#------------------------------------------------------------------------------
#$Date: 2015-05-24 05:47:19 +0300 (Sun, 24 May 2015) $
#$Revision: 137296 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/07/2240763.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_2240763
loop_
_publ_author_name
'Lamberts, Kevin'
'Englert, Ulli'
_publ_section_title
;
 Crystal structures of coordination polymers from CaI₂ and proline
;
_journal_coeditor_code           GK2631
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              675
_journal_page_last               680
_journal_paper_doi               10.1107/S2056989015009597
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ca (C5 H9 N O2)2 (H2 O)2] I2'
_chemical_formula_moiety         'C10 H22 Ca N2 O6 2+, 2(I -)'
_chemical_formula_sum            'C10 H22 Ca I2 N2 O6'
_chemical_formula_weight         560.17
_chemical_name_systematic
;
catena-Poly[[diaquadi-m₂-DL-proline-calcium] diiodide]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                105.757(10)
_cell_angle_beta                 104.501(11)
_cell_angle_gamma                97.911(12)
_cell_formula_units_Z            2
_cell_length_a                   7.958(7)
_cell_length_b                   9.080(8)
_cell_length_c                   13.591(11)
_cell_measurement_reflns_used    1555
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.84
_cell_measurement_theta_min      2.39
_cell_volume                     892.5(13)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2008)
;
_computing_data_collection
;
SMART (Bruker, 2008)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2008)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2008)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Bruker D8 with APEX CCD area detector and Incoatec microsource
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.132
_diffrn_reflns_theta_min         2.390
_exptl_absorpt_coefficient_mu    3.835
_exptl_absorpt_correction_T_max  .7453
_exptl_absorpt_correction_T_min  .4469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.084
_exptl_crystal_description       plate
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.051
_refine_diff_density_min         -2.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3533
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0200P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                2603
_reflns_number_total             3533
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gk2631sup1.cif
_cod_data_source_block           2
_cod_database_code               2240763
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.486
_shelx_estimated_absorpt_t_max   0.831
_shelxl_version_number           20.13
loop_
_space_group_symop_operation_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_occupancy
Ca Ca1 0.7566(2) 0.11114(16) 0.03989(10) 0.0214(3) Uani d 1
O O1 0.4901(7) 0.0237(6) 0.1072(4) 0.0294(12) Uani d 1
O O2 0.7073(7) 0.2219(6) 0.2165(4) 0.0302(12) Uani d 1
O O5 0.6524(7) 0.3423(6) 0.0331(4) 0.0248(12) Uani d 1
H H1W 0.576(8) 0.367(9) 0.063(6) 0.030 Uiso d 1
H H2W 0.625(10) 0.331(9) -0.032(2) 0.030 Uiso d 1
O O6 1.0260(8) 0.2610(7) 0.1713(4) 0.0360(14) Uani d 1
H H3W 1.125(6) 0.313(7) 0.169(6) 0.043 Uiso d 1
H H4W 1.028(12) 0.256(10) 0.232(3) 0.043 Uiso d 1
O O3 0.8632(7) -0.1067(6) 0.0374(4) 0.0303(13) Uani d 1
O O4 1.0911(7) -0.2226(6) 0.0632(4) 0.0305(13) Uani d 1
N N2 0.9542(9) -0.4002(8) 0.1626(5) 0.0257(15) Uani d 1
H H2A 1.053(7) -0.415(9) 0.153(6) 0.031 Uiso d 1
H H2B 0.896(10) -0.491(6) 0.120(5) 0.031 Uiso d 1
N N1 0.5637(9) 0.2912(7) 0.3744(5) 0.0250(14) Uani d 1
H H1A 0.480(8) 0.329(9) 0.393(6) 0.030 Uiso d 1
H H1B 0.625(9) 0.362(7) 0.358(6) 0.030 Uiso d 1
C C10 0.8593(11) -0.1694(9) 0.2437(6) 0.0308(18) Uani d 1
H H8 0.8894 -0.0586 0.2463 0.037 Uiso calc 1
H H9 0.7423 -0.1900 0.2563 0.037 Uiso calc 1
C C9 1.0000(12) -0.2034(10) 0.3254(6) 0.038(2) Uani d 1
H H10 0.9776 -0.1760 0.3959 0.045 Uiso calc 1
H H11 1.1193 -0.1437 0.3336 0.045 Uiso calc 1
C C8 0.9858(11) -0.3790(9) 0.2807(5) 0.0312(19) Uani d 1
H H12 1.0970 -0.4091 0.3119 0.037 Uiso calc 1
H H13 0.8848 -0.4402 0.2933 0.037 Uiso calc 1
C C7 0.8560(10) -0.2808(8) 0.1353(5) 0.0246(16) Uani d 1
H H14 0.7302 -0.3332 0.0914 0.030 Uiso calc 1
C C6 0.9462(10) -0.1969(8) 0.0726(5) 0.0240(16) Uani d 1
C C5 0.4773(11) 0.0135(9) 0.3293(6) 0.0292(18) Uani d 1
H H1 0.3804 -0.0009 0.3617 0.035 Uiso calc 1
H H2 0.4713 -0.0866 0.2749 0.035 Uiso calc 1
C C4 0.6589(12) 0.0713(9) 0.4148(6) 0.034(2) Uani d 1
H H3 0.6670 0.0152 0.4683 0.041 Uiso calc 1
H H4 0.7560 0.0567 0.3821 0.041 Uiso calc 1
C C3 0.6678(11) 0.2433(9) 0.4655(5) 0.0287(18) Uani d 1
H H5 0.7926 0.3041 0.4943 0.034 Uiso calc 1
H H6 0.6129 0.2594 0.5243 0.034 Uiso calc 1
C C2 0.4668(11) 0.1463(8) 0.2801(5) 0.0251(15) Uani d 1
H H7 0.3402 0.1509 0.2497 0.030 Uiso calc 1
C C1 0.5620(10) 0.1303(8) 0.1964(5) 0.0211(12) Uani d 1
I I1 0.40641(6) 0.52553(5) 0.18903(3) 0.02488(16) Uani d 1
I I2 0.18089(7) 0.31320(6) 0.44926(3) 0.02940(17) Uani 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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
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
O3 Ca1 O1 . 2_655 92.68(19)
O3 Ca1 O6 . . 88.9(2)
O1 Ca1 O6 2_655 . 171.4(2)
O3 Ca1 O5 . . 176.2(2)
O1 Ca1 O5 2_655 . 86.69(18)
O6 Ca1 O5 . . 91.2(2)
O3 Ca1 O4 . 2_755 102.3(2)
O1 Ca1 O4 2_655 2_755 93.50(19)
O6 Ca1 O4 . 2_755 77.94(19)
O5 Ca1 O4 . 2_755 73.95(19)
O3 Ca1 O2 . . 109.18(18)
O1 Ca1 O2 2_655 . 118.14(19)
O6 Ca1 O2 . . 69.1(2)
O5 Ca1 O2 . . 74.40(17)
O4 Ca1 O2 2_755 . 133.12(19)
O3 Ca1 O1 . . 94.58(19)
O1 Ca1 O1 2_655 . 70.85(19)
O6 Ca1 O1 . . 117.43(18)
O5 Ca1 O1 . . 88.80(18)
O4 Ca1 O1 2_755 . 157.57(16)
O2 Ca1 O1 . . 50.92(16)
O3 Ca1 C1 . . 103.14(19)
O1 Ca1 C1 2_655 . 94.8(2)
O6 Ca1 C1 . . 93.0(2)
O5 Ca1 C1 . . 80.70(18)
O4 Ca1 C1 2_755 . 152.77(19)
O2 Ca1 C1 . . 25.20(17)
O1 Ca1 C1 . . 25.71(17)
O3 Ca1 C6 . 2_755 85.3(2)
O1 Ca1 C6 2_655 2_755 102.18(19)
O6 Ca1 C6 . 2_755 69.55(19)
O5 Ca1 C6 . 2_755 91.14(19)
O4 Ca1 C6 2_755 2_755 18.73(16)
O2 Ca1 C6 . 2_755 135.61(18)
O1 Ca1 C6 . 2_755 173.02(16)
C1 Ca1 C6 . 2_755 160.72(19)
O3 Ca1 Ca1 . 2_655 94.52(16)
O1 Ca1 Ca1 2_655 2_655 37.88(14)
O6 Ca1 Ca1 . 2_655 150.35(15)
O5 Ca1 Ca1 . 2_655 87.31(15)
O4 Ca1 Ca1 2_755 2_655 129.49(14)
O2 Ca1 Ca1 . 2_655 82.06(14)
O1 Ca1 Ca1 . 2_655 32.97(10)
C1 Ca1 Ca1 . 2_655 57.49(15)
C6 Ca1 Ca1 2_755 2_655 140.06(13)
O3 Ca1 H2W . . 159.2(9)
O1 Ca1 H2W 2_655 . 74.4(14)
O6 Ca1 H2W . . 101.6(15)
O5 Ca1 H2W . . 17.6(9)
O4 Ca1 H2W 2_755 . 63.2(15)
O2 Ca1 H2W . . 91.5(10)
O1 Ca1 H2W . . 96.4(16)
C1 Ca1 H2W . . 94.3(13)
C6 Ca1 H2W 2_755 . 81.7(15)
Ca1 Ca1 H2W 2_655 . 85.2(17)
O3 Ca1 H4W . . 85.8(18)
O1 Ca1 H4W 2_655 . 172.4(12)
O6 Ca1 H4W . . 16.2(12)
O5 Ca1 H4W . . 95.3(18)
O4 Ca1 H4W 2_755 . 94.1(12)
O2 Ca1 H4W . . 55.7(15)
O1 Ca1 H4W . . 101.8(12)
C1 Ca1 H4W . . 78.3(13)
C6 Ca1 H4W 2_755 . 85.2(12)
Ca1 Ca1 H4W 2_655 . 134.7(12)
H2W Ca1 H4W . . 109(2)
C1 O1 Ca1 . 2_655 150.9(5)
C1 O1 Ca1 . . 90.1(5)
Ca1 O1 Ca1 2_655 . 109.15(19)
C1 O2 Ca1 . . 96.7(4)
Ca1 O5 H1W . . 120(6)
Ca1 O5 H2W . . 102(5)
H1W O5 H2W . . 115(8)
Ca1 O6 H3W . . 134(5)
Ca1 O6 H4W . . 112(6)
H3W O6 H4W . . 114(8)
C6 O3 Ca1 . . 158.2(5)
C6 O4 Ca1 . 2_755 122.8(4)
C7 N2 C8 . . 108.4(6)
C7 N2 H2A . . 127(6)
C8 N2 H2A . . 103(5)
C7 N2 H2B . . 109(5)
C8 N2 H2B . . 115(5)
H2A N2 H2B . . 94(7)
C2 N1 C3 . . 109.3(5)
C2 N1 H1A . . 104(5)
C3 N1 H1A . . 108(5)
C2 N1 H1B . . 114(5)
C3 N1 H1B . . 114(5)
H1A N1 H1B . . 107(7)
C9 C10 C7 . . 105.1(6)
C9 C10 H8 . . 110.7
C7 C10 H8 . . 110.7
C9 C10 H9 . . 110.7
C7 C10 H9 . . 110.7
H8 C10 H9 . . 108.8
C10 C9 C8 . . 104.3(6)
C10 C9 H10 . . 110.9
C8 C9 H10 . . 110.9
C10 C9 H11 . . 110.9
C8 C9 H11 . . 110.9
H10 C9 H11 . . 108.9
N2 C8 C9 . . 101.0(6)
N2 C8 H12 . . 111.6
C9 C8 H12 . . 111.6
N2 C8 H13 . . 111.6
C9 C8 H13 . . 111.6
H12 C8 H13 . . 109.4
N2 C7 C6 . . 110.1(6)
N2 C7 C10 . . 105.0(5)
C6 C7 C10 . . 112.6(6)
N2 C7 H14 . . 109.7
C6 C7 H14 . . 109.7
C10 C7 H14 . . 109.7
O4 C6 O3 . . 127.2(7)
O4 C6 C7 . . 118.5(6)
O3 C6 C7 . . 114.2(7)
O4 C6 Ca1 . 2_755 38.4(3)
O3 C6 Ca1 . 2_755 88.8(5)
C7 C6 Ca1 . 2_755 156.9(5)
C4 C5 C2 . . 102.8(6)
C4 C5 H1 . . 111.2
C2 C5 H1 . . 111.2
C4 C5 H2 . . 111.2
C2 C5 H2 . . 111.2
H1 C5 H2 . . 109.1
C3 C4 C5 . . 103.7(6)
C3 C4 H3 . . 111.0
C5 C4 H3 . . 111.0
C3 C4 H4 . . 111.0
C5 C4 H4 . . 111.0
H3 C4 H4 . . 109.0
C4 C3 N1 . . 103.9(5)
C4 C3 H5 . . 111.0
N1 C3 H5 . . 111.0
C4 C3 H6 . . 111.0
N1 C3 H6 . . 111.0
H5 C3 H6 . . 109.0
C1 C2 N1 . . 109.3(6)
C1 C2 C5 . . 111.5(6)
N1 C2 C5 . . 103.2(5)
C1 C2 H7 . . 110.9
N1 C2 H7 . . 110.9
C5 C2 H7 . . 110.9
O2 C1 O1 . . 122.3(7)
O2 C1 C2 . . 119.6(6)
O1 C1 C2 . . 118.1(7)
O2 C1 Ca1 . . 58.1(4)
O1 C1 Ca1 . . 64.2(4)
C2 C1 Ca1 . . 177.7(5)
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 . 2.621(6) y
Ca1 O2 . 2.489(6) y
Ca1 O4 2_755 2.396(5) y
Ca1 O5 . 2.376(5) y
Ca1 O6 . 2.365(6) y
Ca1 O1 2_655 2.323(5) y
Ca1 O3 . 2.252(5) y
Ca1 Ca1 2_755 4.829(4) y
Ca1 Ca1 2_655 4.032(4) y
Ca1 C1 . 2.911(8) ?
Ca1 C6 2_755 3.238(8) ?
O1 C1 . 1.263(8) ?
O1 Ca1 2_655 2.323(5) ?
O2 C1 . 1.248(9) ?
O5 H1W . 0.83(2) ?
O5 H2W . 0.83(2) ?
O6 H3W . 0.876(17) ?
O6 H4W . 0.84(2) ?
O3 C6 . 1.241(8) ?
O4 C6 . 1.237(9) ?
O4 Ca1 2_755 2.396(5) ?
N2 C7 . 1.493(9) ?
N2 C8 . 1.515(9) ?
N2 H2A . 0.85(4) ?
N2 H2B . 0.85(4) ?
N1 C2 . 1.509(9) ?
N1 C3 . 1.512(8) ?
N1 H1A . 0.86(4) ?
N1 H1B . 0.86(4) ?
C10 C9 . 1.496(10) ?
C10 C7 . 1.536(10) ?
C10 H8 . 0.9900 ?
C10 H9 . 0.9900 ?
C9 C8 . 1.521(11) ?
C9 H10 . 0.9900 ?
C9 H11 . 0.9900 ?
C8 H12 . 0.9900 ?
C8 H13 . 0.9900 ?
C7 C6 . 1.527(10) ?
C7 H14 . 1.0000 ?
C6 Ca1 2_755 3.238(8) ?
C5 C4 . 1.527(10) ?
C5 C2 . 1.531(10) ?
C5 H1 . 0.9900 ?
C5 H2 . 0.9900 ?
C4 C3 . 1.510(11) ?
C4 H3 . 0.9900 ?
C4 H4 . 0.9900 ?
C3 H5 . 0.9900 ?
C3 H6 . 0.9900 ?
C2 C1 . 1.505(10) ?
C2 H7 . 1.0000 ?
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
_geom_hbond_publ_flag
N1 H1A I2 . 0.85(7) 2.67(7) 3.459(8) 154(7) y
N1 H1B I1 . 0.86(7) 3.33(7) 3.809(7) 118(6) y
N1 H1B I2 2_666 0.86(7) 3.24(7) 3.695(7) 116(5) y
N2 H2A I1 1_645 0.85(6) 2.88(6) 3.700(8) 161(7) y
N2 H2B) O5 1_545 0.86(6) 2.13(7) 2.904(9) 151(7) y
O5 H1W I1 . 0.84(7) 2.68(7) 3.486(6) 163(6) y
O5 H2W I1 2_665 0.83(3) 2.77(6) 3.491(6) 147(7) y
O6 H3W I1 1_655 0.87(6) 2.65(6) 3.509(7) 167(5) y
O6 H4W I2 1_655 0.84(5) 2.77(4) 3.543(6) 155(7) y

_cod_database_fobs_code 2240763
