#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/57/4315774.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_4315774
loop_
_publ_author_name
'Rosana P. Sartoris'
'Ricardo C. Santana'
'Ricardo F. Baggio'
'Octavio Peña'
'Mireille Perec'
'Rafael Calvo'
_publ_section_title
;
 Pyrophosphate-Bridged CuII Chain Magnet: {[Na3Cu(P2O7)(NO3)].3H2O}n
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5650
_journal_page_last               5657
_journal_paper_doi               10.1021/ic100398k
_journal_volume                  49
_journal_year                    2010
_chemical_formula_iupac          'Cu, 3Na, (N O3), (O7 P2), 3(H2 O)'
_chemical_formula_moiety         'Cu N O10 P2, 3(H2 O), 3(Na) '
_chemical_formula_sum            'Cu H6 N Na3 O13 P2'
_chemical_formula_weight         422.51
_chemical_name_systematic
; 
Trisodium Copper(ii) nitrate pyrophosphate, trihydrate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2008-09-23 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.1230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2492(5)
_cell_length_b                   8.2446(6)
_cell_length_c                   9.9050(7)
_cell_measurement_reflns_used    3957
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      2.46
_cell_volume                     565.75(7)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT '
_computing_molecular_graphics    'SHELXTL  (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL '
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker Smart CCD area detector'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_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  0.0136
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4550
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.70
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS in SAINT-NT (Bruker, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0235(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1331
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0181
_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/[σ²(Fo²)+(0.0247P)²+0.5208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0489
_reflns_number_gt                1309
_reflns_number_total             1331
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic100398k_si_002.cif
_cod_data_source_block           Cu-Na-Pyro
_cod_original_formula_sum        ' Cu H6 N Na3 O13 P2'
_cod_database_code               4315774
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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 0.5000 1.0000 0.0000 0.00912(10) Uani 1 2 d S . .
P1 P 0.67287(7) 0.7500 0.24530(5) 0.00790(13) Uani 1 2 d S . .
P2 P 0.26909(7) 0.7500 0.12782(5) 0.00781(13) Uani 1 2 d S . .
O1 O 0.8154(2) 0.7500 0.39071(16) 0.0113(3) Uani 1 2 d S . .
O2 O 0.68493(15) 0.90334(14) 0.16293(11) 0.0135(2) Uani 1 1 d . . .
O3 O 0.4586(2) 0.7500 0.26559(15) 0.0099(3) Uani 1 2 d S . .
O4 O 0.27842(15) 0.90459(13) 0.04567(11) 0.0111(2) Uani 1 1 d . . .
O5 O 0.0969(2) 0.7500 0.18344(16) 0.0111(3) Uani 1 2 d S . .
N1 N 0.6227(3) 1.2500 0.2786(2) 0.0125(4) Uani 1 2 d S . .
O11 O 0.8027(2) 1.2500 0.30780(18) 0.0175(3) Uani 1 2 d S . .
O12 O 0.5449(2) 1.2500 0.37657(17) 0.0212(4) Uani 1 2 d S . .
O13 O 0.5180(2) 1.2500 0.15270(16) 0.0140(3) Uani 1 2 d S . .
Na1 Na 0.96836(9) 1.03419(8) 0.17945(7) 0.01542(16) Uani 1 1 d . . .
Na2 Na 1.15779(13) 0.7500 0.42930(9) 0.01425(19) Uani 1 2 d S . .
O1W O 1.21150(18) 1.03336(16) 0.40520(13) 0.0175(3) Uani 1 1 d D . .
H1WA H 1.196(3) 1.096(2) 0.4674(19) 0.032(6) Uiso 1 1 d D . .
H1WB H 1.312(3) 1.060(3) 0.384(3) 0.046(8) Uiso 1 1 d D . .
O2W O 1.1256(2) 1.2500 0.10720(17) 0.0136(3) Uani 1 2 d SD . .
H2WA H 1.2491(14) 1.2500 0.135(2) 0.009(6) Uiso 1 2 d SD . .
H2WB H 1.098(4) 1.2500 0.0176(11) 0.043(11) Uiso 1 2 d SD . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
O2 Cu1 O2 180.0 . 3_675 y
O2 Cu1 O4 86.80(4) . 3_675 y
O2 Cu1 O4 93.20(4) 3_675 3_675 y
O2 Cu1 O4 93.20(4) . . y
O2 Cu1 O4 86.80(4) 3_675 . y
O4 Cu1 O4 180.0 3_675 . y
O2 Cu1 O13 93.66(5) . 3_675 y
O2 Cu1 O13 86.34(5) 3_675 3_675 y
O4 Cu1 O13 95.19(5) 3_675 3_675 y
O4 Cu1 O13 84.81(5) . 3_675 y
O2 Cu1 O13 86.34(5) . . y
O2 Cu1 O13 93.66(5) 3_675 . y
O4 Cu1 O13 84.81(5) 3_675 . y
O4 Cu1 O13 95.19(5) . . y
O13 Cu1 O13 180.00(6) 3_675 . y
O1 P1 O2 112.43(5) . 4_575 ?
O1 P1 O2 112.43(5) . . ?
O2 P1 O2 112.44(9) 4_575 . ?
O1 P1 O3 107.08(8) . . ?
O2 P1 O3 105.93(5) 4_575 . ?
O2 P1 O3 105.93(5) . . ?
O5 P2 O4 111.55(5) . 4_575 ?
O5 P2 O4 111.55(5) . . ?
O4 P2 O4 113.47(9) 4_575 . ?
O5 P2 O3 106.23(8) . . ?
O4 P2 O3 106.77(5) 4_575 . ?
O4 P2 O3 106.77(5) . . ?
P1 O1 Na2 122.64(9) . . ?
P1 O2 Cu1 130.77(7) . . ?
P1 O2 Na1 123.15(6) . . ?
Cu1 O2 Na1 104.62(5) . . ?
P1 O3 P2 119.91(9) . . ?
P2 O4 Cu1 128.89(6) . . ?
P2 O4 Na1 121.30(6) . 3_675 ?
Cu1 O4 Na1 97.76(4) . 3_675 ?
P2 O5 Na2 117.24(9) . 1_455 ?
P2 O5 Na1 109.71(4) . 4_475 ?
Na2 O5 Na1 88.39(4) 1_455 4_475 ?
P2 O5 Na1 109.71(4) . 1_455 ?
Na2 O5 Na1 88.39(4) 1_455 1_455 ?
Na1 O5 Na1 137.07(7) 4_475 1_455 ?
O11 N1 O13 120.94(18) . . ?
O11 N1 O12 119.77(19) . . ?
O13 N1 O12 119.29(18) . . ?
N1 O11 Na2 91.83(13) . 3_776 ?
N1 O12 Na2 96.63(13) . 3_776 ?
N1 O13 Cu1 120.17(5) . . ?
N1 O13 Cu1 120.17(5) . 2_655 ?
Cu1 O13 Cu1 108.66(6) . 2_655 ?
O2 Na1 O2W 147.97(5) . . ?
O2 Na1 O1W 117.57(5) . . ?
O2W Na1 O1W 89.82(5) . . ?
O2 Na1 O4 68.52(4) . 3_675 ?
O2W Na1 O4 81.76(5) . 3_675 ?
O1W Na1 O4 168.33(5) . 3_675 ?
O2 Na1 O5 83.26(5) . 1_655 ?
O2W Na1 O5 120.12(5) . 1_655 ?
O1W Na1 O5 79.41(5) . 1_655 ?
O4 Na1 O5 111.80(5) 3_675 1_655 ?
O2 Na1 Cu1 34.09(3) . . ?
O2W Na1 Cu1 114.30(4) . . ?
O1W Na1 Cu1 147.58(4) . . ?
O4 Na1 Cu1 35.39(3) 3_675 . ?
O5 Na1 Cu1 104.05(4) 1_655 . ?
O2 Na1 Na2 83.59(4) . . ?
O2W Na1 Na2 128.35(5) . . ?
O1W Na1 Na2 44.86(3) . . ?
O4 Na1 Na2 146.26(4) 3_675 . ?
O5 Na1 Na2 43.70(4) 1_655 . ?
Cu1 Na1 Na2 117.30(2) . . ?
O5 Na2 O1W 83.26(4) 1_655 . ?
O5 Na2 O1W 83.26(4) 1_655 4_575 ?
O1W Na2 O1W 155.22(7) . 4_575 ?
O5 Na2 O1 88.00(6) 1_655 . ?
O1W Na2 O1 100.10(4) . . ?
O1W Na2 O1 100.10(4) 4_575 . ?
O5 Na2 O12 132.39(7) 1_655 3_776 ?
O1W Na2 O12 86.93(4) . 3_776 ?
O1W Na2 O12 86.93(4) 4_575 3_776 ?
O1 Na2 O12 139.61(7) . 3_776 ?
O5 Na2 O11 175.84(7) 1_655 3_776 ?
O1W Na2 O11 97.47(4) . 3_776 ?
O1W Na2 O11 97.47(4) 4_575 3_776 ?
O1 Na2 O11 87.84(6) . 3_776 ?
O12 Na2 O11 51.78(5) 3_776 3_776 ?
O5 Na2 Na1 47.92(2) 1_655 4_575 ?
O1W Na2 Na1 130.16(4) . 4_575 ?
O1W Na2 Na1 45.18(3) 4_575 4_575 ?
O1 Na2 Na1 72.90(3) . 4_575 ?
O12 Na2 Na1 130.68(3) 3_776 4_575 ?
O11 Na2 Na1 130.45(3) 3_776 4_575 ?
O5 Na2 Na1 47.92(2) 1_655 . ?
O1W Na2 Na1 45.18(3) . . ?
O1W Na2 Na1 130.16(4) 4_575 . ?
O1 Na2 Na1 72.90(3) . . ?
O12 Na2 Na1 130.68(3) 3_776 . ?
O11 Na2 Na1 130.45(3) 3_776 . ?
Na1 Na2 Na1 87.41(3) 4_575 . ?
Na2 O1W Na1 89.96(5) . . ?
Na2 O1W H1WA 118.1(16) . . ?
Na1 O1W H1WA 117.4(16) . . ?
Na2 O1W H1WB 117.2(19) . . ?
Na1 O1W H1WB 102.9(18) . . ?
H1WA O1W H1WB 109.3(19) . . ?
Na1 O2W Na1 99.21(7) . 4_585 ?
Na1 O2W H2WA 117.5(8) . . ?
Na1 O2W H2WA 117.5(8) 4_585 . ?
Na1 O2W H2WB 109.5(12) . . ?
Na1 O2W H2WB 109.5(12) 4_585 . ?
H2WA O2W H2WB 104(2) . . ?
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 O2 1.9398(10) . y
Cu1 O2 1.9398(10) 3_675 y
Cu1 O4 1.9574(10) 3_675 y
Cu1 O4 1.9574(10) . y
Cu1 O13 2.5371(9) 3_675 y
Cu1 O13 2.5371(9) . y
P1 O1 1.5053(15) . y
P1 O2 1.5210(11) 4_575 y
P1 O2 1.5210(11) . y
P1 O3 1.6238(15) . y
P2 O5 1.5052(15) . y
P2 O4 1.5243(11) 4_575 y
P2 O4 1.5243(11) . y
P2 O3 1.6266(15) . y
N1 O11 1.250(2) . ?
N1 O13 1.255(2) . ?
N1 O12 1.258(2) . ?
Na1 O2W 2.3362(12) . y
Na1 O1W 2.4054(14) . y
Na1 O4 2.4655(12) 3_675 y
Na1 O5 2.5177(9) 1_655 y
Na1 Na2 3.3910(9) . y
Na2 O5 2.3435(17) 1_655 y
Na2 O1W 2.3919(13) . y
Na2 O1W 2.3919(13) 4_575 y
Na2 O12 2.4295(19) 3_776 y
Na2 O11 2.5345(19) 3_776 y
Na2 Na1 3.3910(9) 4_575 y
Cu1 Na1 3.3486(7) . y
Cu1 Na1 3.3486(7) 3_675 y
O1W H1WA 0.840(9) . ?
O1W H1WB 0.844(10) . ?
O2W H2WA 0.855(10) . ?
O2W H2WB 0.851(10) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O1 0.840(9) 1.911(10) 2.7472(17) 174(2) 3_776
O1W H1WB O12 0.844(10) 2.320(17) 3.0847(18) 151(2) 1_655
O2W H2WA O13 0.855(10) 1.905(12) 2.746(2) 167(2) 1_655
O2W H2WB O5 0.851(10) 2.075(15) 2.856(2) 152(3) 3_675
