#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/99/2019907.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_2019907
loop_
_publ_author_name
'Lamberts, Kevin'
'Şerb, Mihaela-Diana'
'Englert, Ulli'
_publ_section_title
;
 One- and two-dimensional polymers from proline and calcium bromide
;
_journal_coeditor_code           YP3093
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615005008
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ca (C5 H9 N1 O2)2 (H2 O1)2] Br2'
_chemical_formula_moiety         'C10 H22 Ca N2 O6 2+, 2(Br -)'
_chemical_formula_sum            'C10 H22 Br2 Ca N2 O6'
_chemical_formula_weight         466.19
_chemical_name_systematic
catena-Poly[[aquacalcium(II)]-μ-aqua-μ₃-DL-proline-μ₂-DL-proline]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.9880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5177(13)
_cell_length_b                   7.8151(7)
_cell_length_c                   16.3815(16)
_cell_measurement_reflns_used    5444
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.21
_cell_measurement_theta_min      2.29
_cell_volume                     1663.6(3)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2008)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2008)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_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 0.954
_diffrn_measurement_device_type
'Bruker d8 goniometer with an APEX CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24328
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.733
_diffrn_reflns_theta_min         2.587
_exptl_absorpt_coefficient_mu    5.206
_exptl_absorpt_correction_T_max  .7461
_exptl_absorpt_correction_T_min  .4269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       needle
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.438
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4950
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0353
_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
;
w=1/[σ²(Fo²)+(0.0220P)²+0.9000P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                4307
_reflns_number_total             4950
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            yp3093sup1.cif
_cod_data_source_block           1
_cod_database_code               2019907
_cod_database_fobs_code          2019907
#BEGIN Tags that were not found in dictionaries:
_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   0.345
_shelx_estimated_absorpt_t_max   0.652
_shelxl_version_number           20.13
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 -0.03024(3) 0.73199(5) -0.03630(2) 0.00994(8) Uani d 1
Br Br1 0.39471(2) 0.09604(3) 0.21768(2) 0.01529(6) Uani d 1
Br Br2 0.25796(2) 0.51410(3) -0.14487(2) 0.01390(5) Uani d 1
O O1 0.13614(11) 0.71883(18) 0.06342(9) 0.0134(3) Uani d 1
O O2 0.17880(11) 0.44177(18) 0.09274(9) 0.0133(3) Uani d 1
C C1 0.19681(15) 0.5995(3) 0.09691(12) 0.0113(4) Uani d 1
C C2 0.30554(15) 0.6591(3) 0.14306(12) 0.0116(4) Uani d 1
H H2 0.3027 0.7641 0.1772 0.014 Uiso calc 1
C C3 0.36813(16) 0.6948(3) 0.07862(13) 0.0157(4) Uani d 1
H H3A 0.3223 0.6991 0.0200 0.019 Uiso calc 1
H H3B 0.4056 0.8047 0.0915 0.019 Uiso calc 1
C C4 0.44328(16) 0.5450(3) 0.08921(14) 0.0166(4) Uani d 1
H H4A 0.4103 0.4439 0.0564 0.020 Uiso calc 1
H H4B 0.5052 0.5767 0.0714 0.020 Uiso calc 1
C C5 0.46954(16) 0.5122(3) 0.18362(14) 0.0167(4) Uani d 1
H H5A 0.5017 0.3984 0.1984 0.020 Uiso calc 1
H H5B 0.5160 0.6014 0.2161 0.020 Uiso calc 1
N N1 0.36515(14) 0.5202(2) 0.19917(11) 0.0126(3) Uani d 1
H H1N 0.3719(19) 0.542(3) 0.2524(11) 0.015 Uiso d 1
H H2N 0.3339(18) 0.426(2) 0.1853(15) 0.015 Uiso d 1
O O3 0.07574(11) 0.82890(19) -0.12582(9) 0.0146(3) Uani d 1
O O4 0.05729(11) 1.0672(2) -0.05780(9) 0.0169(3) Uani d 1
C C6 0.10168(15) 0.9775(3) -0.10027(12) 0.0108(4) Uani d 1
C C7 0.19624(15) 1.0570(3) -0.11861(13) 0.0118(4) Uani d 1
H H7 0.1749 1.1590 -0.1562 0.014 Uiso calc 1
C C8 0.27868(16) 1.1100(3) -0.03832(14) 0.0157(4) Uani d 1
H H8A 0.2658 1.2267 -0.0201 0.019 Uiso calc 1
H H8B 0.2820 1.0289 0.0088 0.019 Uiso calc 1
C C9 0.37676(16) 1.1036(3) -0.06692(15) 0.0195(5) Uani d 1
H H9A 0.3828 1.2062 -0.1007 0.023 Uiso calc 1
H H9B 0.4384 1.0959 -0.0176 0.023 Uiso calc 1
C C10 0.36426(16) 0.9424(3) -0.12097(14) 0.0164(4) Uani d 1
H H10A 0.4018 0.9525 -0.1648 0.020 Uiso calc 1
H H10B 0.3898 0.8406 -0.0854 0.020 Uiso calc 1
N N2 0.24971(13) 0.9306(2) -0.16118(11) 0.0125(3) Uani d 1
H H3N 0.2416(19) 0.947(3) -0.2149(11) 0.015 Uiso d 1
H H4N 0.2262(18) 0.831(2) -0.1566(15) 0.015 Uiso d 1
O O5 -0.03995(11) 0.53197(19) 0.08375(9) 0.0119(3) Uani d 1
H H1W -0.0034(17) 0.555(3) 0.1264(12) 0.014 Uiso d 1
H H2W -0.0915(15) 0.516(3) 0.0947(16) 0.014 Uiso d 1
O O6 -0.15013(11) 0.93335(19) -0.13128(9) 0.0131(3) Uani d 1
H H3W -0.140(2) 1.023(2) -0.1128(16) 0.016 Uiso d 1
H H4W -0.2080(13) 0.920(3) -0.1470(15) 0.016 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'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
O4 Ca1 O2 3_575 3_565 112.06(5)
O4 Ca1 O1 3_575 . 82.22(5)
O2 Ca1 O1 3_565 . 140.57(5)
O4 Ca1 O3 3_575 . 114.84(5)
O2 Ca1 O3 3_565 . 120.98(5)
O1 Ca1 O3 . . 79.98(5)
O4 Ca1 O6 3_575 . 77.88(5)
O2 Ca1 O6 3_565 . 77.48(5)
O1 Ca1 O6 . . 141.84(5)
O3 Ca1 O6 . . 79.39(5)
O4 Ca1 O5 3_575 3_565 157.25(5)
O2 Ca1 O5 3_565 3_565 76.09(5)
O1 Ca1 O5 . 3_565 79.02(5)
O3 Ca1 O5 . 3_565 74.40(5)
O6 Ca1 O5 . 3_565 124.85(5)
O4 Ca1 O5 3_575 . 81.34(5)
O2 Ca1 O5 3_565 . 74.52(5)
O1 Ca1 O5 . . 71.61(5)
O3 Ca1 O5 . . 145.15(5)
O6 Ca1 O5 . . 135.39(5)
O5 Ca1 O5 3_565 . 80.62(5)
O4 Ca1 O4 3_575 . 67.36(6)
O2 Ca1 O4 3_565 . 141.66(5)
O1 Ca1 O4 . . 77.64(5)
O3 Ca1 O4 . . 47.70(4)
O6 Ca1 O4 . . 64.73(5)
O5 Ca1 O4 3_565 . 120.16(5)
O5 Ca1 O4 . . 138.55(5)
O4 Ca1 C6 3_575 . 90.99(6)
O2 Ca1 C6 3_565 . 138.23(5)
O1 Ca1 C6 . . 74.22(5)
O3 Ca1 C6 . . 23.87(5)
O6 Ca1 C6 . . 73.92(5)
O5 Ca1 C6 3_565 . 96.13(5)
O5 Ca1 C6 . . 145.67(5)
O4 Ca1 C6 . . 24.32(5)
O4 Ca1 Ca1 3_575 3_565 119.83(4)
O2 Ca1 Ca1 3_565 3_565 70.56(4)
O1 Ca1 Ca1 . 3_565 70.56(4)
O3 Ca1 Ca1 . 3_565 111.73(4)
O6 Ca1 Ca1 . 3_565 147.41(4)
O5 Ca1 Ca1 3_565 3_565 40.90(3)
O5 Ca1 Ca1 . 3_565 39.73(3)
O4 Ca1 Ca1 . 3_565 145.37(3)
C6 Ca1 Ca1 . 3_565 128.11(4)
O4 Ca1 Ca1 3_575 3_575 38.32(4)
O2 Ca1 Ca1 3_565 3_575 136.42(4)
O1 Ca1 Ca1 . 3_575 77.58(4)
O3 Ca1 Ca1 . 3_575 76.63(4)
O6 Ca1 Ca1 . 3_575 66.60(4)
O5 Ca1 Ca1 3_565 3_575 145.35(4)
O5 Ca1 Ca1 . 3_575 115.11(4)
O4 Ca1 Ca1 . 3_575 29.04(3)
C6 Ca1 Ca1 . 3_575 52.91(4)
Ca1 Ca1 Ca1 3_565 3_575 144.53(2)
C1 O1 Ca1 . . 134.82(13)
C1 O2 Ca1 . 3_565 135.17(13)
O2 C1 O1 . . 127.49(18)
O2 C1 C2 . . 118.15(17)
O1 C1 C2 . . 114.27(17)
N1 C2 C1 . . 111.27(16)
N1 C2 C3 . . 104.18(16)
C1 C2 C3 . . 110.43(16)
N1 C2 H2 . . 110.3
C1 C2 H2 . . 110.3
C3 C2 H2 . . 110.3
C4 C3 C2 . . 104.80(17)
C4 C3 H3A . . 110.8
C2 C3 H3A . . 110.8
C4 C3 H3B . . 110.8
C2 C3 H3B . . 110.8
H3A C3 H3B . . 108.9
C5 C4 C3 . . 102.00(17)
C5 C4 H4A . . 111.4
C3 C4 H4A . . 111.4
C5 C4 H4B . . 111.4
C3 C4 H4B . . 111.4
H4A C4 H4B . . 109.2
N1 C5 C4 . . 101.52(16)
N1 C5 H5A . . 111.5
C4 C5 H5A . . 111.5
N1 C5 H5B . . 111.5
C4 C5 H5B . . 111.5
H5A C5 H5B . . 109.3
C5 N1 C2 . . 107.24(16)
C5 N1 H1N . . 109.5(17)
C2 N1 H1N . . 111.1(17)
C5 N1 H2N . . 109.8(17)
C2 N1 H2N . . 108.6(17)
H1N N1 H2N . . 110(2)
C6 O3 Ca1 . . 104.14(12)
C6 O4 Ca1 . 3_575 160.85(14)
C6 O4 Ca1 . . 80.65(12)
Ca1 O4 Ca1 3_575 . 112.64(6)
O4 C6 O3 . . 124.95(19)
O4 C6 C7 . . 115.98(17)
O3 C6 C7 . . 119.04(17)
O4 C6 Ca1 . . 75.03(11)
O3 C6 Ca1 . . 51.99(10)
C7 C6 Ca1 . . 160.37(13)
N2 C7 C6 . . 111.10(16)
N2 C7 C8 . . 104.32(16)
C6 C7 C8 . . 113.16(17)
N2 C7 H7 . . 109.4
C6 C7 H7 . . 109.4
C8 C7 H7 . . 109.4
C9 C8 C7 . . 102.50(17)
C9 C8 H8A . . 111.3
C7 C8 H8A . . 111.3
C9 C8 H8B . . 111.3
C7 C8 H8B . . 111.3
H8A C8 H8B . . 109.2
C10 C9 C8 . . 103.84(17)
C10 C9 H9A . . 111.0
C8 C9 H9A . . 111.0
C10 C9 H9B . . 111.0
C8 C9 H9B . . 111.0
H9A C9 H9B . . 109.0
N2 C10 C9 . . 103.91(16)
N2 C10 H10A . . 111.0
C9 C10 H10A . . 111.0
N2 C10 H10B . . 111.0
C9 C10 H10B . . 111.0
H10A C10 H10B . . 109.0
C7 N2 C10 . . 108.90(16)
C7 N2 H3N . . 115.6(17)
C10 N2 H3N . . 105.2(17)
C7 N2 H4N . . 108.8(16)
C10 N2 H4N . . 112.3(17)
H3N N2 H4N . . 106(2)
Ca1 O5 Ca1 3_565 . 99.38(5)
Ca1 O5 H1W 3_565 . 106(2)
Ca1 O5 H1W . . 113.9(19)
Ca1 O5 H2W 3_565 . 112.3(19)
Ca1 O5 H2W . . 121.4(19)
H1W O5 H2W . . 103(3)
Ca1 O6 H3W . . 109(2)
Ca1 O6 H4W . . 124(2)
H3W O6 H4W . . 108(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ca1 O4 3_575 2.2984(15)
Ca1 O2 3_565 2.3894(14)
Ca1 O1 . 2.3903(14)
Ca1 O3 . 2.4360(15)
Ca1 O6 . 2.4768(16)
Ca1 O5 3_565 2.4832(15)
Ca1 O5 . 2.5437(15)
Ca1 O4 . 2.9355(16)
Ca1 C6 . 2.998(2)
Ca1 Ca1 3_565 3.8334(8)
Ca1 Ca1 3_575 4.3698(9)
O1 C1 . 1.263(2)
O2 C1 . 1.255(2)
O2 Ca1 3_565 2.3894(14)
C1 C2 . 1.528(3)
C2 N1 . 1.505(3)
C2 C3 . 1.549(3)
C2 H2 . 1.0000
C3 C4 . 1.528(3)
C3 H3A . 0.9900
C3 H3B . 0.9900
C4 C5 . 1.510(3)
C4 H4A . 0.9900
C4 H4B . 0.9900
C5 N1 . 1.503(3)
C5 H5A . 0.9900
C5 H5B . 0.9900
N1 H1N . 0.868(16)
N1 H2N . 0.850(16)
O3 C6 . 1.251(2)
O4 C6 . 1.251(2)
O4 Ca1 3_575 2.2984(15)
C6 C7 . 1.524(3)
C7 N2 . 1.504(3)
C7 C8 . 1.528(3)
C7 H7 . 1.0000
C8 C9 . 1.524(3)
C8 H8A . 0.9900
C8 H8B . 0.9900
C9 C10 . 1.523(3)
C9 H9A . 0.9900
C9 H9B . 0.9900
C10 N2 . 1.509(3)
C10 H10A . 0.9900
C10 H10B . 0.9900
N2 H3N . 0.865(16)
N2 H4N . 0.853(16)
O5 Ca1 3_565 2.4832(15)
O5 H1W . 0.758(16)
O5 H2W . 0.777(16)
O6 H3W . 0.762(16)
O6 H4W . 0.760(16)
