#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322351.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_4322351
loop_
_publ_author_name
'Li-Min Zheng'
'Hui-Hua Song'
'Chun-Ying Duan'
Xin
_publ_section_title
;
 Template-Directed One- and Two-Dimensional Copper(II) Diphosphonates:
 Structures and Characterizations of (NH4)2Cu3(hedp)2(H2O)4,
 [NH3(CH2)4NH3]Cu3(hedp)2.2H2O, and [NH2(C2H4)2NH2]Cu3(hedp)2 (hedp =
 1-Hydroxyethylidenediphosphonate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5061
_journal_page_last               5066
_journal_paper_doi               10.1021/ic990481r
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C8 H20 Cu3 N2 O14 P4'
_chemical_formula_weight         682.76
_chemical_name_systematic
; 
 ? 
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                112.611(13)
_cell_angle_beta                 90.819(8)
_cell_angle_gamma                92.824(7)
_cell_formula_units_Z            1
_cell_length_a                   7.0155(6)
_cell_length_b                   8.0904(9)
_cell_length_c                   9.2644(11)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.83
_cell_measurement_theta_min      8.77
_cell_volume                     484.51(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2θ/ω 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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2648
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        4.83
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.669
_exptl_absorpt_correction_T_max  0.5098
_exptl_absorpt_correction_T_min  0.3150
_exptl_absorpt_correction_type   'empirical psi-scan'
_exptl_crystal_colour            'blue                 '
_exptl_crystal_density_diffrn    2.340
_exptl_crystal_description       'block                 '
_exptl_crystal_F_000             341
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.511
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0474(50)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_obs          0.0297
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0512P)²+0.6758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0849
_refine_ls_wR_factor_obs         0.0839
_reflns_number_observed          2047
_reflns_number_total             2139
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990481r_3.cif
_cod_data_source_block           (H2pip)cu3(hedp)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.6758P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.6758P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        484.51(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4322351
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu1 Cu 1.0000 0.5000 1.0000 0.0149(2) Uani 1 d S .
Cu2 Cu 1.14460(4) 0.26335(4) 0.49718(4) 0.01378(15) Uani 1 d . .
P1 P 0.86280(9) 0.50291(8) 0.69649(7) 0.0134(2) Uani 1 d . .
P2 P 0.89967(9) 0.14963(8) 0.71474(7) 0.0134(2) Uani 1 d . .
O1 O 0.8352(3) 0.5807(3) 0.8748(2) 0.0183(4) Uani 1 d . .
O3 O 0.7531(3) 0.6119(3) 0.6263(2) 0.0173(4) Uani 1 d . .
O2 O 1.0729(3) 0.4861(2) 0.6591(2) 0.0180(4) Uani 1 d . .
O4 O 0.9044(3) 0.2517(3) 0.8912(2) 0.0188(4) Uani 1 d . .
O6 O 0.8013(3) -0.0370(2) 0.6743(2) 0.0183(4) Uani 1 d . .
O5 O 1.0971(3) 0.1399(2) 0.6424(2) 0.0166(4) Uani 1 d . .
O7 O 0.7848(3) 0.1984(3) 0.4575(2) 0.0237(4) Uani 1 d . .
H7O H 0.8004(55) 0.0916(58) 0.4243(45) 0.024(9) Uiso 1 d . .
C1 C 0.7568(4) 0.2721(3) 0.6249(3) 0.0156(5) Uani 1 d . .
C2 C 0.5457(4) 0.2691(5) 0.6604(4) 0.0261(6) Uani 1 d . .
H2B H 0.5428(57) 0.3286(55) 0.7733(51) 0.031(10) Uiso 1 d . .
H2A H 0.5087(73) 0.1613(71) 0.6253(59) 0.053(14) Uiso 1 d . .
H2C H 0.4878(74) 0.3556(72) 0.6249(63) 0.058(14) Uiso 1 d . .
N1 N 0.6503(4) 0.8860(4) 0.9261(3) 0.0234(5) Uani 1 d . .
H1NA H 0.6905(50) 0.9288(47) 0.8625(43) 0.018(8) Uiso 1 d . .
H1NB H 0.7264(66) 0.7885(64) 0.9193(53) 0.043(12) Uiso 1 d . .
C3 C 0.4460(5) 0.8201(4) 0.8900(4) 0.0271(6) Uani 1 d . .
H3A H 0.4157(54) 0.7620(52) 0.9576(46) 0.027(9) Uiso 1 d . .
H3B H 0.4317(55) 0.7450(55) 0.7957(49) 0.027(10) Uiso 1 d . .
C4 C 0.3187(5) 0.9729(5) 0.9138(4) 0.0284(7) Uani 1 d . .
H4A H 0.3433(51) 1.0237(48) 0.8444(43) 0.018(8) Uiso 1 d . .
H4B H 0.1961(65) 0.9418(56) 0.9097(49) 0.034(11) Uiso 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 . 2_767 ?
O1 Cu1 O4 92.00(8) . . ?
O1 Cu1 O4 88.00(8) 2_767 . ?
O1 Cu1 O4 88.00(8) . 2_767 ?
O1 Cu1 O4 92.00(8) 2_767 2_767 ?
O4 Cu1 O4 180.0 . 2_767 ?
O3 Cu2 O2 91.68(8) 2_766 . ?
O3 Cu2 O6 88.17(8) 2_766 2_756 ?
O2 Cu2 O6 175.76(8) . 2_756 ?
O3 Cu2 O5 167.50(8) 2_766 . ?
O2 Cu2 O5 89.24(8) . . ?
O6 Cu2 O5 91.82(8) 2_756 . ?
O3 P1 O2 115.94(11) . . ?
O3 P1 O1 108.07(11) . . ?
O2 P1 O1 111.40(11) . . ?
O3 P1 C1 109.71(12) . . ?
O2 P1 C1 105.68(11) . . ?
O1 P1 C1 105.52(11) . . ?
O4 P2 O6 109.18(11) . . ?
O4 P2 O5 113.68(11) . . ?
O6 P2 O5 112.01(11) . . ?
O4 P2 C1 108.15(12) . . ?
O6 P2 C1 108.35(12) . . ?
O5 P2 C1 105.21(11) . . ?
P1 O1 Cu1 116.91(11) . . ?
P1 O3 Cu2 126.42(12) . 2_766 ?
P1 O2 Cu2 117.31(11) . . ?
P2 O4 Cu1 124.98(12) . . ?
P2 O6 Cu2 128.18(12) . 2_756 ?
P2 O5 Cu2 118.63(11) . . ?
O7 C1 C2 111.3(2) . . ?
O7 C1 P1 105.5(2) . . ?
C2 C1 P1 111.2(2) . . ?
O7 C1 P2 108.4(2) . . ?
C2 C1 P2 113.4(2) . . ?
P1 C1 P2 106.71(13) . . ?
C4 N1 C3 112.5(2) 2_677 . ?
N1 C3 C4 111.2(3) . . ?
N1 C4 C3 110.8(3) 2_677 . ?
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 O1 1.931(2) . ?
Cu1 O1 1.931(2) 2_767 ?
Cu1 O4 1.948(2) . ?
Cu1 O4 1.948(2) 2_767 ?
Cu2 O3 1.919(2) 2_766 ?
Cu2 O2 1.945(2) . ?
Cu2 O6 1.967(2) 2_756 ?
Cu2 O5 1.983(2) . ?
P1 O3 1.512(2) . ?
P1 O2 1.520(2) . ?
P1 O1 1.544(2) . ?
P1 C1 1.837(3) . ?
P2 O4 1.521(2) . ?
P2 O6 1.533(2) . ?
P2 O5 1.540(2) . ?
P2 C1 1.841(3) . ?
O3 Cu2 1.919(2) 2_766 ?
O6 Cu2 1.967(2) 2_756 ?
O7 C1 1.452(3) . ?
C1 C2 1.523(4) . ?
N1 C4 1.488(4) 2_677 ?
N1 C3 1.492(4) . ?
C3 C4 1.510(4) . ?
C4 N1 1.488(4) 2_677 ?
