#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:00:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180367 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/36/7203682.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_7203682
loop_
_publ_author_name
'Stock, Norbert'
'Bein, Thomas'
_publ_section_title
;
 High-throughput investigation of metal carboxyarylphosphonate hybrid
 compounds
;
_journal_issue                   13
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1384
_journal_paper_doi               10.1039/b413318h
_journal_volume                  15
_journal_year                    2005
_chemical_formula_moiety         'Cu 2+, 2(HO3PCH2C6H4COOH)-, 2H2 O'
_chemical_formula_sum            'C16 H20 Cu O12 P2'
_chemical_formula_weight         529.80
_chemical_name_common
'Copper di(4-methylene-hydrogenphosphono-benzoic acid)-di-hydrate'
_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-97
_cell_angle_alpha                81.513(16)
_cell_angle_beta                 86.272(16)
_cell_angle_gamma                82.251(15)
_cell_formula_units_Z            1
_cell_length_a                   4.5914(6)
_cell_length_b                   5.9810(8)
_cell_length_c                   17.811(3)
_cell_measurement_temperature    293(2)
_cell_volume                     478.83(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_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  0.0774
_diffrn_reflns_av_sigmaI/netI    0.1498
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4646
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.8988
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             271
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0132(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0395
_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)+(0.0111P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                1234
_reflns_number_total             2127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b413318h.txt
_cod_data_source_block           Cu(HO3PCH2C6H4COOH)2_2H2O
_cod_original_cell_volume        478.82(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203682
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_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 1.5000 0.5000 0.5000 0.0080(2) Uani 1 2 d S . .
P1 P 1.0064(2) 0.34132(15) 0.38554(5) 0.0068(3) Uani 1 1 d . . .
O1 O 0.8153(6) 0.5279(4) 0.42088(14) 0.0089(6) Uani 1 1 d . . .
O2 O 1.2743(5) 0.2304(4) 0.42975(14) 0.0089(6) Uani 1 1 d . . .
O3 O 0.8193(6) 0.1496(5) 0.37354(18) 0.0154(7) Uani 1 1 d . . .
H31 H 0.692(11) 0.169(9) 0.384(3) 0.018 Uiso 1 1 d . . .
O4 O 0.1853(7) 1.0703(5) 0.06959(18) 0.0279(9) Uani 1 1 d . . .
O5 O 0.2040(7) 0.7325(5) 0.02854(18) 0.0261(9) Uani 1 1 d . . .
H51 H 0.123(12) 0.792(9) 0.000(3) 0.031 Uiso 1 1 d . . .
O6 O 1.2689(6) 0.7660(6) 0.4427(2) 0.0151(8) Uani 1 1 d . . .
H61 H 1.295(11) 0.902(8) 0.444(3) 0.018 Uiso 1 1 d . . .
H62 H 1.152(12) 0.759(10) 0.440(3) 0.018 Uiso 1 1 d . . .
C1 C 1.1436(9) 0.4564(6) 0.2930(2) 0.0120(9) Uani 1 1 d . . .
H1B H 1.2659 0.5722 0.2991 0.014 Uiso 1 1 calc R . .
H1A H 1.2685 0.3356 0.2714 0.014 Uiso 1 1 calc R . .
C2 C 0.9113(9) 0.5607(6) 0.2368(2) 0.0121(9) Uani 1 1 d . . .
C3 C 0.8338(9) 0.4371(7) 0.1829(2) 0.0154(9) Uani 1 1 d . . .
H3A H 0.9218 0.2878 0.1826 0.018 Uiso 1 1 calc R . .
C4 C 0.6272(9) 0.5308(6) 0.1292(2) 0.0146(9) Uani 1 1 d . . .
H4A H 0.5774 0.4454 0.0935 0.018 Uiso 1 1 calc R . .
C5 C 0.4963(9) 0.7557(6) 0.1302(2) 0.0125(9) Uani 1 1 d . . .
C6 C 0.5727(9) 0.8803(6) 0.1843(2) 0.0140(9) Uani 1 1 d . . .
H6A H 0.4859 1.0299 0.1846 0.017 Uiso 1 1 calc R . .
C7 C 0.7755(9) 0.7846(6) 0.2375(2) 0.0155(9) Uani 1 1 d . . .
H7A H 0.8221 0.8690 0.2739 0.019 Uiso 1 1 calc R . .
C8 C 0.2808(9) 0.8640(7) 0.0727(2) 0.0156(9) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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(1) 1_655 2_766 ?
O1 Cu1 O6 91.48(11) 1_655 2_866 ?
O1 Cu1 O6 88.52(11) 2_766 2_866 ?
O1 Cu1 O6 88.52(11) 1_655 . ?
O1 Cu1 O6 91.48(11) 2_766 . ?
O6 Cu1 O6 180.00(19) 2_866 . ?
O1 P1 O2 115.37(15) . . ?
O1 P1 O3 110.19(15) . . ?
O2 P1 O3 108.30(15) . . ?
O1 P1 C1 109.26(16) . . ?
O2 P1 C1 106.53(16) . . ?
O3 P1 C1 106.81(18) . . ?
P1 O1 Cu1 128.67(15) . 1_455 ?
C2 C1 P1 115.6(3) . . ?
C3 C2 C7 118.8(3) . . ?
C3 C2 C1 120.5(3) . . ?
C7 C2 C1 120.8(4) . . ?
C2 C3 C4 121.7(3) . . ?
C3 C4 C5 118.7(4) . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 C8 119.7(3) . . ?
C4 C5 C8 120.4(4) . . ?
C7 C6 C5 120.8(3) . . ?
C6 C7 C2 120.2(4) . . ?
O4 C8 O5 124.0(4) . . ?
O4 C8 C5 120.1(4) . . ?
O5 C8 C5 116.0(3) . . ?
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 1.960(2) 1_655 ?
Cu1 O1 1.960(2) 2_766 ?
Cu1 O6 1.976(3) 2_866 ?
Cu1 O6 1.976(3) . ?
P1 O1 1.511(2) . ?
P1 O2 1.525(3) . ?
P1 O3 1.569(4) . ?
P1 C1 1.798(4) . ?
O1 Cu1 1.960(2) 1_455 ?
O4 C8 1.247(5) . ?
O5 C8 1.287(5) . ?
C1 C2 1.518(5) . ?
C2 C3 1.385(6) . ?
C2 C7 1.400(5) . ?
C3 C4 1.395(6) . ?
C4 C5 1.399(5) . ?
C5 C6 1.390(6) . ?
C5 C8 1.486(5) . ?
C6 C7 1.380(6) . ?
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
O3 H31 O2 0.60(5) 2.04(5) 2.643(4) 175(7) 1_455
O5 H51 O4 0.68(5) 1.96(5) 2.621(4) 167(7) 2_575
O6 H61 O2 0.84(5) 1.93(5) 2.756(4) 166(5) 1_565
O6 H62 O1 0.55(6) 2.28(6) 2.754(5) 146(7) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 Cu1 -83.9(2) . . . 1_455 ?
O3 P1 O1 Cu1 39.1(2) . . . 1_455 ?
C1 P1 O1 Cu1 156.1(2) . . . 1_455 ?
O1 P1 C1 C2 -59.1(3) . . . . ?
O2 P1 C1 C2 175.6(3) . . . . ?
O3 P1 C1 C2 60.0(3) . . . . ?
P1 C1 C2 C3 -98.5(4) . . . . ?
P1 C1 C2 C7 82.7(4) . . . . ?
C7 C2 C3 C4 0.7(6) . . . . ?
C1 C2 C3 C4 -178.2(4) . . . . ?
C2 C3 C4 C5 0.1(6) . . . . ?
C3 C4 C5 C6 -0.3(6) . . . . ?
C3 C4 C5 C8 178.4(4) . . . . ?
C4 C5 C6 C7 -0.3(6) . . . . ?
C8 C5 C6 C7 -179.0(4) . . . . ?
C5 C6 C7 C2 1.1(6) . . . . ?
C3 C2 C7 C6 -1.2(6) . . . . ?
C1 C2 C7 C6 177.6(4) . . . . ?
C6 C5 C8 O4 5.2(6) . . . . ?
C4 C5 C8 O4 -173.5(4) . . . . ?
C6 C5 C8 O5 -174.7(4) . . . . ?
C4 C5 C8 O5 6.6(6) . . . . ?
