#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322350.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_4322350
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 H13 Cu1.5 N O8 P2'
_chemical_formula_weight         360.40
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                111.68(2)
_cell_angle_beta                 96.188(14)
_cell_angle_gamma                96.97(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4840(12)
_cell_length_b                   8.032(3)
_cell_length_c                   10.007(2)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.32
_cell_measurement_theta_min      6.80
_cell_volume                     547.2(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       '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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2017
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.22
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.261
_exptl_absorpt_correction_T_max  0.4738
_exptl_absorpt_correction_T_min  0.3397
_exptl_absorpt_correction_type   'empirical psi-scan'
_exptl_crystal_colour            pale-blue
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_description       block
_exptl_crystal_F_000             363
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         '1.422 (0.954\%A from Cu(2))'
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       0.0020(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         1865
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_obs          0.0527
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0952P)²+2.3994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1523
_refine_ls_wR_factor_obs         0.1432
_reflns_number_observed          1589
_reflns_number_total             1865
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990481r_2.cif
_cod_data_source_block           '[NH3(CH2)4NH3]Cu3(hedp)2.2H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+2.3994P] 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^)+(0.0952P)^2^+2.3994P] 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        547.3(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C4 H13 Cu1.50 N O8 P2'
_cod_database_code               4322350
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 0.5000 1.0000 1.5000 0.0180(2) Uani 1 d S .
Cu2 Cu 0.62843(8) 0.77638(7) 0.99437(6) 0.0133(2) Uani 1 d . .
P1 P 0.3924(2) 0.9946(2) 1.18735(12) 0.0118(3) Uani 1 d . .
P2 P 0.4432(2) 0.6422(2) 1.20352(13) 0.0144(3) Uani 1 d . .
O1 O 0.4002(5) 1.0793(4) 1.3516(4) 0.0195(8) Uani 1 d . .
O3 O 0.2698(5) 1.0852(4) 1.1121(4) 0.0173(8) Uani 1 d . .
O2 O 0.5797(5) 0.9936(4) 1.1418(4) 0.0152(8) Uani 1 d . .
O5 O 0.6186(5) 0.6547(4) 1.1370(4) 0.0170(8) Uani 1 d . .
O6 O 0.3530(5) 0.4444(4) 1.1639(4) 0.0218(8) Uani 1 d U .
O4 O 0.4739(6) 0.7447(5) 1.3670(4) 0.0265(9) Uani 1 d . .
O7 O 0.2824(5) 0.6811(5) 0.9668(4) 0.0195(8) Uani 1 d . .
H7O H 0.3245(5) 0.6033(5) 0.8613(4) 0.023 Uiso 1 d R .
C1 C 0.2880(7) 0.7532(6) 1.1237(5) 0.0124(10) Uani 1 d . .
C2 C 0.0961(8) 0.7273(8) 1.1614(7) 0.0302(14) Uani 1 d . .
H2A H 0.1015(8) 0.7904(8) 1.2767(7) 0.045 Uiso 1 d R .
H2B H 0.0300(8) 0.7884(8) 1.1289(7) 0.045 Uiso 1 d R .
H2C H 0.0420(8) 0.6055(8) 1.1364(7) 0.045 Uiso 1 d R .
O1W O 0.1593(8) 1.0059(7) 1.5920(6) 0.0513(14) Uani 1 d . .
H1WB H 0.2779(8) 1.1389(7) 1.6591(6) 0.062 Uiso 1 d R .
H1WA H 0.1291(8) 0.8968(7) 1.6419(6) 0.062 Uiso 1 d R .
C7 C 0.0862(8) 0.5241(17) 0.4746(12) 0.036(4) Uiso 0.341(6) d PD 1
H7A H 0.0757(8) 0.4652(17) 0.3707(12) 0.044 Uiso 0.341(6) d PR 1
H7B H 0.1143(8) 0.6533(17) 0.5016(12) 0.044 Uiso 0.341(6) d PR 1
C6 C 0.2329(13) 0.4629(21) 0.5479(15) 0.034(4) Uiso 0.341(6) d PD 1
H6A H 0.1941(13) 0.3383(21) 0.5337(15) 0.040 Uiso 0.341(6) d PR 1
H6B H 0.2546(13) 0.5350(21) 0.6507(15) 0.040 Uiso 0.341(6) d PR 1
N2 N 0.4059(12) 0.4807(14) 0.4897(11) 0.005(2) Uiso 0.341(6) d PD 1
H2D H 0.4934(12) 0.4429(14) 0.5347(11) 0.007 Uiso 0.341(6) d PR 1
H2E H 0.3852(12) 0.4119(14) 0.3935(11) 0.007 Uiso 0.341(6) d PR 1
H2F H 0.4424(12) 0.5978(14) 0.5041(11) 0.007 Uiso 0.341(6) d PR 1
C3 C 0.0011(13) 0.6348(13) 0.6642(10) 0.060(3) Uiso 0.659(6) d PD 2
H3A H -0.0463(13) 0.5550(13) 0.7084(10) 0.072 Uiso 0.659(6) d PR 2
H3B H -0.0939(13) 0.6320(13) 0.5904(10) 0.072 Uiso 0.329(3) d PR 2
H3C H 0.1152(13) 0.5994(13) 0.6399(10) 0.072 Uiso 0.329(3) d PR 3
C4 C 0.1558(20) 0.5626(20) 0.5899(22) 0.065(7) Uiso 0.329(3) d PD 2
H4A H 0.2493(20) 0.5620(20) 0.6633(22) 0.078 Uiso 0.329(3) d PR 2
H4B H 0.2055(20) 0.6445(20) 0.5483(22) 0.078 Uiso 0.329(3) d PR 2
C5 C 0.1037(29) 0.3754(21) 0.4743(14) 0.055(6) Uiso 0.329(3) d PD 2
H5A H 0.0309(29) 0.3000(21) 0.5106(14) 0.065 Uiso 0.329(3) d PR 2
H5B H 0.2128(29) 0.3259(21) 0.4542(14) 0.065 Uiso 0.329(3) d PR 2
N1 N 0.0498(8) 0.8264(8) 0.7789(6) 0.0160(14) Uiso 0.659(6) d PD .
H1A H 0.1628(8) 0.8193(8) 0.8151(6) 0.019 Uiso 0.659(6) d PR .
H1B H -0.0185(8) 0.8130(8) 0.8441(6) 0.019 Uiso 0.659(6) d PR .
H1N H 0.0635(8) 0.9482(8) 0.8085(6) 0.019 Uiso 0.659(6) d PR .
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 180.000(2) 2_678 . ?
O1 Cu1 O4 85.37(15) 2_678 . ?
O1 Cu1 O4 94.63(15) . . ?
O1 Cu1 O4 94.63(15) 2_678 2_678 ?
O1 Cu1 O4 85.37(15) . 2_678 ?
O4 Cu1 O4 180.000(2) . 2_678 ?
O6 Cu2 O2 173.1(2) 2_667 . ?
O6 Cu2 O3 89.00(15) 2_667 2_677 ?
O2 Cu2 O3 91.59(15) . 2_677 ?
O6 Cu2 O5 93.1(2) 2_667 . ?
O2 Cu2 O5 88.82(14) . . ?
O3 Cu2 O5 159.27(15) 2_677 . ?
O2 P1 O1 113.3(2) . . ?
O2 P1 O3 112.3(2) . . ?
O1 P1 O3 110.3(2) . . ?
O2 P1 C1 105.1(2) . . ?
O1 P1 C1 107.7(2) . . ?
O3 P1 C1 107.6(2) . . ?
O4 P2 O6 109.9(2) . . ?
O4 P2 O5 113.0(2) . . ?
O6 P2 O5 112.0(2) . . ?
O4 P2 C1 107.2(2) . . ?
O6 P2 C1 108.9(2) . . ?
O5 P2 C1 105.4(2) . . ?
P1 O1 Cu1 129.4(2) . . ?
P1 O3 Cu2 120.6(2) . 2_677 ?
P1 O2 Cu2 119.3(2) . . ?
P2 O5 Cu2 118.7(2) . . ?
P2 O6 Cu2 130.9(2) . 2_667 ?
P2 O4 Cu1 135.7(2) . . ?
O7 C1 C2 110.9(4) . . ?
O7 C1 P2 108.8(3) . . ?
C2 C1 P2 111.9(4) . . ?
O7 C1 P1 105.0(3) . . ?
C2 C1 P1 112.5(3) . . ?
P2 C1 P1 107.4(2) . . ?
C6 C7 C7 106.7(11) . 2_566 ?
C7 C6 N2 111.3(10) . . ?
N2 N2 C6 150.6(12) 2_666 . ?
C5 C3 C4 92.1(13) 2_566 . ?
C5 C3 N1 113.0(9) 2_566 . ?
C4 C3 N1 115.0(8) . . ?
C5 C4 C3 114.1(13) . . ?
C3 C5 C4 114.7(15) 2_566 . ?
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 1.935(4) 2_678 ?
Cu1 O1 1.935(4) . ?
Cu1 O4 1.961(4) . ?
Cu1 O4 1.961(4) 2_678 ?
Cu2 O6 1.925(3) 2_667 ?
Cu2 O2 1.930(3) . ?
Cu2 O3 1.949(4) 2_677 ?
Cu2 O5 2.008(4) . ?
P1 O2 1.520(4) . ?
P1 O1 1.521(4) . ?
P1 O3 1.534(4) . ?
P1 C1 1.841(5) . ?
P2 O4 1.512(4) . ?
P2 O6 1.534(4) . ?
P2 O5 1.544(4) . ?
P2 C1 1.833(5) . ?
O3 Cu2 1.949(4) 2_677 ?
O6 Cu2 1.925(3) 2_667 ?
O7 C1 1.453(6) . ?
C1 C2 1.533(7) . ?
C7 C6 1.486(10) . ?
C7 C7 1.497(10) 2_566 ?
C6 N2 1.488(11) . ?
N2 N2 1.38(2) 2_666 ?
C3 C5 1.486(11) 2_566 ?
C3 C4 1.503(10) . ?
C3 N1 1.512(9) . ?
C4 C5 1.492(11) . ?
C5 C3 1.486(11) 2_566 ?
