#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/88/4318868.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_4318868
loop_
_publ_author_name
'Rong Cao'
'Qian Shi'
'Daofeng Sun'
'Maochun Hong'
'Wenghua Bi'
'Yingjun Zhao'
_publ_section_title
;
 Syntheses and Characterizations of Copper(II) Polymeric Complexes
 Constructed from 1,2,4,5-Benzenetetracarboxylic Acid
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6161
_journal_page_last               6168
_journal_paper_doi               10.1021/ic0258577
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C5 H4 Cu1.5 O5'
_chemical_formula_weight         239.39
_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                98.85(3)
_cell_angle_beta                 92.06(3)
_cell_angle_gamma                94.27(3)
_cell_formula_units_Z            1
_cell_length_a                   5.0155(10)
_cell_length_b                   5.8109(12)
_cell_length_c                   9.6258(19)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      3.56
_cell_volume                     276.11(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.861
_diffrn_measured_fraction_theta_max 0.861
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0048
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1112
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    2.895
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             118
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.001(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1112
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          1.387
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0342P)²+0.4571P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                1110
_reflns_number_total             1112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0258577-2_s2_4.cif
_cod_data_source_block           '[Cu3(btec)(OH)2]n'
_cod_original_formula_sum        'C5 H4 Cu1.50 O5'
_cod_database_code               4318868
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 1.0000 0.5000 0.0000 0.00463(14) Uani 1 2 d S . .
Cu2 Cu 0.18782(5) 0.04247(4) 0.12446(3) 0.00523(14) Uani 1 1 d . . .
O1 O 0.2138(3) 0.9274(3) 0.30411(16) 0.0084(3) Uani 1 1 d . . .
O2 O 0.4154(3) 0.6763(3) 0.15360(16) 0.0078(3) Uani 1 1 d . . .
O3 O 0.9050(3) 0.4399(3) 0.19088(16) 0.0083(3) Uani 1 1 d . . .
O4 O 0.5492(3) 0.1897(3) 0.13737(16) 0.0073(3) Uani 1 1 d . . .
O5 O 0.8880(3) 0.8159(2) 0.04290(15) 0.0044(3) Uani 1 1 d D . .
C1 C 0.3450(4) 0.7475(4) 0.2758(2) 0.0061(4) Uani 1 1 d . . .
C2 C 0.6796(4) 0.3511(3) 0.2188(2) 0.0049(4) Uani 1 1 d . . .
C3 C 0.4234(4) 0.6200(4) 0.3918(2) 0.0062(4) Uani 1 1 d . . .
C4 C 0.5835(4) 0.4311(4) 0.3644(2) 0.0055(4) Uani 1 1 d . . .
C5 C 0.6602(4) 0.3133(4) 0.4722(2) 0.0072(4) Uani 1 1 d . . .
H5A H 0.7677 0.1895 0.4539 0.009 Uiso 1 1 calc R . .
H5 H 0.729(5) 0.790(7) 0.086(4) 0.028(9) Uiso 1 1 d 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'
Cu Cu 0.3201 1.2651 '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
O5 Cu1 O5 180.0 . 2_765 ?
O5 Cu1 O3 90.25(7) . . ?
O5 Cu1 O3 89.75(7) 2_765 . ?
O5 Cu1 O3 89.75(7) . 2_765 ?
O5 Cu1 O3 90.25(7) 2_765 2_765 ?
O3 Cu1 O3 180.00(9) . 2_765 ?
O4 Cu2 O1 95.57(7) . 1_545 ?
O4 Cu2 O5 89.54(7) . 2_665 ?
O1 Cu2 O5 170.60(6) 1_545 2_665 ?
O4 Cu2 O5 155.58(6) . 1_445 ?
O1 Cu2 O5 95.48(7) 1_545 1_445 ?
O5 Cu2 O5 82.83(7) 2_665 1_445 ?
O4 Cu2 Cu2 127.24(5) . 2 ?
O1 Cu2 Cu2 135.90(5) 1_545 2 ?
O5 Cu2 Cu2 41.69(5) 2_665 2 ?
O5 Cu2 Cu2 41.13(5) 1_445 2 ?
C1 O1 Cu2 103.17(14) . 1_565 ?
C2 O3 Cu1 123.97(14) . . ?
C2 O4 Cu2 135.89(14) . . ?
Cu1 O5 Cu2 113.54(7) . 2_665 ?
Cu1 O5 Cu2 111.85(7) . 1_665 ?
Cu2 O5 Cu2 97.17(7) 2_665 1_665 ?
Cu1 O5 H5 102(2) . . ?
Cu2 O5 H5 109(2) 2_665 . ?
Cu2 O5 H5 125(2) 1_665 . ?
O2 C1 O1 122.3(2) . . ?
O2 C1 C3 118.60(19) . . ?
O1 C1 C3 119.05(19) . . ?
O4 C2 O3 122.95(19) . . ?
O4 C2 C4 120.16(18) . . ?
O3 C2 C4 116.57(18) . . ?
C5 C3 C4 119.6(2) 2_666 . ?
C5 C3 C1 120.53(19) 2_666 . ?
C4 C3 C1 119.86(19) . . ?
C5 C4 C3 120.20(19) . . ?
C5 C4 C2 118.00(18) . . ?
C3 C4 C2 121.81(19) . . ?
C4 C5 C3 120.19(19) . 2_666 ?
C4 C5 H5A 119.9 . . ?
C3 C5 H5A 119.9 2_666 . ?
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
Cu1 O5 1.9474(15) . ?
Cu1 O5 1.9474(15) 2_765 ?
Cu1 O3 1.9901(16) . ?
Cu1 O3 1.9901(16) 2_765 ?
Cu2 O4 1.9373(16) . ?
Cu2 O1 1.9512(16) 1_545 ?
Cu2 O5 1.9566(16) 2_665 ?
Cu2 O5 1.9783(16) 1_445 ?
Cu2 Cu2 2.9510(11) 2 ?
O1 C1 1.276(3) . ?
O1 Cu2 1.9512(16) 1_565 ?
O2 C1 1.258(3) . ?
O3 C2 1.262(3) . ?
O4 C2 1.252(3) . ?
O5 Cu2 1.9566(16) 2_665 ?
O5 Cu2 1.9783(16) 1_665 ?
O5 H5 0.926(19) . ?
C1 C3 1.489(3) . ?
C2 C4 1.515(3) . ?
C3 C5 1.395(3) 2_666 ?
C3 C4 1.406(3) . ?
C4 C5 1.386(3) . ?
C5 C3 1.395(3) 2_666 ?
C5 H5A 0.9300 . ?
