#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/79/2207922.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2207922
loop_
_publ_author_name
'Zibaseresht, Ramin'
'Hartshorn, Richard M.'
_publ_section_title
;
 Hexaaquacopper(II) dinitrate: absence of Jahn--Teller distortion
;
_journal_coeditor_code           WM6123
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i19
_journal_page_last               i22
_journal_paper_doi               10.1107/S1600536805041851
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Cu (H2 O1)6] (N O3)2'
_chemical_formula_moiety         'Cu H12 O6 2+, 2N O3 -'
_chemical_formula_sum            'Cu H12 N2 O12'
_chemical_formula_weight         295.67
_chemical_name_systematic
;
Hexaaquacopper(II) dinitrate
;
_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                106.428(2)
_cell_angle_beta                 98.399(2)
_cell_angle_gamma                101.504(2)
_cell_formula_units_Z            2
_cell_length_a                   5.7404(8)
_cell_length_b                   7.6452(10)
_cell_length_c                   11.4655(15)
_cell_measurement_reflns_used    2722
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      26.345
_cell_measurement_theta_min      2.872
_cell_volume                     461.84(11)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics
;
SHELXTL and MERCURY (Version 1.4; Bruno et al.,  2002)
;
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2917
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.432
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.3411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.598
_refine_diff_density_min         -1.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1556
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0546P)²+2.7318P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                1494
_reflns_number_total             1556
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm6123.cif
_cod_data_source_block           II
_cod_original_formula_sum        'Cu H12  N2 O12'
_cod_database_code               2207922
_cod_database_fobs_code          2207922
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cu 0.17237(7) 0.14519(6) 0.23243(4) 0.00973(18) Uani d . 1 Cu
O1 0.2520(4) -0.0653(4) 0.1031(2) 0.0095(5) Uani d D 1 O
H1A 0.230(7) -0.058(5) 0.018(2) 0.011 Uiso d D 1 H
H1B 0.180(7) -0.189(4) 0.106(3) 0.011 Uiso d D 1 H
O2 0.5425(4) 0.2400(4) 0.3146(2) 0.0094(5) Uani d D 1 O
H2A 0.607(7) 0.372(3) 0.323(3) 0.011 Uiso d D 1 H
H2B 0.581(7) 0.216(5) 0.394(2) 0.011 Uiso d D 1 H
O3 0.0978(4) 0.3582(4) 0.3683(2) 0.0102(5) Uani d D 1 O
H3A 0.185(7) 0.479(4) 0.365(3) 0.012 Uiso d D 1 H
H3B 0.138(7) 0.343(5) 0.449(2) 0.012 Uiso d D 1 H
O4 -0.1905(4) 0.0364(3) 0.1453(2) 0.0088(5) Uani d D 1 O
H4A -0.291(6) 0.107(4) 0.190(3) 0.011 Uiso d D 1 H
H4B -0.234(7) -0.097(3) 0.137(4) 0.011 Uiso d D 1 H
O5 0.2220(4) 0.3095(4) 0.1238(2) 0.0105(5) Uani d D 1 O
H5A 0.388(4) 0.340(5) 0.111(4) 0.013 Uiso d D 1 H
H5B 0.144(6) 0.412(4) 0.134(4) 0.013 Uiso d D 1 H
O6 0.1346(4) -0.0050(4) 0.3531(2) 0.0096(5) Uani d D 1 O
H6A -0.037(4) -0.048(5) 0.352(4) 0.012 Uiso d D 1 H
H6B 0.221(6) -0.102(5) 0.356(4) 0.012 Uiso d D 1 H
N1 0.7929(5) 0.5522(4) 0.1275(3) 0.0093(6) Uani d . 1 N
O11 0.6585(4) 0.6598(4) 0.1232(2) 0.0119(5) Uani d . 1 O
O12 0.7080(4) 0.3869(4) 0.1234(2) 0.0124(5) Uani d . 1 O
O13 1.0202(4) 0.6086(4) 0.1371(2) 0.0132(6) Uani d . 1 O
N2 0.5813(5) 0.7634(4) 0.3903(3) 0.0102(6) Uani d . 1 N
O21 0.6533(5) 0.9126(4) 0.3697(2) 0.0124(5) Uani d . 1 O
O22 0.3683(4) 0.7234(4) 0.4107(2) 0.0145(6) Uani d . 1 O
O23 0.7148(4) 0.6530(4) 0.3925(2) 0.0125(5) Uani d . 1 O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O5 Cu O1 89.49(10) y
O5 Cu O6 175.94(10) y
O1 Cu O6 93.58(10) y
O5 Cu O4 91.38(10) y
O1 Cu O4 88.81(10) y
O6 Cu O4 91.34(10) y
O5 Cu O3 91.72(10) y
O1 Cu O3 178.31(10) y
O6 Cu O3 85.17(10) y
O4 Cu O3 92.35(10) y
O5 Cu O2 89.50(10) y
O1 Cu O2 87.93(10) y
O6 Cu O2 87.96(10) y
O4 Cu O2 176.61(9) y
O3 Cu O2 90.89(10) y
Cu O1 H1A 116(2) ?
Cu O1 H1B 113(2) ?
H1A O1 H1B 113(2) ?
Cu O2 H2A 112(2) ?
Cu O2 H2B 113(2) ?
H2A O2 H2B 112(2) ?
Cu O3 H3A 108(2) ?
Cu O3 H3B 110(2) ?
H3A O3 H3B 113(2) ?
Cu O4 H4A 111(2) ?
Cu O4 H4B 108(2) ?
H4A O4 H4B 113(2) ?
Cu O5 H5A 114(2) ?
Cu O5 H5B 118(2) ?
H5A O5 H5B 114(3) ?
Cu O6 H6A 110(2) ?
Cu O6 H6B 122(2) ?
H6A O6 H6B 112(2) ?
O11 N1 O12 120.8(3) ?
O11 N1 O13 120.7(3) ?
O12 N1 O13 118.5(3) ?
O21 N2 O23 121.1(3) ?
O21 N2 O22 118.9(3) ?
O23 N2 O22 120.0(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cu O5 2.014(2) y
Cu O1 2.034(2) y
Cu O6 2.041(2) y
Cu O4 2.064(2) y
Cu O3 2.074(2) y
Cu O2 2.084(2) y
O1 H1A 0.981(18) ?
O1 H1B 0.966(18) ?
O2 H2A 0.976(18) ?
O2 H2B 0.981(18) ?
O3 H3A 0.977(18) ?
O3 H3B 0.966(18) ?
O4 H4A 0.970(18) ?
O4 H4B 0.974(18) ?
O5 H5A 0.974(18) ?
O5 H5B 0.963(18) ?
O6 H6A 0.973(18) ?
O6 H6B 0.978(18) ?
N1 O11 1.241(4) y
N1 O12 1.245(4) y
N1 O13 1.268(4) y
N2 O21 1.233(4) y
N2 O23 1.252(4) y
N2 O22 1.272(4) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1A O4 2 0.981(18) 1.914(18) 2.894(3) 179(3)
O1 H1B O13 1_445 0.966(18) 1.788(19) 2.741(4) 168(4)
O2 H2B O22 2_666 0.981(18) 2.12(2) 3.038(4) 156(3)
O2 H2A O23 . 0.976(18) 2.00(2) 2.940(4) 162(3)
O2 H2B O21 1_545 0.981(18) 2.38(3) 2.912(4) 113(3)
O3 H3A O22 . 0.977(18) 1.83(2) 2.779(4) 162(3)
O3 H3B O23 2_666 0.966(18) 1.88(2) 2.827(4) 167(3)
O4 H4A O2 1_455 0.970(18) 1.99(2) 2.942(4) 167(4)
O4 H4A O1 1_455 0.970(18) 2.60(4) 3.070(3) 110(3)
O4 H4B O11 1_445 0.974(18) 1.79(2) 2.763(4) 175(3)
O5 H5A O12 . 0.974(18) 1.78(2) 2.735(3) 166(4)
O5 H5A N1 . 0.974(18) 2.50(3) 3.417(4) 156(3)
O5 H5A O11 . 0.974(18) 2.58(3) 3.285(3) 130(3)
O5 H5B O13 1_455 0.963(18) 1.78(2) 2.740(4) 172(4)
O5 H5B N1 1_455 0.963(18) 2.47(2) 3.365(4) 155(3)
O5 H5B O12 1_455 0.963(18) 2.45(3) 3.123(3) 126(3)
O6 H6B O21 1_545 0.978(18) 2.44(3) 3.154(3) 130(3)
O6 H6B O22 1_545 0.978(18) 1.91(2) 2.860(4) 162(4)
O6 H6B N2 1_545 0.978(18) 2.51(2) 3.436(4) 157(3)
