#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:44:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180353 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/22/7202288.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_7202288
loop_
_publ_author_name
'Samanamu, Christian R.'
'Zamora, Elena N.'
'Lesikar, Leslie A.'
'Montchamp, Jean-Luc'
'Richards, Anne F.'
_publ_section_title
;
 5-Pyrimidyl phosphonic acid as a building block for the synthesis of
 coordination polymers
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1372
_journal_paper_doi               10.1039/b809504n
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C10 H20 Cu2 F6 N4 O18 P2 S2'
_chemical_formula_weight         851.44
_chemical_name_common            (((PymPO3(H))2Cu2(H2O)4)(SO3CF3)2.H2O)n
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.025(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9181(15)
_cell_length_b                   11.6269(13)
_cell_length_c                   18.8112(16)
_cell_measurement_reflns_used    5133
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.2825
_cell_measurement_theta_min      2.3345
_cell_volume                     2735.4(5)
_computing_cell_refinement       'Bruker SAINT+ v. 6.36a'
_computing_data_collection       'Bruker SMART v. 5.626'
_computing_data_reduction        'Bruker SAINT+ v. 6.36a'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 6.12'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 6.12'
_computing_structure_solution    'XS, Bruker SHELXTL v. 6.12'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15631
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        <0.01
_exptl_absorpt_coefficient_mu    1.951
_exptl_absorpt_correction_T_max  0.9676
_exptl_absorpt_correction_T_min  0.9438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS: SAINT+, 2001'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6462
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0394P)²+2.0698P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                5004
_reflns_number_total             6462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809504n.txt
_cod_data_source_block           c:\pympox~1\pympoc~1\ar476xx
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to 'constr'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7202288
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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 0.23613(3) 0.07326(3) 0.48680(2) 0.01158(9) Uani 1 1 d . . .
Cu2 Cu 0.23860(3) 0.57023(3) 0.49833(2) 0.01126(9) Uani 1 1 d . . .
S2 S 0.12619(6) 0.73637(6) 0.62738(4) 0.01638(16) Uani 1 1 d . . .
P1 P 0.00311(6) 0.68963(6) 0.37363(4) 0.01011(15) Uani 1 1 d . . .
P2 P 0.53174(6) 0.80335(6) 0.41547(4) 0.01177(15) Uani 1 1 d . . .
F4 F 0.1433(2) 0.8013(3) 0.76387(16) 0.0727(9) Uani 1 1 d . . .
F5 F 0.29041(18) 0.8097(2) 0.75305(13) 0.0522(7) Uani 1 1 d . . .
F6 F 0.2269(2) 0.6467(3) 0.76674(14) 0.0682(8) Uani 1 1 d . . .
O1 O 0.09592(15) 0.61726(17) 0.42601(12) 0.0155(4) Uani 1 1 d . . .
O2 O 0.02080(16) 0.81335(16) 0.36126(12) 0.0157(4) Uani 1 1 d . . .
O3 O -0.05588(16) 0.62710(18) 0.29166(12) 0.0176(4) Uani 1 1 d D . .
O4 O 0.25390(17) 0.48908(18) 0.39043(13) 0.0219(5) Uani 1 1 d D . .
O5 O 0.38394(16) 0.52603(17) 0.57108(13) 0.0213(5) Uani 1 1 d D . .
H5B H 0.4021 0.4554 0.5792 0.026 Uiso 1 1 d RD . .
O6 O 0.62189(15) 0.86454(18) 0.48185(13) 0.0192(5) Uani 1 1 d . . .
O7 O 0.49270(19) 0.87921(19) 0.33961(13) 0.0265(5) Uani 1 1 d D . .
O8 O 0.54828(16) 0.68157(17) 0.40199(13) 0.0185(5) Uani 1 1 d . . .
O9 O 0.20360(19) 0.1685(2) 0.36842(13) 0.0283(5) Uani 1 1 d D . .
H9B H 0.1572 0.1606 0.3188 0.034 Uiso 1 1 d RD . .
O10 O 0.08639(15) 0.01222(17) 0.43950(13) 0.0204(5) Uani 1 1 d D . .
O11 O 0.26942(18) -0.00344(18) 0.60852(13) 0.0240(5) Uani 1 1 d D . .
O15 O 0.09962(18) 0.8540(2) 0.60074(16) 0.0330(6) Uani 1 1 d . . .
O16 O 0.03478(17) 0.66700(19) 0.61682(13) 0.0247(5) Uani 1 1 d . . .
O17 O 0.20029(19) 0.68339(19) 0.60322(14) 0.0277(5) Uani 1 1 d . . .
N1 N 0.18271(18) 0.42198(19) 0.52400(13) 0.0118(5) Uani 1 1 d . . .
N3 N 0.30057(18) 0.7186(2) 0.48138(14) 0.0126(5) Uani 1 1 d . . .
N4 N 0.29209(18) 0.92031(19) 0.46598(13) 0.0111(5) Uani 1 1 d . . .
N5 N 0.18309(18) 0.2186(2) 0.51954(14) 0.0119(5) Uani 1 1 d . . .
C1 C 0.1217(2) 0.4183(2) 0.56274(16) 0.0131(6) Uani 1 1 d . . .
H1 H 0.1006 0.4877 0.5773 0.016 Uiso 1 1 calc R . .
C2 C -0.0888(2) 0.6849(2) 0.41794(16) 0.0111(5) Uani 1 1 d . . .
C3 C 0.2103(2) 0.3215(2) 0.50367(17) 0.0123(6) Uani 1 1 d . . .
H3 H 0.2523 0.3239 0.4759 0.015 Uiso 1 1 calc R . .
C4 C 0.3815(2) 0.7147(2) 0.46048(17) 0.0138(6) Uani 1 1 d . . .
H4 H 0.4124 0.6433 0.4593 0.017 Uiso 1 1 calc R . .
C5 C 0.2601(2) 0.8213(2) 0.48400(17) 0.0122(5) Uani 1 1 d . . .
H5 H 0.2047 0.8241 0.4998 0.015 Uiso 1 1 calc R . .
C6 C 0.3717(2) 0.9159(2) 0.44375(16) 0.0109(5) Uani 1 1 d . . .
H6 H 0.3950 0.9845 0.4299 0.013 Uiso 1 1 calc R . .
C7 C -0.1230(2) 0.7842(2) 0.44052(16) 0.0123(6) Uani 1 1 d . . .
H7 H -0.1037 0.8559 0.4276 0.015 Uiso 1 1 calc R . .
C8 C 0.4203(2) 0.8131(2) 0.44068(16) 0.0115(5) Uani 1 1 d . . .
C10 C 0.2011(3) 0.7489(4) 0.7339(2) 0.0343(9) Uani 1 1 d . . .
S1 S 0.39745(6) 0.29464(7) 0.29264(5) 0.02049(17) Uani 1 1 d . . .
F1 F 0.4632(2) 0.1080(2) 0.24977(14) 0.0510(7) Uani 1 1 d . . .
F2 F 0.33938(18) 0.08103(18) 0.28673(15) 0.0466(6) Uani 1 1 d . . .
F3 F 0.49913(18) 0.11683(19) 0.37285(12) 0.0421(6) Uani 1 1 d . . .
O12 O 0.3760(2) 0.3158(2) 0.35966(15) 0.0313(6) Uani 1 1 d . . .
O13 O 0.49776(19) 0.3441(2) 0.30011(13) 0.0287(5) Uani 1 1 d . . .
O14 O 0.3102(2) 0.3101(2) 0.21632(16) 0.0407(7) Uani 1 1 d . . .
C9 C 0.4269(3) 0.1409(3) 0.29989(19) 0.0245(7) Uani 1 1 d . . .
O18 O 0.03738(16) 0.43320(17) 0.28048(12) 0.0219(5) Uani 1 1 d D . .
H3A H -0.0282 0.5625 0.2934 0.038(11) Uiso 1 1 d RD . .
H18B H 0.0176 0.3954 0.2377 0.043(12) Uiso 1 1 d RD . .
H18A H 0.0119 0.3812 0.3014 0.055(14) Uiso 1 1 d RD . .
H9A H 0.2658 0.1981 0.3783 0.09(2) Uiso 1 1 d RD . .
H10B H 0.0672 -0.0499 0.4105 0.034(11) Uiso 1 1 d RD . .
H10A H 0.0286 0.0498 0.4266 0.047(12) Uiso 1 1 d RD . .
H11B H 0.2198 -0.0441 0.6193 0.046(12) Uiso 1 1 d RD . .
H11A H 0.2939 0.0400 0.6525 0.075(16) Uiso 1 1 d RD . .
H4A H 0.1906 0.4728 0.3503 0.068(15) Uiso 1 1 d RD . .
H4B H 0.2852 0.4427 0.3695 0.055(13) Uiso 1 1 d RD . .
H5A H 0.4183 0.5732 0.6162 0.084(18) Uiso 1 1 d RD . .
H7A H 0.5153 0.8578 0.3091 0.073(17) Uiso 1 1 d RD . .
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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
O6 Cu1 O10 172.35(9) 3_666 . ?
O6 Cu1 N5 93.13(9) 3_666 . ?
O10 Cu1 N5 89.07(9) . . ?
O6 Cu1 N4 87.68(9) 3_666 1_545 ?
O10 Cu1 N4 90.93(8) . 1_545 ?
N5 Cu1 N4 173.62(9) . 1_545 ?
O6 Cu1 O11 96.22(8) 3_666 . ?
O10 Cu1 O11 91.18(8) . . ?
N5 Cu1 O11 87.84(9) . . ?
N4 Cu1 O11 85.78(8) 1_545 . ?
O6 Cu1 O9 81.89(9) 3_666 . ?
O10 Cu1 O9 90.91(9) . . ?
N5 Cu1 O9 87.18(9) . . ?
N4 Cu1 O9 99.20(9) 1_545 . ?
O11 Cu1 O9 174.57(8) . . ?
O1 Cu2 O5 178.73(9) . . ?
O1 Cu2 N3 91.46(9) . . ?
O5 Cu2 N3 87.28(9) . . ?
O1 Cu2 N1 91.43(9) . . ?
O5 Cu2 N1 89.83(9) . . ?
N3 Cu2 N1 175.84(9) . . ?
O1 Cu2 O4 87.70(8) . . ?
O5 Cu2 O4 92.38(8) . . ?
N3 Cu2 O4 89.99(9) . . ?
N1 Cu2 O4 93.11(8) . . ?
O17 S2 O16 115.37(14) . . ?
O17 S2 O15 113.93(14) . . ?
O16 S2 O15 113.83(14) . . ?
O17 S2 C10 103.85(16) . . ?
O16 S2 C10 103.98(15) . . ?
O15 S2 C10 104.04(18) . . ?
O1 P1 O2 119.41(12) . . ?
O1 P1 O3 108.36(11) . . ?
O2 P1 O3 110.07(12) . . ?
O1 P1 C2 105.10(12) . . ?
O2 P1 C2 107.43(12) . . ?
O3 P1 C2 105.51(12) . . ?
O8 P2 O6 117.42(12) . . ?
O8 P2 O7 113.83(13) . . ?
O6 P2 O7 108.72(13) . . ?
O8 P2 C8 108.71(12) . . ?
O6 P2 C8 104.54(12) . . ?
O7 P2 C8 102.09(13) . . ?
P1 O1 Cu2 161.72(14) . . ?
P1 O3 H3A 110.0 . . ?
Cu2 O4 H4A 112.9 . . ?
Cu2 O4 H4B 152.0 . . ?
H4A O4 H4B 89.4 . . ?
Cu2 O5 H5B 120.9 . . ?
Cu2 O5 H5A 115.9 . . ?
H5B O5 H5A 113.9 . . ?
P2 O6 Cu1 142.82(13) . 3_666 ?
P2 O7 H7A 112.9 . . ?
Cu1 O9 H9B 134.9 . . ?
Cu1 O9 H9A 103.0 . . ?
H9B O9 H9A 117.8 . . ?
Cu1 O10 H10B 123.0 . . ?
Cu1 O10 H10A 127.8 . . ?
H10B O10 H10A 104.7 . . ?
Cu1 O11 H11B 124.6 . . ?
Cu1 O11 H11A 121.8 . . ?
H11B O11 H11A 95.9 . . ?
C3 N1 C1 117.2(2) . . ?
C3 N1 Cu2 119.00(18) . . ?
C1 N1 Cu2 123.76(19) . . ?
C5 N3 C4 117.6(2) . . ?
C5 N3 Cu2 123.00(18) . . ?
C4 N3 Cu2 119.23(18) . . ?
C5 N4 C6 117.3(2) . . ?
C5 N4 Cu1 120.32(18) . 1_565 ?
C6 N4 Cu1 121.78(18) . 1_565 ?
C3 N5 C7 117.1(2) . 3_566 ?
C3 N5 Cu1 120.04(18) . . ?
C7 N5 Cu1 122.83(18) 3_566 . ?
N1 C1 C2 122.1(2) . 3_566 ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 3_566 . ?
C7 C2 C1 116.3(2) . 3_566 ?
C7 C2 P1 121.6(2) . . ?
C1 C2 P1 122.0(2) 3_566 . ?
N5 C3 N1 125.2(3) . . ?
N5 C3 H3 117.4 . . ?
N1 C3 H3 117.4 . . ?
N3 C4 C8 121.7(3) . . ?
N3 C4 H4 119.1 . . ?
C8 C4 H4 119.1 . . ?
N3 C5 N4 124.9(3) . . ?
N3 C5 H5 117.5 . . ?
N4 C5 H5 117.5 . . ?
N4 C6 C8 121.9(2) . . ?
N4 C6 H6 119.0 . . ?
C8 C6 H6 119.0 . . ?
N5 C7 C2 122.1(3) 3_566 . ?
N5 C7 H7 118.9 3_566 . ?
C2 C7 H7 118.9 . . ?
C4 C8 C6 116.5(2) . . ?
C4 C8 P2 119.9(2) . . ?
C6 C8 P2 123.6(2) . . ?
F6 C10 F4 108.0(3) . . ?
F6 C10 F5 108.9(3) . . ?
F4 C10 F5 108.1(3) . . ?
F6 C10 S2 110.7(3) . . ?
F4 C10 S2 110.3(3) . . ?
F5 C10 S2 110.9(2) . . ?
O14 S1 O12 116.59(16) . . ?
O14 S1 O13 113.77(15) . . ?
O12 S1 O13 113.97(15) . . ?
O14 S1 C9 105.23(15) . . ?
O12 S1 C9 103.17(14) . . ?
O13 S1 C9 101.81(15) . . ?
F1 C9 F3 109.1(3) . . ?
F1 C9 F2 108.9(3) . . ?
F3 C9 F2 107.3(3) . . ?
F1 C9 S1 112.2(2) . . ?
F3 C9 S1 109.1(2) . . ?
F2 C9 S1 110.0(2) . . ?
H18B O18 H18A 92.4 . . ?
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 O6 1.9373(19) 3_666 ?
Cu1 O10 2.003(2) . ?
Cu1 N5 2.044(2) . ?
Cu1 N4 2.047(2) 1_545 ?
Cu1 O11 2.307(2) . ?
Cu1 O9 2.347(2) . ?
Cu2 O1 1.9294(19) . ?
Cu2 O5 1.949(2) . ?
Cu2 N3 2.015(2) . ?
Cu2 N1 2.035(2) . ?
Cu2 O4 2.331(2) . ?
S2 O17 1.436(2) . ?
S2 O16 1.445(2) . ?
S2 O15 1.447(2) . ?
S2 C10 1.814(4) . ?
P1 O1 1.493(2) . ?
P1 O2 1.495(2) . ?
P1 O3 1.572(2) . ?
P1 C2 1.808(3) . ?
P2 O8 1.474(2) . ?
P2 O6 1.505(2) . ?
P2 O7 1.559(2) . ?
P2 C8 1.814(3) . ?
F4 C10 1.317(4) . ?
F5 C10 1.335(4) . ?
F6 C10 1.314(5) . ?
O3 H3A 0.8379 . ?
O4 H4A 0.8935 . ?
O4 H4B 0.8872 . ?
O5 H5B 0.8527 . ?
O5 H5A 0.9448 . ?
O6 Cu1 1.9373(19) 3_666 ?
O7 H7A 0.8068 . ?
O9 H9B 0.8770 . ?
O9 H9A 0.8725 . ?
O10 H10B 0.8732 . ?
O10 H10A 0.8513 . ?
O11 H11B 0.9299 . ?
O11 H11A 0.8991 . ?
N1 C3 1.337(3) . ?
N1 C1 1.340(3) . ?
N3 C5 1.330(3) . ?
N3 C4 1.346(3) . ?
N4 C5 1.331(3) . ?
N4 C6 1.346(3) . ?
N4 Cu1 2.047(2) 1_565 ?
N5 C3 1.328(3) . ?
N5 C7 1.348(3) 3_566 ?
C1 C2 1.388(4) 3_566 ?
C1 H1 0.9400 . ?
C2 C7 1.386(4) . ?
C2 C1 1.388(4) 3_566 ?
C3 H3 0.9400 . ?
C4 C8 1.384(4) . ?
C4 H4 0.9400 . ?
C5 H5 0.9400 . ?
C6 C8 1.387(4) . ?
C6 H6 0.9400 . ?
C7 N5 1.348(3) 3_566 ?
C7 H7 0.9400 . ?
S1 O14 1.428(3) . ?
S1 O12 1.439(2) . ?
S1 O13 1.459(2) . ?
S1 C9 1.825(3) . ?
F1 C9 1.307(4) . ?
F2 C9 1.329(4) . ?
F3 C9 1.327(4) . ?
O18 H18B 0.8500 . ?
O18 H18A 0.8765 . ?
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
O4 H4B O12 0.89 2.00 2.854(3) 160.3 .
O4 H4A O18 0.89 2.01 2.883(3) 166.5 .
O3 H3A O18 0.84 1.83 2.655(3) 168.1 .
