#------------------------------------------------------------------------------
#$Date: 2019-07-03 13:24:39 +0300 (Wed, 03 Jul 2019) $
#$Revision: 216710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/51/76/1517655.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_1517655
loop_
_publ_author_name
'Mohammad Hedayetullah Mir'
'Jagadese J. Vittal'
_publ_section_title
;
 Muconate bridged coordination polymers of Cu(II): Effect of auxiliary
 ligand on their structural architectures
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              97
_journal_page_last               101
_journal_volume                  403
_journal_year                    2013
_chemical_formula_sum            'C16 H16 Cu N2 O6'
_chemical_formula_weight         395.85
_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
_cell_angle_alpha                116.2250(10)
_cell_angle_beta                 107.3190(10)
_cell_angle_gamma                92.4780(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7526(5)
_cell_length_b                   9.9887(6)
_cell_length_c                   11.2859(7)
_cell_measurement_reflns_used    3923
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.29
_cell_volume                     827.21(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4843
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.356
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2904
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0268
_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)+(0.0339P)²+0.4617P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                2729
_reflns_number_total             2904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-403-97-101-1.cif
_cod_data_source_block           compound-1
_cod_depositor_comments
;

2019-06-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C32 H32 Cu2 N4 O12'
_cod_original_formula_weight         791.70
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1517655
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
Cu1 Cu 0.58859(3) 0.40386(2) 0.20410(2) 0.02059(10) Uani 1 1 d .
N1 N 0.4369(2) 0.51483(19) 0.30093(18) 0.0239(4) Uani 1 1 d .
C1 C 0.4220(3) 0.6598(2) 0.3378(2) 0.0319(5) Uani 1 1 d .
H1 H 0.4866 0.7183 0.3172 0.038 Uiso 1 1 calc R
C2 C 0.3159(3) 0.7261(3) 0.4045(3) 0.0359(5) Uani 1 1 d .
H2A H 0.3097 0.8284 0.4305 0.043 Uiso 1 1 calc R
C3 C 0.2191(3) 0.6398(3) 0.4325(2) 0.0338(5) Uani 1 1 d .
H3 H 0.1459 0.6825 0.4782 0.041 Uiso 1 1 calc R
C4 C 0.2310(3) 0.4897(3) 0.3924(2) 0.0301(5) Uani 1 1 d .
H4 H 0.1643 0.4284 0.4089 0.036 Uiso 1 1 calc R
C5 C 0.3416(2) 0.4305(2) 0.3281(2) 0.0226(4) Uani 1 1 d .
N2 N 0.48901(19) 0.23966(18) 0.23268(17) 0.0219(3) Uani 1 1 d .
C6 C 0.3679(2) 0.2728(2) 0.2850(2) 0.0227(4) Uani 1 1 d .
C7 C 0.2756(3) 0.1660(2) 0.2963(2) 0.0290(5) Uani 1 1 d .
H7 H 0.1919 0.1913 0.3335 0.035 Uiso 1 1 calc R
C8 C 0.3089(3) 0.0211(3) 0.2517(2) 0.0332(5) Uani 1 1 d .
H8 H 0.2466 -0.0540 0.2568 0.040 Uiso 1 1 calc R
C9 C 0.4344(3) -0.0124(2) 0.1997(2) 0.0318(5) Uani 1 1 d .
H9A H 0.4599 -0.1098 0.1703 0.038 Uiso 1 1 calc R
C10 C 0.5216(3) 0.0997(2) 0.1918(2) 0.0268(4) Uani 1 1 d .
H10 H 0.6071 0.0771 0.1563 0.032 Uiso 1 1 calc R
C11 C 0.9624(2) 0.9255(2) 0.4835(2) 0.0252(4) Uani 1 1 d .
H11A H 0.9776 0.9022 0.5578 0.030 Uiso 1 1 calc R
C12 C 0.8725(2) 0.8187(2) 0.3531(2) 0.0270(4) Uani 1 1 d .
H12 H 0.8582 0.8393 0.2773 0.032 Uiso 1 1 calc R
C13 C 0.7946(2) 0.6680(2) 0.3253(2) 0.0236(4) Uani 1 1 d .
O1 O 0.67946(16) 0.58757(15) 0.20386(14) 0.0234(3) Uani 1 1 d .
O2 O 0.83591(19) 0.62589(17) 0.41534(15) 0.0326(3) Uani 1 1 d .
C14 C 0.9959(3) 0.4463(2) 0.0267(2) 0.0249(4) Uani 1 1 d .
H14 H 1.0923 0.4144 0.0580 0.030 Uiso 1 1 calc R
C15 C 0.8604(2) 0.3901(2) 0.0342(2) 0.0239(4) Uani 1 1 d .
H15 H 0.7622 0.4173 -0.0012 0.029 Uiso 1 1 calc R
C16 C 0.8570(2) 0.2859(2) 0.0960(2) 0.0217(4) Uani 1 1 d .
O3 O 0.74691(17) 0.28358(16) 0.14857(16) 0.0278(3) Uani 1 1 d .
O4 O 0.95905(18) 0.20327(16) 0.09421(17) 0.0307(3) Uani 1 1 d .
O5 O 0.3970(2) 0.30003(19) -0.01375(17) 0.0345(4) Uani 1 1 d D
H5A H 0.370(3) 0.330(3) -0.064(2) 0.033(7) Uiso 1 1 d D
H5B H 0.329(3) 0.238(3) -0.035(3) 0.037(8) Uiso 1 1 d D
O6 O 1.1310(2) 0.0795(2) -0.0873(2) 0.0371(4) Uani 1 1 d D
H6A H 1.087(4) 0.120(3) -0.039(3) 0.054(10) Uiso 1 1 d D
H6B H 1.123(3) 0.002(2) -0.095(3) 0.050(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'
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'
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_3
O3 Cu1 O1 97.73(6) .
O3 Cu1 N2 89.48(6) .
O1 Cu1 N2 170.69(6) .
O3 Cu1 N1 165.68(7) .
O1 Cu1 N1 91.47(6) .
N2 Cu1 N1 80.36(6) .
O3 Cu1 O5 95.96(7) .
O1 Cu1 O5 96.32(6) .
N2 Cu1 O5 88.73(6) .
N1 Cu1 O5 93.90(7) .
C1 N1 C5 118.43(18) .
C1 N1 Cu1 126.70(14) .
C5 N1 Cu1 114.87(13) .
N1 C1 C2 122.6(2) .
C3 C2 C1 118.9(2) .
C2 C3 C4 119.0(2) .
C5 C4 C3 119.4(2) .
N1 C5 C4 121.65(19) .
N1 C5 C6 114.50(17) .
C4 C5 C6 123.85(18) .
C10 N2 C6 118.88(17) .
C10 N2 Cu1 125.83(14) .
C6 N2 Cu1 114.93(13) .
N2 C6 C7 121.82(18) .
N2 C6 C5 114.93(17) .
C7 C6 C5 123.24(18) .
C8 C7 C6 118.76(19) .
C9 C8 C7 119.45(19) .
C10 C9 C8 118.7(2) .
N2 C10 C9 122.37(19) .
C12 C11 C11 123.4(3) 2_776
C11 C12 C13 121.16(19) .
O2 C13 O1 123.04(18) .
O2 C13 C12 120.94(18) .
O1 C13 C12 116.00(17) .
C13 O1 Cu1 106.63(12) .
C15 C14 C14 124.2(2) 2_765
C14 C15 C16 123.08(19) .
O4 C16 O3 121.75(18) .
O4 C16 C15 119.74(17) .
O3 C16 C15 118.51(17) .
C16 O3 Cu1 138.16(13) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O3 1.9371(14) .
Cu1 O1 1.9696(13) .
Cu1 N2 2.0162(16) .
Cu1 N1 2.0261(17) .
Cu1 O5 2.2525(16) .
N1 C1 1.342(3) .
N1 C5 1.349(3) .
C1 C2 1.377(3) .
C2 C3 1.377(3) .
C3 C4 1.380(3) .
C4 C5 1.379(3) .
C5 C6 1.480(3) .
N2 C10 1.338(3) .
N2 C6 1.347(3) .
C6 C7 1.384(3) .
C7 C8 1.383(3) .
C8 C9 1.380(3) .
C9 C10 1.379(3) .
C11 C12 1.332(3) .
C11 C11 1.437(4) 2_776
C12 C13 1.483(3) .
C13 O2 1.229(2) .
C13 O1 1.294(2) .
C14 C15 1.331(3) .
C14 C14 1.453(4) 2_765
C15 C16 1.490(3) .
C16 O4 1.241(2) .
C16 O3 1.277(2) .
