#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322349.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_4322349
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            'C4 H24 Cu3 N2 O18 P4'
_chemical_formula_weight         702.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.834(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.2137(13)
_cell_length_b                   14.7472(15)
_cell_length_c                   11.1802(12)
_cell_measurement_reflns_used    66
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.80
_cell_measurement_theta_min      5.78
_cell_volume                     985.6(3)
_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       'θ/2θ 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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2434
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        12.47
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.625
_exptl_absorpt_correction_T_max  0.2319
_exptl_absorpt_correction_T_min  0.0786
_exptl_absorpt_correction_type   'empirical psi-scan'
_exptl_crystal_colour            'blue                '
_exptl_crystal_density_diffrn    2.368
_exptl_crystal_description       'block                '
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       0.0512(35)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         1735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_obs          0.0435
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0832P)²+1.2921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1174
_refine_ls_wR_factor_obs         0.1168
_reflns_number_observed          1713
_reflns_number_total             1735
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990481r_1.cif
_cod_data_source_block           (NH4)2Cu3(hedp)2(H2O)4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+1.2921P] 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^)+(0.0832P)^2^+1.2921P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4322349
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu1 Cu -0.5000 0.5000 0.5000 0.0196(3) Uani 1 d S .
Cu2 Cu -1.14302(7) 0.61348(3) 0.20736(4) 0.0188(3) Uani 1 d . .
P1 P -0.89858(15) 0.42483(6) 0.30018(8) 0.0177(3) Uani 1 d . .
P2 P -0.64064(14) 0.58134(6) 0.23978(9) 0.0172(3) Uani 1 d . .
O1W O -1.0047(6) 0.6492(2) 0.4118(3) 0.0286(7) Uani 1 d . .
H1WA H -0.8960(109) 0.6479(46) 0.4193(58) 0.041(19) Uiso 1 d . .
H1WB H -1.0521(117) 0.6093(50) 0.4559(62) 0.058(19) Uiso 1 d . .
O2W O -1.2044(6) 0.7421(2) 0.1554(3) 0.0296(7) Uani 1 d . .
H2WA H -1.3013(109) 0.7597(43) 0.1686(55) 0.044(18) Uiso 1 d . .
H2WB H -1.1129(114) 0.7684(43) 0.1671(59) 0.044(19) Uiso 1 d . .
O1 O -0.7987(4) 0.4479(2) 0.4381(2) 0.0248(6) Uani 1 d . .
O2 O -1.1047(4) 0.4828(2) 0.2396(3) 0.0219(6) Uani 1 d . .
O3 O -0.9519(4) 0.3255(2) 0.2786(3) 0.0250(6) Uani 1 d . .
O4 O -0.5827(5) 0.6007(2) 0.3800(3) 0.0241(6) Uani 1 d . .
O5 O -0.8595(4) 0.6262(2) 0.1692(3) 0.0207(6) Uani 1 d . .
O6 O -0.4592(4) 0.6064(2) 0.1795(3) 0.0237(6) Uani 1 d . .
O7 O -0.4717(4) 0.4188(2) 0.3068(3) 0.0241(6) Uani 1 d . .
H7O H -0.3796(121) 0.4289(57) 0.2758(68) 0.070(24) Uiso 1 d . .
C1 C -0.6777(6) 0.4584(2) 0.2278(3) 0.0182(7) Uani 1 d . .
C2 C -0.7187(8) 0.4236(3) 0.0957(4) 0.0290(9) Uani 1 d . .
H2A H -0.6178(87) 0.4381(37) 0.0528(47) 0.033(12) Uiso 1 d . .
H2B H -0.7164(107) 0.3624(53) 0.0875(61) 0.059(19) Uiso 1 d . .
H2C H -0.8448(118) 0.4498(50) 0.0567(60) 0.063(20) Uiso 1 d . .
N1 N -0.3261(7) 0.7650(3) 0.4644(4) 0.0310(8) Uani 1 d . .
H1NB H -0.1763(175) 0.7466(65) 0.4512(80) 0.108(30) Uiso 1 d . .
H1NA H -0.4012(89) 0.7925(38) 0.3989(49) 0.033(13) Uiso 1 d . .
H1NC H -0.3817(117) 0.7214(56) 0.4663(66) 0.055(22) Uiso 1 d . .
H1ND H -0.3460(88) 0.7998(38) 0.5306(50) 0.036(13) 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 3_466 . ?
O1 Cu1 O4 90.51(12) 3_466 3_466 ?
O1 Cu1 O4 89.49(12) . 3_466 ?
O1 Cu1 O4 89.49(12) 3_466 . ?
O1 Cu1 O4 90.51(12) . . ?
O4 Cu1 O4 180.0 3_466 . ?
O6 Cu2 O5 158.55(13) 1_455 . ?
O6 Cu2 O2 92.53(11) 1_455 . ?
O5 Cu2 O2 93.64(11) . . ?
O6 Cu2 O2W 84.14(13) 1_455 . ?
O5 Cu2 O2W 87.52(13) . . ?
O2 Cu2 O2W 173.37(13) . . ?
O6 Cu2 O1W 105.49(13) 1_455 . ?
O5 Cu2 O1W 94.70(12) . . ?
O2 Cu2 O1W 92.82(12) . . ?
O2W Cu2 O1W 93.59(13) . . ?
O3 P1 O2 110.5(2) . . ?
O3 P1 O1 112.8(2) . . ?
O2 P1 O1 112.3(2) . . ?
O3 P1 C1 110.4(2) . . ?
O2 P1 C1 106.8(2) . . ?
O1 P1 C1 103.7(2) . . ?
O6 P2 O5 109.4(2) . . ?
O6 P2 O4 114.5(2) . . ?
O5 P2 O4 112.0(2) . . ?
O6 P2 C1 107.7(2) . . ?
O5 P2 C1 108.4(2) . . ?
O4 P2 C1 104.4(2) . . ?
P1 O1 Cu1 121.9(2) . . ?
P1 O2 Cu2 132.3(2) . . ?
P2 O4 Cu1 119.9(2) . . ?
P2 O5 Cu2 125.6(2) . . ?
P2 O6 Cu2 143.4(2) . 1_655 ?
O7 C1 C2 109.8(3) . . ?
O7 C1 P2 106.3(2) . . ?
C2 C1 P2 113.0(3) . . ?
O7 C1 P1 105.2(2) . . ?
C2 C1 P1 112.9(3) . . ?
P2 C1 P1 109.2(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 O1 1.953(3) 3_466 ?
Cu1 O1 1.953(3) . ?
Cu1 O4 1.973(3) 3_466 ?
Cu1 O4 1.973(3) . ?
Cu2 O6 1.906(3) 1_455 ?
Cu2 O5 1.931(3) . ?
Cu2 O2 1.963(3) . ?
Cu2 O2W 1.990(3) . ?
Cu2 O1W 2.273(3) . ?
P1 O3 1.506(3) . ?
P1 O2 1.535(3) . ?
P1 O1 1.535(3) . ?
P1 C1 1.841(4) . ?
P2 O6 1.509(3) . ?
P2 O5 1.524(3) . ?
P2 O4 1.537(3) . ?
P2 C1 1.828(4) . ?
O6 Cu2 1.906(3) 1_655 ?
O7 C1 1.464(4) . ?
C1 C2 1.518(5) . ?
