#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:52:43 +0100 (jue 24 de mar de 2016) $
#$Revision: 179544 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/13/4501371.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_4501371
loop_
_publ_author_name
'Braga, Dario'
'Grepioni, Fabrizia'
'Lampronti, Giulio I.'
'Maini, Lucia'
'Turrina, Alessandro'
_publ_section_title
;
 Ionic Co-crystals of Organic Molecules with Metal Halides: A New Prospect
 in the Solid Formulation of Active Pharmaceutical Ingredients
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5621
_journal_paper_doi               10.1021/cg201177p
_journal_volume                  11
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C4 H17 Ca1 Cl2 N1 O7'
_chemical_formula_sum            'C4 H17 Ca Cl2 N O7'
_chemical_formula_weight         302.17
_chemical_name_systematic
;
diaceamide CaCl2 (H2O)5
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-02-14T15:22:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.815(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8917(5)
_cell_length_b                   7.2632(5)
_cell_length_c                   12.9379(8)
_cell_measurement_reflns_used    1561
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2309
_cell_measurement_theta_min      2.7988
_cell_volume                     723.12(8)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
        (compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
        (compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
        (compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.134
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3488
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.3
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.85937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
        (compiled Aug 27 2010,11:50:40)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2253
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0864P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                1881
_reflns_number_total             2253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201177p_si_001.cif
_cod_data_source_block           diacetamideCaCl2(H2O)5
_cod_database_code               4501371
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_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_type_symbol
Ca1 1.26985(12) 0.25680(15) 0.71958(6) 0.0435(3) Uani d . 1 Ca
Cl2 1.34243(17) 0.2460(3) 1.08227(10) 0.0596(4) Uani d . 1 Cl
Cl3 0.70722(18) 0.2984(3) 0.52107(12) 0.0626(5) Uani d . 1 Cl
C1 0.8464(8) 0.2592(14) 0.9230(5) 0.0726(19) Uani d . 1 C
H1A 0.7738 0.3572 0.9379 0.109 Uiso calc R 1 H
H1B 0.932 0.2298 0.986 0.109 Uiso calc R 1 H
H1C 0.7765 0.1525 0.8997 0.109 Uiso calc R 1 H
C2 0.9342(6) 0.3178(9) 0.8390(4) 0.0447(12) Uani d . 1 C
C3 0.9608(8) 0.5813(8) 0.7232(4) 0.0468(13) Uani d . 1 C
C4 0.8848(10) 0.7639(13) 0.6921(5) 0.083(2) Uani d . 1 C
H4A 0.8024 0.7937 0.7342 0.124 Uiso calc R 1 H
H4B 0.8271 0.7621 0.6185 0.124 Uiso calc R 1 H
H4C 0.9753 0.8549 0.7034 0.124 Uiso calc R 1 H
O1 1.0332(5) 0.2182(6) 0.8063(3) 0.0534(10) Uani d . 1 O
O2 1.0696(5) 0.5139(6) 0.6806(3) 0.0507(10) Uani d . 1 O
N1 0.8989(6) 0.4952(7) 0.8028(4) 0.0486(11) Uani d . 1 N
H1 0.837(7) 0.565(9) 0.845(4) 0.048(15) Uiso d . 1 H
O1X 1.4230(7) 0.4695(8) 0.6351(5) 0.0806(17) Uani d . 1 O
O4X 1.3366(8) 0.0113(10) 0.8454(5) 0.101(2) Uani d . 1 O
O2X 1.4935(8) 0.0762(9) 0.6637(5) 0.0889(18) Uani d . 1 O
O3X 1.3853(8) 0.4350(9) 0.8723(4) 0.088(2) Uani d . 1 O
O5X 1.0861(5) 0.1263(7) 0.5697(3) 0.0673(13) Uani d . 1 O
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
Ca1 0.0446(5) 0.0479(7) 0.0411(4) 0.0099(6) 0.0159(4) 0.0051(6)
Cl2 0.0606(7) 0.0557(9) 0.0672(7) -0.0078(9) 0.0240(6) 0.0124(9)
Cl3 0.0582(8) 0.0586(11) 0.0788(9) -0.0059(8) 0.0319(7) -0.0081(8)
C1 0.076(4) 0.062(4) 0.096(4) 0.019(5) 0.054(3) 0.026(5)
C2 0.041(2) 0.045(3) 0.049(3) 0.001(2) 0.011(2) 0.005(2)
C3 0.059(3) 0.036(3) 0.048(3) 0.008(3) 0.019(2) -0.002(3)
C4 0.107(5) 0.061(5) 0.092(4) 0.028(5) 0.046(4) 0.025(5)
O1 0.052(2) 0.045(3) 0.070(2) 0.012(2) 0.0290(17) 0.005(2)
O2 0.056(2) 0.048(2) 0.056(2) 0.006(2) 0.0280(18) 0.0025(19)
N1 0.059(3) 0.043(3) 0.050(2) 0.009(2) 0.025(2) -0.003(2)
O1X 0.079(3) 0.077(4) 0.102(4) 0.017(3) 0.055(3) 0.029(3)
O4X 0.106(4) 0.105(5) 0.100(4) 0.055(4) 0.042(3) 0.048(4)
O2X 0.089(4) 0.082(4) 0.111(4) 0.034(3) 0.055(3) 0.021(4)
O3X 0.105(4) 0.111(5) 0.049(2) -0.042(4) 0.015(3) -0.005(3)
O5X 0.070(3) 0.077(4) 0.054(2) 0.009(3) 0.0114(19) -0.010(2)
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O5X Ca1 O3X 164.22(19)
O5X Ca1 O1X 99.60(19)
O3X Ca1 O1X 83.5(2)
O5X Ca1 O4X 105.3(2)
O3X Ca1 O4X 81.6(2)
O1X Ca1 O4X 137.8(2)
O5X Ca1 O1 86.38(15)
O3X Ca1 O1 82.49(17)
O1X Ca1 O1 145.15(18)
O4X Ca1 O1 70.80(17)
O5X Ca1 O2 83.38(15)
O3X Ca1 O2 82.25(19)
O1X Ca1 O2 77.18(16)
O4X Ca1 O2 138.55(16)
O1 Ca1 O2 69.40(13)
O5X Ca1 O2X 83.83(19)
O3X Ca1 O2X 111.9(2)
O1X Ca1 O2X 74.75(19)
O4X Ca1 O2X 74.70(19)
O1 Ca1 O2X 140.08(19)
O2 Ca1 O2X 146.62(17)
O1 C2 N1 122.6(5)
O1 C2 C1 122.1(6)
N1 C2 C1 115.3(6)
O2 C3 N1 123.7(5)
O2 C3 C4 121.5(6)
N1 C3 C4 114.9(5)
C2 O1 Ca1 136.5(4)
C3 O2 Ca1 134.9(4)
C2 N1 C3 126.7(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ca1 O5X 2.349(4)
Ca1 O3X 2.369(5)
Ca1 O1X 2.373(5)
Ca1 O4X 2.393(6)
Ca1 O1 2.399(4)
Ca1 O2 2.426(4)
Ca1 O2X 2.434(5)
C1 C2 1.475(7)
C2 O1 1.208(6)
C2 N1 1.378(8)
C3 O2 1.221(6)
C3 N1 1.383(7)
C3 C4 1.475(10)
