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#$Date: 2016-03-26 15:54:31 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180362 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/31/7203108.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_7203108
loop_
_publ_author_name
'Zvicka Deutsch'
'Janice M. Rubin-Preminger'
'Joel Bernstein'
'James Y. Becker'
_publ_section_title
;
 Three crystal forms of
 tetrakis(μ<small>₂</small>-2-nitrobenzoato-O,O′)-diaqua-di-copper(<small>II</small>)
;
_journal_name_full               CrystEngComm
_journal_page_first              41
_journal_page_last               50
_journal_paper_doi               10.1039/b511326a
_journal_year                    2006
_chemical_formula_moiety         Cu2(2-NO2C6H4COO)4(H2O)2
_chemical_formula_sum            'C28 H20 Cu2 N4 O18'
_chemical_formula_weight         827.56
_chemical_melting_point          'dehydration at 423K'
_chemical_name_common
Tetrakis(?2-2-nitrobenzoato-O,O?)-diaqua-di-copper(ii)
_chemical_name_systematic
Tetrakis(?2-2-nitrobenzoato-O,O?)-diaqua-di-copper(ii)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.101(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.534(2)
_cell_length_b                   13.411(4)
_cell_length_c                   15.404(4)
_cell_measurement_reflns_used    3725
_cell_measurement_temperature    295(2)
_cell_volume                     1544.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART 1000K CCD detector'
_diffrn_measurement_method
'Mo K? radiation with a graphite monochromator at 15 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9511
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         5.77
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.471
_exptl_crystal_colour            'emerald green'
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_recrystallization_method 'from water at ambient conditions'
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.47
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0316
_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/[\\s²(Fo²)+(0.0540P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                3043
_reflns_number_total             3725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b511326a.txt
_cod_data_source_block           form1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7203108
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.23331(17) 0.58617(10) 0.55684(10) 0.0314(3) Uani 1 1 d . . .
C1 C -0.1179(2) 0.65446(14) 0.56870(12) 0.0251(4) Uani 1 1 d . . .
C2 C -0.1772(2) 0.75299(14) 0.60134(14) 0.0283(4) Uani 1 1 d . . .
C3 C -0.2616(3) 0.81766(17) 0.53886(16) 0.0387(5) Uani 1 1 d . . .
C4 C -0.3122(3) 0.91194(19) 0.5636(2) 0.0506(7) Uani 1 1 d . . .
C5 C -0.2803(4) 0.94313(19) 0.6486(2) 0.0538(8) Uani 1 1 d . . .
C6 C -0.1995(3) 0.88040(19) 0.7115(2) 0.0471(6) Uani 1 1 d . . .
C7 C -0.1483(3) 0.78646(15) 0.68758(14) 0.0326(4) Uani 1 1 d . . .
N1 N -0.0662(3) 0.71975(17) 0.75587(13) 0.0415(4) Uani 1 1 d . . .
O2 O -0.0238(3) 0.63712(14) 0.73533(12) 0.0535(5) Uani 1 1 d . . .
O3 O -0.0447(3) 0.7496(2) 0.83098(14) 0.0794(7) Uani 1 1 d . . .
O4 O 0.03828(17) 0.65008(10) 0.54902(10) 0.0310(3) Uani 1 1 d . . .
O11 O 0.22574(19) 0.48121(12) 0.60946(9) 0.0343(3) Uani 1 1 d . . .
C11 C 0.1131(3) 0.43494(14) 0.64853(13) 0.0275(4) Uani 1 1 d . . .
C12 C 0.1761(3) 0.40109(15) 0.73966(13) 0.0301(4) Uani 1 1 d . . .
C13 C 0.2674(3) 0.4681(2) 0.79680(16) 0.0387(5) Uani 1 1 d . . .
C14 C 0.3108(3) 0.4439(2) 0.88425(16) 0.0490(6) Uani 1 1 d . . .
C15 C 0.2633(4) 0.3537(3) 0.91539(17) 0.0545(8) Uani 1 1 d . . .
C16 C 0.1742(3) 0.2849(2) 0.85983(17) 0.0477(6) Uani 1 1 d . . .
C17 C 0.1339(3) 0.30899(16) 0.77300(14) 0.0347(5) Uani 1 1 d . . .
N11 N 0.0544(3) 0.23028(14) 0.71406(15) 0.0441(5) Uani 1 1 d . . .
O12 O 0.1002(3) 0.22494(15) 0.64150(13) 0.0606(5) Uani 1 1 d . . .
O13 O -0.0480(3) 0.17156(15) 0.74247(17) 0.0716(6) Uani 1 1 d . . .
O14 O -0.04672(18) 0.41871(11) 0.62036(9) 0.0318(3) Uani 1 1 d . . .
Cu1 Cu 0.15744(3) 0.539782(16) 0.494929(14) 0.02180(9) Uani 1 1 d . . .
O6 O 0.4050(2) 0.61720(13) 0.48337(12) 0.0367(3) Uani 1 1 d . . .
H15 H -0.285(4) 0.795(2) 0.4776(19) 0.046(7) Uiso 1 1 d . . .
H10 H 0.291(4) 0.526(2) 0.7784(19) 0.046(8) Uiso 1 1 d . . .
H23 H 0.291(4) 0.342(2) 0.970(2) 0.058(8) Uiso 1 1 d . . .
H21 H 0.367(4) 0.491(2) 0.921(2) 0.050(8) Uiso 1 1 d . . .
H7A H 0.509(4) 0.604(2) 0.508(2) 0.056(8) Uiso 1 1 d . . .
H17 H -0.353(5) 0.957(3) 0.522(3) 0.070(10) Uiso 1 1 d . . .
H26 H -0.173(4) 0.895(2) 0.766(2) 0.055(9) Uiso 1 1 d . . .
H25 H -0.313(5) 1.001(3) 0.660(2) 0.079(11) Uiso 1 1 d . . .
H28 H 0.153(4) 0.221(3) 0.878(2) 0.066(9) Uiso 1 1 d . . .
H7B H 0.410(5) 0.652(3) 0.437(2) 0.073(10) Uiso 1 1 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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 Cu1 89.15(4) . 3_566 ?
O1 C1 C2 117.33(16) 3_566 . ?
C1 O1 Cu1 116.70(12) 3_566 . ?
C1 O4 Cu1 128.99(13) . . ?
C2 C7 N1 119.49(18) . . ?
C2 C3 H15 119.0(16) . . ?
C3 C2 C7 117.61(19) . . ?
C3 C2 C1 116.55(19) . . ?
C3 C4 H17 119(2) . . ?
C4 C3 C2 119.7(2) . . ?
C4 C3 H15 121.3(16) . . ?
C4 C5 H25 117(2) . . ?
C5 C4 C3 121.4(3) . . ?
C5 C4 H17 119(2) . . ?
C5 C6 C7 119.2(3) . . ?
C5 C6 H26 125(2) . . ?
C6 C5 C4 120.0(2) . . ?
C6 C5 H25 123(2) . . ?
C6 C7 C2 122.1(2) . . ?
C6 C7 N1 118.3(2) . . ?
C7 C6 H26 116(2) . . ?
C7 C2 C1 125.78(18) . . ?
O2 N1 O3 123.0(2) . . ?
O2 N1 C7 118.46(18) . . ?
O3 N1 C7 118.6(2) . . ?
O11 C11 C12 116.28(18) . . ?
O11 Cu1 O14 168.43(6) . . ?
O11 Cu1 O4 90.17(7) . . ?
O11 Cu1 O1 87.91(7) . . ?
O11 Cu1 O6 97.74(7) . . ?
O11 Cu1 Cu1 85.49(5) . 3_566 ?
C11 O14 Cu1 123.60(13) 3_566 . ?
C11 O11 Cu1 120.93(13) . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 H10 119.2(19) . . ?
C12 C17 N11 120.29(19) . . ?
C13 C12 C17 117.5(2) . . ?
C13 C12 C11 118.4(2) . . ?
C13 C14 H21 118.7(19) . . ?
C14 C15 C16 120.3(2) . . ?
C14 C15 H23 118(2) . . ?
C14 C13 H10 120(2) . . ?
C15 C14 C13 120.6(3) . . ?
C15 C14 H21 120.7(19) . . ?
C15 C16 H28 121.4(19) . . ?
C16 C17 C12 122.4(2) . . ?
C16 C17 N11 117.2(2) . . ?
C16 C15 H23 122(2) . . ?
C17 C16 C15 118.7(3) . . ?
C17 C16 H28 120(2) . . ?
C17 C12 C11 123.78(19) . . ?
O12 N11 O13 123.9(2) . . ?
O12 N11 C17 118.1(2) . . ?
O13 N11 C17 118.0(2) . . ?
O14 C11 C12 117.00(17) 3_566 . ?
O14 Cu1 O4 90.28(6) . . ?
O14 Cu1 O1 89.37(6) . . ?
O14 Cu1 O6 93.68(7) . . ?
O14 Cu1 Cu1 83.23(4) . 3_566 ?
O14 C11 O11 126.63(18) 3_566 . ?
O4 C1 O1 125.65(17) . 3_566 ?
O4 C1 C2 116.74(16) . . ?
O4 Cu1 O1 168.58(5) . . ?
O4 Cu1 O6 96.73(6) . . ?
O1 Cu1 O6 94.68(6) . . ?
O4 Cu1 Cu1 79.48(4) . 3_566 ?
O6 Cu1 Cu1 175.07(5) . 3_566 ?
Cu1 O6 H7A 128(2) . . ?
Cu1 O6 H7B 117(2) . . ?
H7A O6 H7B 111(3) . . ?
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
O1 C1 1.261(2) 3_566 ?
O1 Cu1 1.9822(14) . ?
C1 O4 1.252(2) . ?
C1 O1 1.261(2) 3_566 ?
C1 C2 1.501(3) . ?
C3 C4 1.388(3) . ?
C3 C2 1.390(3) . ?
C3 H15 0.99(3) . ?
C4 C5 1.368(5) . ?
C4 H17 0.91(4) . ?
C5 C6 1.368(4) . ?
C5 H25 0.84(4) . ?
C6 H26 0.86(3) . ?
C7 C6 1.381(3) . ?
C7 C2 1.394(3) . ?
C7 N1 1.459(3) . ?
N1 O3 1.216(3) . ?
O2 N1 1.206(3) . ?
C11 O14 1.248(2) 3_566 ?
C11 O11 1.262(2) . ?
C11 C12 1.496(3) . ?
C12 C17 1.390(3) . ?
C13 C12 1.380(3) . ?
C13 C14 1.385(4) . ?
C13 H10 0.85(3) . ?
C14 C15 1.365(4) . ?
C14 H21 0.92(3) . ?
C15 C16 1.375(5) . ?
C15 H23 0.86(3) . ?
C16 H28 0.92(3) . ?
C17 C16 1.373(3) . ?
N11 O13 1.221(3) . ?
N11 C17 1.471(3) . ?
O12 N11 1.212(3) . ?
O14 C11 1.248(2) 3_566 ?
O14 Cu1 1.9477(14) . ?
Cu1 O11 1.9416(15) . ?
Cu1 O4 1.9681(13) . ?
Cu1 O6 2.1611(16) . ?
Cu1 Cu1 2.6233(7) 3_566 ?
O6 H7A 0.84(3) . ?
O6 H7B 0.86(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -82.7(2) 3_566 . . . ?
O4 C1 C2 C7 -85.4(2) . . . . ?
O1 C1 C2 C7 100.2(2) 3_566 . . . ?
C1 O1 Cu1 O11 87.09(14) 3_566 . . . ?
C1 O1 Cu1 O14 -81.66(14) 3_566 . . . ?
C1 O1 Cu1 O4 6.6(4) 3_566 . . . ?
C1 O1 Cu1 O6 -175.30(14) 3_566 . . . ?
C1 O1 Cu1 Cu1 1.58(13) 3_566 . . 3_566 ?
C2 C3 C4 C5 0.2(4) . . . . ?
C2 C1 O4 Cu1 -174.10(13) . . . . ?
C2 C7 C6 C5 -0.4(3) . . . . ?
C6 C7 N1 O2 178.9(2) . . . . ?
C2 C7 N1 O2 0.7(3) . . . . ?
C6 C7 N1 O3 -0.6(3) . . . . ?
C2 C7 N1 O3 -178.8(2) . . . . ?
C4 C3 C2 C7 0.5(3) . . . . ?
C4 C3 C2 C1 -176.87(19) . . . . ?
C6 C7 C2 C3 -0.4(3) . . . . ?
N1 C7 C2 C3 177.73(18) . . . . ?
C6 C7 C2 C1 176.66(19) . . . . ?
N1 C7 C2 C1 -5.2(3) . . . . ?
O4 C1 C2 C3 91.7(2) . . . . ?
C3 C4 C5 C6 -1.0(4) . . . . ?
C4 C5 C6 C7 1.1(4) . . . . ?
N1 C7 C6 C5 -178.5(2) . . . . ?
C11 O14 Cu1 O11 15.8(4) 3_566 . . . ?
C11 O14 Cu1 O4 -76.42(16) 3_566 . . . ?
C11 O14 Cu1 O1 92.17(16) 3_566 . . . ?
C11 O14 Cu1 O6 -173.19(16) 3_566 . . . ?
C11 O14 Cu1 Cu1 2.95(15) 3_566 . . 3_566 ?
C12 C11 O11 Cu1 -174.57(13) . . . . ?
C12 C17 C16 C15 -1.5(3) . . . . ?
C13 C12 C17 C16 2.3(3) . . . . ?
C11 C12 C17 C16 -171.5(2) . . . . ?
C13 C12 C17 N11 -173.3(2) . . . . ?
C11 C12 C17 N11 12.9(3) . . . . ?
O12 N11 C17 C16 -141.7(2) . . . . ?
O13 N11 C17 C16 35.2(3) . . . . ?
O12 N11 C17 C12 34.2(3) . . . . ?
O13 N11 C17 C12 -148.9(2) . . . . ?
C12 C13 C14 C15 -0.3(4) . . . . ?
C13 C14 C15 C16 1.1(4) . . . . ?
C14 C13 C12 C17 -1.3(3) . . . . ?
C14 C13 C12 C11 172.8(2) . . . . ?
O13 C11 C12 C13 -129.9(2) 3_566 . . . ?
O11 C11 C12 C13 47.0(3) . . . . ?
O14 C11 C12 C17 43.8(3) 3_566 . . . ?
O11 C11 C12 C17 -139.3(2) . . . . ?
O14 C11 O11 Cu1 1.9(3) 3_566 . . . ?
O14 Cu1 O11 C11 -15.9(4) . . . . ?
O4 Cu1 O11 C11 76.35(16) . . . . ?
O1 Cu1 O11 C11 -92.39(16) . . . . ?
O6 Cu1 O11 C11 173.17(15) . . . . ?
Cu1 Cu1 O11 C11 -3.08(15) 3_566 . . . ?
O1 C1 O4 Cu1 -0.2(3) 3_566 . . . ?
O11 Cu1 O4 C1 -86.20(17) . . . . ?
O14 Cu1 O4 C1 82.25(18) . . . . ?
O1 Cu1 O4 C1 -5.9(4) . . . . ?
O6 Cu1 O4 C1 175.99(17) . . . . ?
Cu1 Cu1 O4 C1 -0.81(16) 3_566 . . . ?
N11 C17 C16 C15 174.2(2) . . . . ?
C14 C15 C16 C17 -0.2(4) . . . . ?
