8 1.391(7) .
C8 C7 1.386(7) .
C21 C22 1.364(8) .
C21 C20 1.394(7) .
C7 C12 1.384(7) .
C13 C3 1.492(7) .
C5 C4 1.383(7) .
C3 C4 1.400(8) .
C22 C20 1.385(8) 2_765
C11 C10 1.386(8) .
C11 C12 1.391(7) .
C11 C15 1.510(7) .
C18 C17 1.342(8) .
C15 Co2 2.505(6) 1_565
C20 C22 1.385(8) 2_765
