#------------------------------------------------------------------------------
#$Date: 2016-06-20 12:08:03 +0300 (Mon, 20 Jun 2016) $
#$Revision: 183806 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/57/4115722.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_4115722
loop_
_publ_author_name
'Konstantinos D. Demadis'
'John D. Sallis'
'Raphael G. Raptis'
'Peter Baran'
_publ_section_title
;
 A Crystallographically Characterized Nine-Coordinate
 Calcium-Phosphocitrate Complex as Calcification Inhibitor in Vivo
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10129
_journal_page_last               10130
_journal_paper_doi               10.1021/ja016384q
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         {NaCa(phosphocitrate)2(H2O)}n
_chemical_formula_sum            'C12 H17 Ca Na O21 P2'
_chemical_formula_weight         622.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.877(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.331(3)
_cell_length_b                   7.9655(10)
_cell_length_c                   13.2329(16)
_cell_measurement_temperature    301(2)
_cell_volume                     2240.2(5)
_computing_cell_refinement       'BRUKER SMART-NT V5.0'
_computing_data_collection       'BRUKER SMART-NT V5.0'
_computing_data_reduction        'BRUKER SAINT-NT V5/6.0'
_computing_molecular_graphics    'BRUKER SHELXTL-NT V5.1'
_computing_publication_material  'BRUKER SHELXTL-NT V5.1'
_computing_structure_refinement  'BRUKER SHELXTL-NT V5.1'
_computing_structure_solution    'BRUKER SHELXTL-NT V5.1'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS SMART CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4751
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0277
_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)+(0.0471P)²+2.3511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                1478
_reflns_number_total             1612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016384q_s2.cif
_cod_data_source_block           rgr018
_cod_original_formula_sum        'C6 H8.50 Ca0.50 Na0.50 O10.50 P'
_cod_database_code               4115722
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ca1 Ca 0.5000 0.13634(7) 0.7500 0.02180(19) Uani 1 2 d S
Na1 Na 0.5000 0.5000 0.5000 0.0377(3) Uani 1 2 d S
P1 P 0.58714(2) 0.17130(7) 0.59306(4) 0.01857(18) Uani 1 1 d .
O1 O 0.57993(8) 0.6442(2) 0.63920(16) 0.0451(5) Uani 1 1 d .
O2 O 0.67432(8) 0.7671(2) 0.68887(18) 0.0517(5) Uani 1 1 d .
H2O H 0.6543 0.8487 0.6587 0.078 Uiso 1 1 calc R
O3 O 0.60159(7) 0.0605(2) 0.87648(13) 0.0399(4) Uani 1 1 d .
O4 O 0.70027(7) 0.0298(2) 0.97835(13) 0.0398(4) Uani 1 1 d .
H4O H 0.6837 -0.0178 1.0178 0.060 Uiso 1 1 calc R
O5 O 0.55247(7) 0.3998(2) 0.85437(12) 0.0295(4) Uani 1 1 d .
O6 O 0.63600(8) 0.5713(2) 0.89903(14) 0.0394(4) Uani 1 1 d .
H6O H 0.6169 0.6171 0.9354 0.059 Uiso 1 1 calc R
O7 O 0.58595(6) 0.27298(17) 0.69855(10) 0.0204(3) Uani 1 1 d .
O8 O 0.52952(7) 0.06103(19) 0.58597(11) 0.0279(4) Uani 1 1 d .
H8O H 0.5000 0.0000 0.5000 0.033 Uiso 1 2 d SR
O9 O 0.64812(7) 0.07804(18) 0.61588(11) 0.0271(4) Uani 1 1 d .
O10 O 0.57416(7) 0.2951(2) 0.50379(11) 0.0302(4) Uani 1 1 d .
O11 O 0.5000 -0.1635(3) 0.7500 0.0465(7) Uani 1 2 d S
H1W H 0.5016 -0.2359 0.6995 0.056 Uiso 1 1 d R
C1 C 0.63617(11) 0.6377(3) 0.67949(18) 0.0279(5) Uani 1 1 d .
C2 C 0.67222(10) 0.4817(3) 0.72727(17) 0.0239(5) Uani 1 1 d .
H2A H 0.7103 0.5155 0.7819 0.029 Uiso 1 1 calc R
H2B H 0.6847 0.4239 0.6725 0.029 Uiso 1 1 calc R
C3 C 0.63635(10) 0.3577(2) 0.77611(16) 0.0202(5) Uani 1 1 d .
C4 C 0.68364(10) 0.2308(3) 0.84384(16) 0.0231(5) Uani 1 1 d .
H4A H 0.7041 0.1741 0.7984 0.028 Uiso 1 1 calc R
H4B H 0.7158 0.2922 0.8970 0.028 Uiso 1 1 calc R
C5 C 0.65666(10) 0.0997(3) 0.89933(17) 0.0252(5) Uani 1 1 d .
C6 C 0.60285(10) 0.4474(3) 0.84719(16) 0.0229(5) 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
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
Ca Ca 0.2262 0.3064 '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
O11 Ca1 O3 75.71(4) . 2_656
O11 Ca1 O3 75.71(4) . .
O3 Ca1 O3 151.41(8) 2_656 .
O11 Ca1 O7 116.07(3) . .
O3 Ca1 O7 123.69(5) 2_656 .
O3 Ca1 O7 70.26(5) . .
O11 Ca1 O7 116.07(3) . 2_656
O3 Ca1 O7 70.26(5) 2_656 2_656
O3 Ca1 O7 123.69(5) . 2_656
O7 Ca1 O7 127.86(7) . 2_656
O11 Ca1 O8 76.27(4) . 2_656
O3 Ca1 O8 95.59(6) 2_656 2_656
O3 Ca1 O8 77.60(5) . 2_656
O7 Ca1 O8 140.26(5) . 2_656
O7 Ca1 O8 55.92(4) 2_656 2_656
O11 Ca1 O8 76.27(4) . .
O3 Ca1 O8 77.60(5) 2_656 .
O3 Ca1 O8 95.59(6) . .
O7 Ca1 O8 55.92(4) . .
O7 Ca1 O8 140.26(5) 2_656 .
O8 Ca1 O8 152.53(7) 2_656 .
O11 Ca1 O5 144.22(4) . .
O3 Ca1 O5 137.62(6) 2_656 .
O3 Ca1 O5 70.24(6) . .
O7 Ca1 O5 61.84(5) . .
O7 Ca1 O5 76.05(5) 2_656 .
O8 Ca1 O5 85.91(5) 2_656 .
O8 Ca1 O5 117.16(5) . .
O11 Ca1 O5 144.22(4) . 2_656
O3 Ca1 O5 70.24(6) 2_656 2_656
O3 Ca1 O5 137.62(6) . 2_656
O7 Ca1 O5 76.05(5) . 2_656
O7 Ca1 O5 61.84(5) 2_656 2_656
O8 Ca1 O5 117.16(5) 2_656 2_656
O8 Ca1 O5 85.91(5) . 2_656
O5 Ca1 O5 71.56(7) . 2_656
O11 Ca1 P1 94.893(14) . 2_656
O3 Ca1 P1 81.23(4) 2_656 2_656
O3 Ca1 P1 101.22(4) . 2_656
O7 Ca1 P1 143.22(4) . 2_656
O7 Ca1 P1 28.85(3) 2_656 2_656
O8 Ca1 P1 27.15(3) 2_656 2_656
O8 Ca1 P1 158.49(3) . 2_656
O5 Ca1 P1 81.48(4) . 2_656
O5 Ca1 P1 90.56(4) 2_656 2_656
O11 Ca1 P1 94.893(14) . .
O3 Ca1 P1 101.22(4) 2_656 .
O3 Ca1 P1 81.23(4) . .
O7 Ca1 P1 28.85(3) . .
O7 Ca1 P1 143.22(4) 2_656 .
O8 Ca1 P1 158.49(3) 2_656 .
O8 Ca1 P1 27.15(3) . .
O5 Ca1 P1 90.56(4) . .
O5 Ca1 P1 81.48(4) 2_656 .
P1 Ca1 P1 170.21(3) 2_656 .
O10 Na1 O10 180.00(7) . 5_666
O10 Na1 O1 87.86(6) . .
O10 Na1 O1 92.14(6) 5_666 .
O10 Na1 O1 92.14(6) . 5_666
O10 Na1 O1 87.86(6) 5_666 5_666
O1 Na1 O1 180.0 . 5_666
O10 Na1 O5 104.09(5) . 2_656
O10 Na1 O5 75.91(5) 5_666 2_656
O1 Na1 O5 88.69(6) . 2_656
O1 Na1 O5 91.31(6) 5_666 2_656
O10 Na1 O5 75.91(5) . 6_565
O10 Na1 O5 104.09(5) 5_666 6_565
O1 Na1 O5 91.31(6) . 6_565
O1 Na1 O5 88.69(6) 5_666 6_565
O5 Na1 O5 180.0 2_656 6_565
O10 Na1 P1 155.79(4) . 5_666
O10 Na1 P1 24.21(4) 5_666 5_666
O1 Na1 P1 96.95(4) . 5_666
O1 Na1 P1 83.05(4) 5_666 5_666
O5 Na1 P1 99.74(3) 2_656 5_666
O5 Na1 P1 80.26(3) 6_565 5_666
O10 Na1 P1 24.21(4) . .
O10 Na1 P1 155.79(4) 5_666 .
O1 Na1 P1 83.05(4) . .
O1 Na1 P1 96.95(4) 5_666 .
O5 Na1 P1 80.26(3) 2_656 .
O5 Na1 P1 99.74(3) 6_565 .
P1 Na1 P1 180.0 5_666 .
O10 P1 O9 115.43(9) . .
O10 P1 O8 111.88(9) . .
O9 P1 O8 114.90(9) . .
O10 P1 O7 107.45(8) . .
O9 P1 O7 109.17(8) . .
O8 P1 O7 95.93(8) . .
O10 P1 Ca1 123.31(6) . .
O9 P1 Ca1 120.79(6) . .
O8 P1 Ca1 48.60(5) . .
O7 P1 Ca1 47.50(5) . .
O10 P1 Na1 39.34(6) . .
O9 P1 Na1 150.70(6) . .
O8 P1 Na1 92.54(6) . .
O7 P1 Na1 76.05(5) . .
Ca1 P1 Na1 84.595(16) . .
C1 O1 Na1 137.68(16) . .
C5 O3 Ca1 139.73(15) . .
C6 O5 Ca1 119.26(13) . .
C6 O5 Na1 125.75(13) . 2_656
Ca1 O5 Na1 113.66(5) . 2_656
C3 O7 P1 129.28(13) . .
C3 O7 Ca1 120.87(11) . .
P1 O7 Ca1 103.65(6) . .
P1 O8 Ca1 104.25(7) . .
P1 O10 Na1 116.45(8) . .
O1 C1 O2 124.3(2) . .
O1 C1 C2 124.8(2) . .
O2 C1 C2 110.96(19) . .
C1 C2 C3 115.22(18) . .
O7 C3 C2 113.41(17) . .
O7 C3 C4 110.79(16) . .
C2 C3 C4 108.39(17) . .
O7 C3 C6 103.44(16) . .
C2 C3 C6 111.83(16) . .
C4 C3 C6 108.89(17) . .
C5 C4 C3 115.77(17) . .
O3 C5 O4 122.4(2) . .
O3 C5 C4 125.7(2) . .
O4 C5 C4 111.86(18) . .
O5 C6 O6 125.9(2) . .
O5 C6 C3 122.34(18) . .
O6 C6 C3 111.68(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O11 2.388(2) .
Ca1 O3 2.4456(16) 2_656
Ca1 O3 2.4456(16) .
Ca1 O7 2.4768(14) .
Ca1 O7 2.4768(14) 2_656
Ca1 O8 2.5266(15) 2_656
Ca1 O8 2.5266(15) .
Ca1 O5 2.5864(16) .
Ca1 O5 2.5864(15) 2_656
Ca1 P1 3.2648(6) 2_656
Ca1 P1 3.2648(6) .
Na1 O10 2.3146(15) .
Na1 O10 2.3146(15) 5_666
Na1 O1 2.4250(17) .
Na1 O1 2.4250(17) 5_666
Na1 O5 2.6665(15) 2_656
Na1 O5 2.6665(15) 6_565
Na1 P1 3.2692(6) 5_666
Na1 P1 3.2692(6) .
P1 O10 1.4974(15) .
P1 O9 1.4982(15) .
P1 O8 1.5370(15) .
P1 O7 1.6212(14) .
O1 C1 1.205(3) .
O2 C1 1.319(3) .
O3 C5 1.214(3) .
O4 C5 1.314(3) .
O5 C6 1.218(3) .
O5 Na1 2.6665(15) 2_656
O6 C6 1.297(3) .
O7 C3 1.437(2) .
C1 C2 1.509(3) .
C2 C3 1.534(3) .
C3 C4 1.536(3) .
C3 C6 1.545(3) .
C4 C5 1.504(3) .
