#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/43/2104367.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_2104367
loop_
_publ_author_name
'Le Bail, A.'
'Bazin, D.'
'Daudon, M.'
'Brochot, A.'
'Robbez-Masson, V.'
'Maisonneuve, V.'
_publ_section_title
;
 Racemic calcium tartrate tetrahydrate [form (II)] in rat urinary
 stones
;
_journal_coeditor_code           KD5029
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              350
_journal_page_last               354
_journal_paper_doi               10.1107/S0108768109013688
_journal_volume                  65
_journal_year                    2009
_chemical_formula_moiety         'C4 H12 Ca1 O10'
_chemical_formula_sum            'C4 H12 Ca O10'
_chemical_formula_weight         260.22
_chemical_name_common            'Calcium tartrate tetrahydrate'
_chemical_name_systematic
;
Calcium tartrate tetrahydrate
;
_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_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.92(4)
_cell_angle_beta                 106.00(5)
_cell_angle_gamma                107.55(3)
_cell_formula_units_Z            2
_cell_length_a                   6.241(2)
_cell_length_b                   8.214(3)
_cell_length_c                   10.411(5)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2
_cell_volume                     480.8(4)
_computing_cell_refinement       Stadi4
_computing_data_collection       'Stadi4 (Stoe, 1998)'
_computing_data_reduction        'XRED32 (Stoe, 1998)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'ENCIFER (Allen et al. (2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'ESPOIR (Le Bail, 2001)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Siemens AED2 diffractometer'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2222
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        15
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.562
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2144
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0647
_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)+(0.0918P)²+1.4964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1874
_reflns_number_gt                1495
_reflns_number_total             2222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            kd5029.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (19 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (19 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C4 H12 Ca1 O10'
_cod_database_code               2104367
_cod_database_fobs_code          2104367
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca Ca1 0.34040(16) 0.19006(12) 0.27379(10) 0.0191(3) Uani d . 1 . .
O O1 0.3163(6) -0.0233(4) 0.0927(3) 0.0232(7) Uani d . 1 . .
O O2 1.1726(6) -0.0267(5) 0.3928(4) 0.0273(8) Uani d . 1 . .
O O3 0.9111(6) 0.0269(4) 0.1676(3) 0.0223(7) Uani d D 1 . .
O O4 0.6207(6) 0.0217(4) 0.3327(3) 0.0217(7) Uani d D 1 . .
O O5 0.9267(7) -0.2925(5) 0.3736(4) 0.0301(8) Uani d . 1 . .
O O6 0.2977(6) -0.2968(5) 0.0343(4) 0.0260(8) Uani d . 1 . .
C C1 0.9834(8) -0.1508(6) 0.3352(5) 0.0186(9) Uani d . 1 . .
C C2 0.3817(8) -0.1506(6) 0.1127(5) 0.0194(9) Uani d . 1 . .
C C3 0.8071(8) -0.1289(6) 0.2081(4) 0.0166(9) Uani d D 1 . .
C C4 0.5809(8) -0.1332(6) 0.2429(5) 0.0182(9) Uani d D 1 . .
O OW1 0.6007(6) 0.3134(5) 0.5045(4) 0.0312(9) Uani d D 1 . .
O OW2 0.1417(6) 0.3464(5) 0.3836(4) 0.0285(8) Uani d D 1 . .
O OW3 0.6889(7) 0.3761(5) 0.2295(4) 0.0296(8) Uani d D 1 . .
O OW4 0.1896(7) 0.3524(5) 0.1016(4) 0.0350(9) Uani d D 1 . .
H H1W1 0.686(12) 0.424(4) 0.540(8) 0.074(10) Uiso d D 1 . .
H H2W1 0.683(12) 0.244(8) 0.498(9) 0.074(10) Uiso d D 1 . .
H H1W2 0.118(13) 0.307(11) 0.458(5) 0.074(10) Uiso d D 1 . .
H H2W2 0.006(9) 0.327(11) 0.317(5) 0.074(10) Uiso d D 1 . .
H H1W3 0.679(15) 0.347(9) 0.143(4) 0.074(10) Uiso d D 1 . .
H H2W3 0.758(13) 0.494(4) 0.255(7) 0.074(10) Uiso d D 1 . .
H H1W4 0.033(5) 0.332(10) 0.068(8) 0.074(10) Uiso d D 1 . .
H H2W4 0.268(11) 0.462(5) 0.095(9) 0.074(10) Uiso d D 1 . .
H HC3 0.781(8) -0.210(5) 0.135(4) 0.036(6) Uiso d D 1 . .
H HC4 0.534(8) -0.210(5) 0.293(4) 0.036(6) Uiso d D 1 . .
H HO4 0.669(8) -0.003(6) 0.414(3) 0.036(6) Uiso d D 1 . .
H HO3 0.822(7) 0.015(6) 0.084(3) 0.036(6) Uiso d D 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ca Ca 0.2030 0.3060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ca1 O2 . 1_455 92.85(14) ?
O1 Ca1 OW1 . . 135.84(13) ?
O2 Ca1 OW1 1_455 . 79.50(14) ?
O1 Ca1 OW3 . . 86.36(14) ?
O2 Ca1 OW3 1_455 . 149.10(13) ?
OW1 Ca1 OW3 . . 79.72(15) ?
O1 Ca1 OW2 . . 148.98(13) ?
O2 Ca1 OW2 1_455 . 80.60(14) ?
OW1 Ca1 OW2 . . 73.07(13) ?
OW3 Ca1 OW2 . . 114.51(14) ?
O1 Ca1 OW4 . . 88.75(14) ?
O2 Ca1 OW4 1_455 . 136.45(13) ?
OW1 Ca1 OW4 . . 126.24(15) ?
OW3 Ca1 OW4 . . 74.44(14) ?
OW2 Ca1 OW4 . . 76.18(15) ?
O1 Ca1 O3 . 1_455 75.02(13) ?
O2 Ca1 O3 1_455 1_455 64.86(12) ?
OW1 Ca1 O3 . 1_455 135.03(14) ?
OW3 Ca1 O3 . 1_455 143.17(13) ?
OW2 Ca1 O3 . 1_455 74.77(13) ?
OW4 Ca1 O3 . 1_455 73.68(13) ?
O1 Ca1 O4 . . 63.86(12) ?
O2 Ca1 O4 1_455 . 73.58(12) ?
OW1 Ca1 O4 . . 72.32(13) ?
OW3 Ca1 O4 . . 78.46(13) ?
OW2 Ca1 O4 . . 139.80(12) ?
OW4 Ca1 O4 . . 142.46(14) ?
O3 Ca1 O4 1_455 . 118.64(12) ?
O5 C1 O2 . . 124.7(4) ?
O5 C1 C3 . . 116.9(4) ?
O2 C1 C3 . . 118.5(4) ?
O1 C2 O6 . . 125.9(4) ?
O1 C2 C4 . . 118.6(4) ?
O6 C2 C4 . . 115.5(4) ?
O3 C3 C1 . . 109.6(4) ?
O3 C3 C4 . . 112.6(4) ?
C1 C3 C4 . . 107.7(4) ?
O3 C3 HC3 . . 102(3) ?
C1 C3 HC3 . . 111(3) ?
C4 C3 HC3 . . 114(3) ?
O4 C4 C2 . . 108.7(4) ?
O4 C4 C3 . . 111.0(4) ?
C2 C4 C3 . . 109.7(4) ?
O4 C4 HC4 . . 99(3) ?
C2 C4 HC4 . . 112(3) ?
C3 C4 HC4 . . 116(3) ?
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
Ca1 O1 . 2.401(4) y
Ca1 O2 1_455 2.403(4) y
Ca1 OW1 . 2.424(4) y
Ca1 OW3 . 2.439(4) y
Ca1 OW2 . 2.447(4) y
Ca1 OW4 . 2.472(4) y
Ca1 O3 1_455 2.479(4) y
Ca1 O4 . 2.522(3) y
O1 C2 . 1.245(6) y
O1 O6 . 2.236(5) y
O2 C1 . 1.254(6) y
O2 O5 . 2.213(5) y
O3 C3 . 1.407(6) y
O3 HO3 . 0.87(3) ?
O4 C4 . 1.426(6) y
O4 HO4 . 0.88(3) ?
O5 C1 . 1.245(6) y
O6 C2 . 1.265(6) y
C1 C3 . 1.533(6) y
C2 C4 . 1.527(6) y
C3 C4 . 1.542(6) y
C3 HC3 . 0.91(3) ?
C4 HC4 . 0.88(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
OW1 H1W1 OW2 2_666 0.89(4) 1.84(5) 2.729(6) 178
OW1 H2W1 O4 1_555 0.89(8) 2.26(8) 2.919(5) 131(7)
OW2 H1W2 O5 2_656 0.90(7) 1.86(6) 2.728(6) 163
OW2 H2W2 OW3 1_455 0.89(6) 2.11(6) 2.933(5) 152
OW3 H1W3 O6 2_655 0.89(5) 1.91(5) 2.798(6) 173
OW3 H2W3 O5 1_565 0.91(4) 1.87(5) 2.738(6) 157
OW4 H1W4 O6 2 0.90(5) 1.96(6) 2.853(5) 170
OW4 H2W4 O6 1_565 0.90(5) 2.10(5) 2.947(5) 155
O4 HO4 O2 2_756 0.88(3) 1.94(3) 2.783(5) 160
O3 HO3 O1 2_655 0.87(3) 1.82(3) 2.683(5) 169
