#------------------------------------------------------------------------------
#$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006516.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006516
loop_
_publ_author_name
'Jerzykiewicz, L. B.'
'Lis, T.'
_publ_section_title
;
 Calcium <small>D</small>-3-Phosphoglycerate Tetrahydrate at 85K
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1249
_journal_page_last               1251
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'Ca 2+, (C3 H5 O7 P1) 2-, 4H2 O'
_chemical_formula_sum            'C3 H13 Ca O11 P'
_chemical_formula_weight         296.18
_chemical_name_systematic
;
calcium D-3-phoshoglycerate tetrahydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 102.76(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.751(2)
_cell_length_b                   7.718(3)
_cell_length_c                   12.469(4)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     539.8(3)
_computing_cell_refinement       'Kuma KM4 Software'
_computing_data_collection       'Kuma KM4 Software (Kuma Diffraction, 1989)'
_computing_data_reduction        'Kuma KM4 Software'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_measurement_device
'Kuma KM4 computer-controlled four-circle \w/2\q diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4382
_diffrn_reflns_theta_max         32.5
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        2.3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.822(2)
_exptl_crystal_density_meas      '1.808 at room temperature'
_exptl_crystal_density_method
'flotation in C~2~H~5~I/CCl~4~   at room temperature'
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.35
_refine_ls_abs_structure_details 'based on known stereochemistry at C(3)'
_refine_ls_abs_structure_Flack   '-0.03(2) (Flack, 1983)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_obs          0.0227
_refine_ls_shift/esd_max         -0.283
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0304P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0567
_refine_ls_wR_factor_obs         0.0550
_reflns_number_observed          3674
_reflns_number_total             3910
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    mu1266.cif
_[local]_cod_data_source_block   I
_cod_original_cell_volume        539.8(4)
_cod_database_code               2006516
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ca 0.00483(8) 0.00562(9) 0.00649(9) 0.00059(8) 0.00141(6) 0.00010(8)
P 0.00603(12) 0.00491(11) 0.00701(12) 0.00025(10) 0.00114(9) -0.00029(10)
O(31) 0.0121(4) 0.0097(4) 0.0073(4) -0.0029(4) 0.0018(3) 0.0000(4)
O(32) 0.0060(4) 0.0091(5) 0.0168(5) 0.0002(3) 0.0006(4) -0.0034(4)
O(33) 0.0097(4) 0.0063(4) 0.0167(5) 0.0028(4) 0.0029(4) -0.0003(4)
O(3) 0.0126(4) 0.0078(4) 0.0059(4) -0.0020(4) 0.0027(3) -0.0002(3)
O(2) 0.0056(4) 0.0117(5) 0.0113(4) -0.0028(4) 0.0040(3) -0.0040(4)
O(1) 0.0072(4) 0.0093(4) 0.0103(4) 0.0013(4) 0.0018(3) -0.0036(4)
O(11) 0.0050(4) 0.0145(5) 0.0105(4) -0.0013(4) 0.0020(3) -0.0035(4)
O(4) 0.0107(4) 0.0084(4) 0.0087(4) 0.0002(4) 0.0040(4) -0.0005(4)
O(5) 0.0066(4) 0.0084(4) 0.0089(4) 0.0009(3) 0.0025(3) 0.0000(3)
O(6) 0.0080(4) 0.0088(4) 0.0151(5) 0.0010(4) 0.0021(4) -0.0020(4)
O(7) 0.0124(5) 0.0150(5) 0.0142(5) 0.0038(4) -0.0035(4) -0.0059(4)
C(1) 0.0067(5) 0.0069(5) 0.0067(5) 0.0008(4) 0.0025(4) 0.0010(4)
C(2) 0.0056(5) 0.0074(5) 0.0061(5) -0.0011(3) 0.0020(4) -0.0008(4)
C(3) 0.0116(5) 0.0071(5) 0.0067(5) 0.0008(4) 0.0025(4) -0.0009(4)
loop_
_atom_site_label
_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_calc_flag
_atom_site_occupancy
Ca 0.24959(4) 0.5 0.22274(2) 0.00562(5) Uani d 1
P 0.50170(5) 1.06060(5) 0.19242(2) 0.00603(6) Uani d 1
O(31) 0.42671(16) 0.99230(16) 0.07690(7) 0.0097(2) Uani d 1
O(32) 0.78241(16) 1.04494(14) 0.23198(8) 0.0109(2) Uani d 1
O(33) 0.42544(17) 1.23728(13) 0.21806(9) 0.0109(2) Uani d 1
O(3) 0.40082(17) 0.91625(12) 0.26249(7) 0.0087(2) Uani d 1
O(2) 0.24489(17) 0.66059(13) 0.39009(8) 0.0092(2) Uani d 1
O(11) 0.63600(16) 0.55679(15) 0.34483(8) 0.0090(2) Uani d 1
O(1) 0.86420(16) 0.73498(13) 0.46652(8) 0.0100(2) Uani d 1
O(4) 0.45310(17) 0.63459(13) 0.09718(8) 0.0090(2) Uani d 1
O(5) -0.01440(16) 0.33976(13) 0.32005(8) 0.0078(2) Uani d 1
O(6) -0.06097(17) 0.71108(14) 0.15874(8) 0.0107(2) Uani d 1
O(7) 0.00134(19) 0.38182(15) 0.05749(9) 0.0149(2) Uani d 1
C(1) 0.6660(3) 0.67847(16) 0.41396(9) 0.0066(2) Uani d 1
C(2) 0.4422(2) 0.76843(16) 0.43376(9) 0.0063(2) Uani d 1
C(3) 0.4210(3) 0.94490(17) 0.37819(10) 0.0084(2) Uani d 1
H(2) 0.460(4) 0.788(3) 0.5117(16) 0.003(4) Uiso d 1
H(3) 0.283(4) 1.001(4) 0.3910(18) 0.019(6) Uiso d 1
H(3') 0.568(4) 1.011(4) 0.4124(16) 0.010(5) Uiso d 1
H(20) 0.138(6) 0.693(4) 0.416(3) 0.035(8) Uiso d 1
H(32) 0.860(5) 1.137(4) 0.256(3) 0.022(6) Uiso d 1
H(4) 0.462(5) 0.587(4) 0.036(3) 0.032(8) Uiso d 1
H(41) 0.424(6) 0.745(5) 0.095(3) 0.042(9) Uiso d 1
H(5) 0.055(5) 0.326(4) 0.392(3) 0.026(7) Uiso d 1
H(51) -0.109(5) 0.416(4) 0.333(3) 0.028(7) Uiso d 1
H(6) -0.205(6) 0.680(5) 0.144(3) 0.040(8) Uiso d 1
H(61) -0.055(5) 0.796(4) 0.192(3) 0.022(6) Uiso d 1
H(7) -0.116(6) 0.421(5) 0.018(3) 0.043(9) Uiso d 1
H(71) 0.059(6) 0.310(5) 0.019(3) 0.037(8) Uiso d 1
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'
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_site_symmetry_1
_geom_angle
_geom_angle_publ_flag
O(31) P O(32) . 109.20(10) yes
O(31) P O(33) . 119.40(10) yes
O(32) P O(33) . 109.30(10) yes
O(31) P O(3) . 102.50(10) yes
O(32) P O(3) . 104.10(10) yes
O(33) P O(3) . 111.10(10) yes
C(3) O(3) P . 118.80(10) yes
O(3) C(3) C(2) . 107.50(10) yes
O(2) C(2) C(3) . 112.00(10) yes
C(3) C(2) C(1) . 108.60(10) yes
O(2) C(2) C(1) . 107.60(10) yes
O(1) C(1) C(2) . 117.1(2) yes
O(11) C(1) C(2) . 117.1(2) yes
O(11) C(1) O(1) . 125.8(2) yes
C(2) O(2) Ca . 118.00(10) ?
C(1) O(11) Ca . 121.90(10) ?
O(33) Ca O(4) 1_545 94.90(10) ?
O(33) Ca O(7) 1_545 79.80(10) ?
O(4) Ca O(7) . 83.60(10) ?
O(33) Ca O(6) 1_545 153.20(10) ?
O(4) Ca O(6) . 85.60(10) ?
O(7) Ca O(6) . 73.60(10) ?
O(33) Ca O(2) 1_545 124.50(10) ?
O(4) Ca O(2) . 116.10(10) ?
O(7) Ca O(2) . 144.00(10) ?
O(6) Ca O(2) . 78.00(10) ?
O(33) Ca O(11) 1_545 80.10(10) ?
O(4) Ca O(11) . 79.70(10) ?
O(7) Ca O(11) . 152.50(10) ?
O(6) Ca O(11) . 126.10(10) ?
O(2) Ca O(11) . 63.50(10) ?
O(33) Ca O(5) 1_545 83.80(10) ?
O(4) Ca O(5) . 168.90(10) ?
O(7) Ca O(5) . 85.30(10) ?
O(6) Ca O(5) . 90.60(10) ?
O(2) Ca O(5) . 73.10(10) ?
O(11) Ca O(5) . 110.90(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
P O(31) . 1.505(2) yes
P O(32) . 1.585(2) yes
P O(33) . 1.489(2) yes
P O(3) . 1.6020(10) yes
O(3) C(3) . 1.439(2) yes
O(2) C(2) . 1.416(2) yes
O(1) C(1) . 1.261(2) yes
O(11) C(1) . 1.261(2) yes
C(1) C(2) . 1.530(2) yes
C(2) C(3) . 1.521(2) yes
Ca O(2) . 2.432(2) yes
Ca O(11) . 2.440(2) yes
Ca O(33) 1_545 2.272(2) yes
Ca O(4) . 2.389(2) yes
Ca O(5) . 2.474(2) yes
Ca O(6) . 2.419(2) yes
Ca O(7) . 2.412(2) yes
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_publ_flag
C(3) O(3) P O(31) -174.70(10) yes
C(3) O(3) P O(32) 71.60(10) yes
C(3) O(3) P O(33) -46.00(10) yes
P O(3) C(3) C(2) -150.10(10) yes
O(2) C(2) C(3) O(3) -58.0(2) yes
O(11) C(1) C(2) O(2) 15.9(2) yes
O(1) C(1) C(2) O(2) -165.5(2) yes
O(1) C(1) C(2) C(3) 73.1(2) yes
O(11) C(1) C(2) C(3) -105.5(2) yes
C(1) C(2) C(3) O(3) 60.7(2) yes