#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/31/2233138.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_2233138
loop_
_publ_author_name
'Zhang, Shi-Yong'
'Zhou, Zhong-Gao'
'Wang, Ke-Jun'
_publ_section_title
;
 Poly[[{μ₃-dihydrogen
 [(pyridin-4-ylmethylimino)bis(methylene)]diphosphonato-κ⁵O:O',N,O'':N'}copper(II)]
 dihydrate]
;
_journal_coeditor_code           FJ2483
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m38
_journal_page_last               m39
_journal_paper_doi               10.1107/S1600536811052512
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu (C8 H12 N2 O6 P2)], 2H2 O'
_chemical_formula_moiety         'C8 H12 Cu N2 O6 P2, 2(H2 O)'
_chemical_formula_sum            'C8 H16 Cu N2 O8 P2'
_chemical_formula_weight         393.71
_chemical_name_systematic
;
Poly[[{μ₃-dihydrogen [(pyridin-4-ylmethylimino)bis(methylene)]diphosphonato-
κ⁵O:O',N,O'':N'}copper(II)] dihydrate]
;
_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                75.648(2)
_cell_angle_beta                 67.124(2)
_cell_angle_gamma                67.126(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9250(3)
_cell_length_b                   9.0000(3)
_cell_length_c                   10.5066(3)
_cell_measurement_reflns_used    1430
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.12
_cell_volume                     711.75(4)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2010)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7659
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.603
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3267
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0459
_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)+(0.0550P)²+0.1702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                2309
_reflns_number_total             3267
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fj2483.cif
_cod_data_source_block           I
_cod_database_code               2233138
_cod_database_fobs_code          2233138
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
Cu Cu1 0.47006(6) 0.60143(5) 0.25556(5) 0.02485(17) Uani d . 1 1
P P1 0.69833(14) 0.32696(12) 0.39341(11) 0.0237(2) Uani d . 1 1
P P2 0.17163(14) 0.57368(13) 0.21239(12) 0.0265(3) Uani d . 1 1
N N1 0.5076(4) -0.1825(4) 0.2025(3) 0.0240(7) Uani d . 1 1
N N2 0.4396(4) 0.3746(4) 0.2980(3) 0.0207(7) Uani d . 1 1
C C1 0.3823(5) -0.0485(5) 0.1777(4) 0.0282(9) Uani d . 1 1
H H1A 0.2869 -0.0590 0.1696 0.034 Uiso calc R 1 1
C C2 0.3912(5) 0.1042(5) 0.1641(4) 0.0293(10) Uani d . 1 1
H H2A 0.3025 0.1945 0.1457 0.035 Uiso calc R 1 1
C C3 0.5301(5) 0.1261(4) 0.1773(4) 0.0233(9) Uani d . 1 1
C C4 0.6596(6) -0.0148(5) 0.1992(4) 0.0294(9) Uani d . 1 1
H H4A 0.7570 -0.0076 0.2065 0.035 Uiso calc R 1 1
C C5 0.6465(5) -0.1652(5) 0.2102(4) 0.0273(9) Uani d . 1 1
H H5A 0.7364 -0.2575 0.2233 0.033 Uiso calc R 1 1
C C6 0.5389(5) 0.2920(4) 0.1674(4) 0.0243(9) Uani d . 1 1
H H6A 0.4964 0.3607 0.0933 0.029 Uiso calc R 1 1
H H6B 0.6587 0.2831 0.1412 0.029 Uiso calc R 1 1
C C7 0.5053(5) 0.2840(5) 0.4152(4) 0.0235(9) Uani d . 1 1
H H7A 0.5324 0.1684 0.4164 0.028 Uiso calc R 1 1
H H7B 0.4179 0.3168 0.5029 0.028 Uiso calc R 1 1
C C8 0.2500(5) 0.4113(5) 0.3387(4) 0.0224(8) Uani d . 1 1
H H8A 0.1931 0.4454 0.4312 0.027 Uiso calc R 1 1
H H8B 0.2255 0.3151 0.3391 0.027 Uiso calc R 1 1
O O1 0.8567(4) 0.1971(3) 0.3047(3) 0.0309(7) Uani d . 1 1
H H1B 0.9034 0.2423 0.2302 0.046 Uiso calc R 1 1
O O2 0.6750(3) 0.4935(3) 0.3111(3) 0.0278(6) Uani d . 1 1
O O3 0.7175(4) 0.3101(3) 0.5319(3) 0.0307(7) Uani d . 1 1
O O4 0.2907(3) 0.6731(3) 0.1706(3) 0.0273(6) Uani d . 1 1
O O5 0.1664(4) 0.5097(3) 0.0961(3) 0.0356(7) Uani d . 1 1
O O6 -0.0163(4) 0.6712(4) 0.2955(3) 0.0393(8) Uani d . 1 1
H H6C -0.0137 0.7334 0.3394 0.059 Uiso calc R 1 1
O O1W 1.0256(4) 0.3000(4) 0.0716(3) 0.0381(8) Uani d D 1 1
H H1WA 1.065(6) 0.366(5) 0.078(5) 0.057 Uiso d D 1 1
H H1WB 0.964(6) 0.344(5) 0.021(5) 0.057 Uiso d D 1 1
O O2W -0.0383(5) 0.8732(4) 0.4421(4) 0.0462(9) Uani d D 1 1
H H2WA -0.037(7) 0.965(4) 0.397(5) 0.069 Uiso d D 1 1
H H2WB 0.053(5) 0.832(6) 0.464(6) 0.069 Uiso d D 1 1
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'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Cu1 O4 . . 167.12(11)
O2 Cu1 N1 . 1_565 93.65(12)
O4 Cu1 N1 . 1_565 92.92(12)
O2 Cu1 N2 . . 86.48(11)
O4 Cu1 N2 . . 86.29(11)
N1 Cu1 N2 1_565 . 176.50(13)
O2 Cu1 O3 . 2_666 96.97(11)
O4 Cu1 O3 . 2_666 94.37(11)
N1 Cu1 O3 1_565 2_666 87.53(12)
N2 Cu1 O3 . 2_666 95.93(11)
O3 P1 O2 . . 116.53(16)
O3 P1 O1 . . 108.57(16)
O2 P1 O1 . . 110.13(17)
O3 P1 C7 . . 110.01(18)
O2 P1 C7 . . 103.88(16)
O1 P1 C7 . . 107.31(17)
O5 P2 O4 . . 115.75(17)
O5 P2 O6 . . 108.56(17)
O4 P2 O6 . . 111.15(16)
O5 P2 C8 . . 112.42(17)
O4 P2 C8 . . 103.00(16)
O6 P2 C8 . . 105.44(18)
C1 N1 C5 . . 118.3(3)
C1 N1 Cu1 . 1_545 120.0(3)
C5 N1 Cu1 . 1_545 121.1(3)
C7 N2 C8 . . 111.7(3)
C7 N2 C6 . . 112.3(3)
C8 N2 C6 . . 112.8(3)
C7 N2 Cu1 . . 107.6(2)
C8 N2 Cu1 . . 104.3(2)
C6 N2 Cu1 . . 107.7(2)
N1 C1 C2 . . 121.7(4)
N1 C1 H1A . . 119.1
C2 C1 H1A . . 119.1
C1 C2 C3 . . 121.3(4)
C1 C2 H2A . . 119.4
C3 C2 H2A . . 119.4
C4 C3 C2 . . 115.6(3)
C4 C3 C6 . . 122.4(4)
C2 C3 C6 . . 121.9(3)
C5 C4 C3 . . 121.1(4)
C5 C4 H4A . . 119.4
C3 C4 H4A . . 119.4
N1 C5 C4 . . 121.9(4)
N1 C5 H5A . . 119.0
C4 C5 H5A . . 119.0
C3 C6 N2 . . 115.5(3)
C3 C6 H6A . . 108.4
N2 C6 H6A . . 108.4
C3 C6 H6B . . 108.4
N2 C6 H6B . . 108.4
H6A C6 H6B . . 107.5
N2 C7 P1 . . 109.1(3)
N2 C7 H7A . . 109.9
P1 C7 H7A . . 109.9
N2 C7 H7B . . 109.9
P1 C7 H7B . . 109.9
H7A C7 H7B . . 108.3
N2 C8 P2 . . 108.1(3)
N2 C8 H8A . . 110.1
P2 C8 H8A . . 110.1
N2 C8 H8B . . 110.1
P2 C8 H8B . . 110.1
H8A C8 H8B . . 108.4
P1 O1 H1B . . 109.5
P1 O2 Cu1 . . 119.08(16)
P1 O3 Cu1 . 2_666 133.88(16)
P2 O4 Cu1 . . 117.93(16)
P2 O6 H6C . . 109.5
H1WA O1W H1WB . . 109(4)
H2WA O2W H2WB . . 107(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 O2 . 1.949(3)
Cu1 O4 . 1.949(2)
Cu1 N1 1_565 2.008(3)
Cu1 N2 . 2.080(3)
Cu1 O3 2_666 2.315(3)
P1 O3 . 1.495(3)
P1 O2 . 1.514(3)
P1 O1 . 1.570(3)
P1 C7 . 1.827(4)
P2 O5 . 1.497(3)
P2 O4 . 1.518(3)
P2 O6 . 1.563(3)
P2 C8 . 1.831(4)
N1 C1 . 1.340(5)
N1 C5 . 1.341(5)
N1 Cu1 1_545 2.008(3)
N2 C7 . 1.489(5)
N2 C8 . 1.492(5)
N2 C6 . 1.507(5)
C1 C2 . 1.376(6)
C1 H1A . 0.9300
C2 C3 . 1.390(5)
C2 H2A . 0.9300
C3 C4 . 1.385(5)
C3 C6 . 1.501(5)
C4 C5 . 1.376(5)
C4 H4A . 0.9300
C5 H5A . 0.9300
C6 H6A . 0.9700
C6 H6B . 0.9700
C7 H7A . 0.9700
C7 H7B . 0.9700
C8 H8A . 0.9700
C8 H8B . 0.9700
O1 H1B . 0.8200
O3 Cu1 2_666 2.315(3)
O6 H6C . 0.8200
O1W H1WA . 0.832(19)
O1W H1WB . 0.836(19)
O2W H2WA . 0.846(19)
O2W H2WB . 0.848(19)
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 H1B O1W . 0.82 1.68 2.494(4) 169
O6 H6C O2W . 0.82 1.75 2.567(5) 172
O1W H1WA O5 1_655 0.832(19) 1.916(19) 2.746(4) 177(5)
O1W H1WB O5 2_665 0.836(19) 1.93(2) 2.747(4) 167(5)
O2W H2WA O1 1_465 0.846(19) 2.09(3) 2.882(4) 155(5)
O2W H2WB O3 2_666 0.848(19) 1.96(3) 2.776(4) 161(6)
