#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:47:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180518 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/87/7218783.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_7218783
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            'C52 H40 Cu5 N4 O23'
_chemical_formula_weight         1406.62
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                107.269(5)
_cell_angle_beta                 95.042(4)
_cell_angle_gamma                115.812(5)
_cell_formula_units_Z            1
_cell_length_a                   10.8509(5)
_cell_length_b                   11.1660(7)
_cell_length_c                   12.6776(7)
_cell_measurement_reflns_used    3447
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.3680
_cell_measurement_theta_min      4.6780
_cell_volume                     1277.63(15)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8868
_diffrn_reflns_theta_full        70.42
_diffrn_reflns_theta_max         70.42
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_T_max  0.529
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             703
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         4775
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0416
_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)+(0.0669P)²+1.0703P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                3956
_reflns_number_total             4775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra09505g2.cif
_cod_data_source_block           htp-20
_cod_original_cell_volume        1277.63(12)
_cod_database_code               7218783
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
Cu1 Cu 0.0000 0.0000 0.5000 0.02673(18) Uani 1 2 d SU . .
Cu2 Cu 0.84834(5) 0.04975(5) 0.25472(4) 0.02437(15) Uani 1 1 d U . .
Cu3 Cu 0.90981(5) 0.70420(5) 0.53163(4) 0.03046(16) Uani 1 1 d U . .
O1 O 0.2033(2) 0.0845(3) 0.5256(2) 0.0360(6) Uani 1 1 d U A .
O2A O 0.2387(11) 0.035(3) 0.3489(6) 0.046(5) Uani 0.52(5) 1 d PU A 2
O2B O 0.2313(9) -0.033(3) 0.371(2) 0.062(8) Uani 0.48(5) 1 d PU A 1
O3 O 0.7399(2) 0.1095(2) 0.35186(19) 0.0268(5) Uani 1 1 d U . .
O4 O 0.9126(2) 0.2998(3) 0.4962(2) 0.0312(6) Uani 1 1 d U . .
O5 O 0.7934(2) 0.6565(3) 0.6384(2) 0.0301(5) Uani 1 1 d U . .
O6 O 1.0003(2) 0.7367(3) 0.7585(2) 0.0354(6) Uani 1 1 d U . .
O7 O 0.9040(3) 0.9236(3) 1.1458(2) 0.0340(6) Uani 1 1 d U . .
O8 O 0.7491(3) 0.7573(3) 1.1983(2) 0.0528(8) Uani 1 1 d U . .
O9W O 1.0012(2) 0.9084(2) 0.6205(2) 0.0251(5) Uani 1 1 d DU . .
O10W O -0.0578(4) -0.2128(4) 0.3717(3) 0.0557(8) Uani 1 1 d U . .
H10A H 0.0139 -0.2135 0.3376 0.084 Uiso 1 1 d R . .
H10B H -0.1344 -0.2458 0.3126 0.084 Uiso 1 1 d R . .
N1 N 0.7004(3) -0.0054(3) 0.1140(2) 0.0289(6) Uani 1 1 d U . .
N2 N 0.2208(3) -0.5184(3) -0.4088(2) 0.0264(6) Uani 1 1 d U . .
C1 C 0.4853(3) 0.2771(4) 0.6194(3) 0.0258(7) Uani 1 1 d U . .
H1 H 0.4204 0.2891 0.6586 0.031 Uiso 1 1 calc R . .
C2 C 0.4373(3) 0.1691(4) 0.5122(3) 0.0255(7) Uani 1 1 d U A .
C3 C 0.5334(3) 0.1475(4) 0.4543(3) 0.0255(7) Uani 1 1 d U . .
H3 H 0.5012 0.0752 0.3825 0.031 Uiso 1 1 calc R . .
C4 C 0.6774(3) 0.2340(3) 0.5041(3) 0.0215(6) Uani 1 1 d U . .
C5 C 0.7244(3) 0.3442(3) 0.6100(3) 0.0242(7) Uani 1 1 d U . .
H5 H 0.8211 0.4033 0.6421 0.029 Uiso 1 1 calc R . .
C6 C 0.6299(3) 0.3680(3) 0.6691(3) 0.0228(7) Uani 1 1 d U . .
C7 C 0.6805(3) 0.4825(3) 0.7848(3) 0.0231(7) Uani 1 1 d U . .
C8 C 0.7922(3) 0.6223(3) 0.8142(3) 0.0236(7) Uani 1 1 d U . .
C9 C 0.8358(3) 0.7212(4) 0.9255(3) 0.0257(7) Uani 1 1 d U . .
H9 H 0.9089 0.8138 0.9436 0.031 Uiso 1 1 calc R . .
C10 C 0.7731(3) 0.6853(4) 1.0102(3) 0.0264(7) Uani 1 1 d U . .
C11 C 0.6647(4) 0.5460(4) 0.9818(3) 0.0326(8) Uani 1 1 d U . .
H11 H 0.6229 0.5190 1.0378 0.039 Uiso 1 1 calc R . .
C12 C 0.6183(4) 0.4475(4) 0.8713(3) 0.0289(7) Uani 1 1 d U . .
H12 H 0.5440 0.3557 0.8538 0.035 Uiso 1 1 calc R . .
C13 C 0.2796(4) 0.0764(4) 0.4593(3) 0.0355(9) Uani 1 1 d U . .
C14 C 0.7859(3) 0.2123(3) 0.4456(3) 0.0217(6) Uani 1 1 d U . .
C15 C 0.8682(3) 0.6748(3) 0.7308(3) 0.0250(7) Uani 1 1 d U . .
C16 C 0.8127(4) 0.7948(4) 1.1269(3) 0.0315(8) Uani 1 1 d U . .
C17 C 0.6476(4) -0.0873(4) -0.0903(3) 0.0337(8) Uani 1 1 d U . .
H17 H 0.6780 -0.0810 -0.1557 0.040 Uiso 1 1 calc R . .
C18 C 0.7399(4) -0.0006(4) 0.0174(3) 0.0342(8) Uani 1 1 d U . .
H18 H 0.8328 0.0634 0.0226 0.041 Uiso 1 1 calc R . .
C19 C 0.5644(4) -0.0896(4) 0.1064(3) 0.0316(8) Uani 1 1 d U . .
H19 H 0.5347 -0.0873 0.1732 0.038 Uiso 1 1 calc R . .
C20 C 0.4664(4) -0.1797(4) 0.0030(3) 0.0325(8) Uani 1 1 d U . .
H20 H 0.3726 -0.2372 0.0007 0.039 Uiso 1 1 calc R . .
C21 C 0.5085(4) -0.1840(4) -0.0979(3) 0.0293(7) Uani 1 1 d U . .
C22 C 0.4091(4) -0.2940(4) -0.2090(3) 0.0278(7) Uani 1 1 d U . .
C23 C 0.2657(4) -0.3402(4) -0.2293(3) 0.0342(8) Uani 1 1 d U . .
H23 H 0.2303 -0.2961 -0.1756 0.041 Uiso 1 1 calc R . .
C24 C 0.1753(4) -0.4516(4) -0.3289(3) 0.0319(8) Uani 1 1 d U . .
H24 H 0.0789 -0.4814 -0.3411 0.038 Uiso 1 1 calc R . .
C25 C 0.3607(4) -0.4692(4) -0.3916(3) 0.0328(8) Uani 1 1 d U . .
H25 H 0.3939 -0.5121 -0.4481 0.039 Uiso 1 1 calc R . .
C26 C 0.4571(4) -0.3584(4) -0.2944(3) 0.0328(8) Uani 1 1 d U . .
H26 H 0.5534 -0.3269 -0.2860 0.039 Uiso 1 1 calc R . .
H9W H 0.947(4) 0.928(4) 0.657(3) 0.036(11) Uiso 1 1 d D . .
O12W O 0.2499(14) -0.2020(11) 0.1706(9) 0.131(5) Uani 0.618(10) 1 d P B 3
O11W O 0.0903(14) -0.2484(13) 0.2188(12) 0.097(5) Uani 0.382(10) 1 d P B 4
O13W O 0.102(2) -0.308(3) 0.1241(12) 0.132(10) Uani 0.28 1 d P C 5
O14W O 0.028(3) -0.447(3) 0.048(3) 0.154(14) Uani 0.22 1 d P . 6
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O1 Cu1 O1 180.000(1) 2_556 .
O1 Cu1 O9W 91.25(10) 2_556 2_666
O1 Cu1 O9W 88.75(10) . 2_666
O1 Cu1 O9W 88.75(10) 2_556 1_445
O1 Cu1 O9W 91.25(10) . 1_445
O9W Cu1 O9W 180.000(1) 2_666 1_445
O1 Cu1 O10W 82.01(12) 2_556 .
O1 Cu1 O10W 97.99(12) . .
O9W Cu1 O10W 94.26(11) 2_666 .
O9W Cu1 O10W 85.74(11) 1_445 .
O1 Cu1 O10W 97.99(12) 2_556 2_556
O1 Cu1 O10W 82.01(12) . 2_556
O9W Cu1 O10W 85.74(11) 2_666 2_556
O9W Cu1 O10W 94.26(11) 1_445 2_556
O10W Cu1 O10W 180.000(1) . 2_556
O3 Cu2 O9W 95.93(10) . 2_766
O3 Cu2 O7 160.48(11) . 1_544
O9W Cu2 O7 90.15(10) 2_766 1_544
O3 Cu2 N1 90.00(11) . .
O9W Cu2 N1 173.90(10) 2_766 .
O7 Cu2 N1 83.77(11) 1_544 .
O3 Cu2 O6 100.77(10) . 2_766
O9W Cu2 O6 87.46(10) 2_766 2_766
O7 Cu2 O6 98.01(10) 1_544 2_766
N1 Cu2 O6 92.86(11) . 2_766
O9W Cu3 O5 92.86(10) . .
O9W Cu3 N2 159.06(12) . 2_655
O5 Cu3 N2 91.46(11) . 2_655
O9W Cu3 O4 95.73(10) . 2_766
O5 Cu3 O4 134.73(12) . 2_766
N2 Cu3 O4 95.72(11) 2_655 2_766
C13 O1 Cu1 131.7(2) . .
C14 O3 Cu2 127.9(2) . .
C14 O4 Cu3 130.6(2) . 2_766
C15 O5 Cu3 110.9(2) . .
C15 O6 Cu2 126.7(2) . 2_766
C16 O7 Cu2 106.7(2) . 1_566
Cu3 O9W Cu2 107.11(12) . 2_766
Cu3 O9W Cu1 104.31(10) . 1_665
Cu2 O9W Cu1 132.24(12) 2_766 1_665
C19 N1 C18 118.3(3) . .
C19 N1 Cu2 118.8(3) . .
C18 N1 Cu2 118.9(2) . .
C24 N2 C25 117.7(3) . .
C24 N2 Cu3 121.8(2) . 2_655
C25 N2 Cu3 119.4(2) . 2_655
C2 C1 C6 120.7(3) . .
C1 C2 C3 120.1(3) . .
C1 C2 C13 119.2(3) . .
C3 C2 C13 120.7(3) . .
C4 C3 C2 119.7(3) . .
C3 C4 C5 119.7(3) . .
C3 C4 C14 121.6(3) . .
C5 C4 C14 118.6(3) . .
C4 C5 C6 121.4(3) . .
C5 C6 C1 118.2(3) . .
C5 C6 C7 121.3(3) . .
C1 C6 C7 120.3(3) . .
C12 C7 C8 117.6(3) . .
C12 C7 C6 118.5(3) . .
C8 C7 C6 123.8(3) . .
C9 C8 C7 120.0(3) . .
C9 C8 C15 116.5(3) . .
C7 C8 C15 123.5(3) . .
C10 C9 C8 121.8(3) . .
C9 C10 C11 118.2(3) . .
C9 C10 C16 121.4(3) . .
C11 C10 C16 120.2(3) . .
C12 C11 C10 120.7(3) . .
C11 C12 C7 121.6(3) . .
O2B C13 O1 118.7(8) . .
O2B C13 O2A 39.5(9) . .
O1 C13 O2A 124.5(4) . .
O2B C13 C2 121.4(6) . .
O1 C13 C2 115.4(3) . .
O2A C13 C2 116.3(7) . .
O4 C14 O3 126.8(3) . .
O4 C14 C4 116.2(3) . .
O3 C14 C4 117.0(3) . .
O6 C15 O5 124.9(3) . .
O6 C15 C8 117.6(3) . .
O5 C15 C8 117.5(3) . .
O8 C16 O7 123.6(3) . .
O8 C16 C10 118.5(3) . .
O7 C16 C10 117.8(3) . .
C18 C17 C21 118.5(4) . .
N1 C18 C17 122.8(3) . .
N1 C19 C20 122.4(3) . .
C19 C20 C21 119.7(3) . .
C20 C21 C17 117.9(3) . .
C20 C21 C22 120.2(3) . .
C17 C21 C22 121.8(3) . .
C23 C22 C26 117.7(3) . .
C23 C22 C21 121.5(3) . .
C26 C22 C21 120.7(3) . .
C24 C23 C22 119.9(3) . .
N2 C24 C23 122.4(3) . .
N2 C25 C26 123.0(3) . .
C25 C26 C22 119.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.934(2) 2_556
Cu1 O1 1.934(2) .
Cu1 O9W 2.077(2) 2_666
Cu1 O9W 2.077(2) 1_445
Cu1 O10W 2.217(3) .
Cu1 O10W 2.217(3) 2_556
Cu2 O3 1.949(2) .
Cu2 O9W 1.957(2) 2_766
Cu2 O7 1.998(2) 1_544
Cu2 N1 2.030(3) .
Cu2 O6 2.300(3) 2_766
Cu3 O9W 1.940(2) .
Cu3 O5 1.963(2) .
Cu3 N2 1.967(3) 2_655
Cu3 O4 2.006(2) 2_766
O1 C13 1.242(4) .
O2A C13 1.303(9) .
O2B C13 1.241(10) .
O3 C14 1.252(4) .
O4 C14 1.249(4) .
O4 Cu3 2.006(2) 2_766
O5 C15 1.273(4) .
O6 C15 1.249(4) .
O6 Cu2 2.300(3) 2_766
O7 C16 1.273(5) .
O7 Cu2 1.998(2) 1_566
O8 C16 1.246(5) .
O9W Cu2 1.957(2) 2_766
O9W Cu1 2.077(2) 1_665
N1 C19 1.336(5) .
N1 C18 1.341(5) .
N2 C24 1.337(4) .
N2 C25 1.342(4) .
N2 Cu3 1.967(3) 2_655
C1 C2 1.388(5) .
C1 C6 1.396(4) .
C2 C3 1.390(4) .
C2 C13 1.514(4) .
C3 C4 1.387(4) .
C4 C5 1.389(4) .
C4 C14 1.514(4) .
C5 C6 1.391(4) .
C6 C7 1.491(4) .
C7 C12 1.401(5) .
C7 C8 1.405(5) .
C8 C9 1.391(5) .
C8 C15 1.497(5) .
C9 C10 1.386(5) .
C10 C11 1.390(5) .
C10 C16 1.492(5) .
C11 C12 1.380(5) .
C17 C18 1.390(5) .
C17 C21 1.396(5) .
C19 C20 1.379(5) .
C20 C21 1.390(5) .
C21 C22 1.486(5) .
C22 C23 1.380(5) .
C22 C26 1.387(5) .
C23 C24 1.375(5) .
C25 C26 1.373(5) .
O14W O14W 1.29(5) 2_545
