#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176809 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/04/2240412.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_2240412
loop_
_publ_author_name
'Sathiskumar, S.'
'Balakrishnan, T.'
'Ramamurthi, K.'
'Thamotharan, S.'
_publ_section_title
;
 Crystal structure of
 catena-poly[[cadmium(II)-di-μ₂-bromido-μ₂-<small>L</small>-proline-κ²O:O']
 monohydrate]
;
_journal_coeditor_code           CV5483
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              217
_journal_page_last               219
_journal_paper_doi               10.1107/S2056989015001176
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Cd Br2 (C5 H9 N O2)], H2 O'
_chemical_formula_moiety         'C5 H9 Cd Br2 N O2, H2 O'
_chemical_formula_sum            'C5 H11 Br2 Cd N O3'
_chemical_formula_weight         405.37
_chemical_name_systematic
'catena-Poly[[cadmium(II)-di-μ₂-bromido-μ₂-L-proline-κ²O:O'] monohydrate]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1891(8)
_cell_length_b                   13.4961(11)
_cell_length_c                   7.4491(5)
_cell_measurement_reflns_used    4066
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      55.178
_cell_measurement_theta_min      5.005
_cell_volume                     1024.35(13)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT and XPREP (Bruker, 2008)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae et al.,  2008)
;
_computing_structure_refinement
;
SHELXL2014/6 (Sheldrick, 2015)
;
_computing_structure_solution
;
atomic coordinates of chlorido analogue (Yukawa et al., 1983)
used as starting values in the initial cycles of the
refinement
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8264
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.231
_diffrn_reflns_theta_min         3.124
_exptl_absorpt_coefficient_mu    9.903
_exptl_absorpt_correction_T_max  0.155
_exptl_absorpt_correction_T_min  0.129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.629
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.068
_refine_ls_abs_structure_details
;
Flack x determined using 705 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   0.035(15)
_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     115
_refine_ls_number_reflns         2481
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0243P)²+1.4185P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                1964
_reflns_number_total             2481
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cv5483sup1.cf
_cod_data_source_block           I
_cod_database_code               2240412
_cod_database_fobs_code          2240412
#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   0.129
_shelx_estimated_absorpt_t_max   0.155
_shelxl_version_number           2014/6
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, 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
Cd Cd1 0.24415(7) 0.00192(7) 0.31349(9) 0.0425(2) Uani d 1
Br Br1 0.44442(8) 0.03071(8) 0.06673(14) 0.0450(3) Uani d 1
Br Br2 0.37743(10) 0.11262(9) 0.56256(15) 0.0537(3) Uani d 1
O O1 0.1309(8) 0.1397(6) 0.2136(9) 0.057(2) Uani d 1
O O2 0.1420(7) 0.1362(6) -0.0865(9) 0.056(2) Uani d 1
N N1 -0.0870(10) 0.2205(8) -0.1393(11) 0.062(3) Uani d 1
H H1A -0.0168 0.2171 -0.2100 0.075 Uiso calc 1
H H1B -0.1202 0.2813 -0.1471 0.075 Uiso calc 1
C C1 0.0861(9) 0.1560(7) 0.0564(15) 0.039(2) Uani d 1
C C2 -0.0488(10) 0.1988(8) 0.0510(15) 0.053(3) Uani d 1
H H2 -0.0524 0.2596 0.1229 0.064 Uiso calc 1
C C3 -0.1523(12) 0.1260(13) 0.115(2) 0.084(5) Uani d 1
H H3A -0.1172 0.0826 0.2066 0.100 Uiso calc 1
H H3B -0.2279 0.1607 0.1627 0.100 Uiso calc 1
C C4 -0.1878(13) 0.0697(13) -0.047(2) 0.094(5) Uani d 1
H H4A -0.2733 0.0392 -0.0326 0.113 Uiso calc 1
H H4B -0.1236 0.0181 -0.0701 0.113 Uiso calc 1
C C5 -0.1899(14) 0.1441(12) -0.200(2) 0.086(5) Uani d 1
H H5A -0.2758 0.1743 -0.2126 0.103 Uiso calc 1
H H5B -0.1651 0.1134 -0.3127 0.103 Uiso calc 1
O O1W 0.111(2) 0.2521(17) 0.587(2) 0.183(8) Uani d 1
H H1W 0.11(3) 0.296(11) 0.50(2) 0.201 Uiso d 1
H H2W 0.13(3) 0.197(8) 0.54(3) 0.201 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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
O1 Cd1 O2 . 2 179.9(3)
O1 Cd1 Br2 . 2_554 90.50(19)
O2 Cd1 Br2 2 2_554 89.53(19)
O1 Cd1 Br1 . 2 90.0(2)
O2 Cd1 Br1 2 2 90.03(19)
Br2 Cd1 Br1 2_554 2 93.59(4)
O1 Cd1 Br2 . . 91.52(19)
O2 Cd1 Br2 2 . 88.44(19)
Br2 Cd1 Br2 2_554 . 177.29(3)
Br1 Cd1 Br2 2 . 88.22(3)
O1 Cd1 Br1 . . 92.4(2)
O2 Cd1 Br1 2 . 87.56(19)
Br2 Cd1 Br1 2_554 . 87.67(4)
Br1 Cd1 Br1 2 . 177.27(4)
Br2 Cd1 Br1 . . 90.44(4)
Cd1 Br1 Cd1 2_554 . 85.27(3)
Cd1 Br2 Cd1 2 . 85.98(3)
C1 O1 Cd1 . . 127.7(6)
C1 O2 Cd1 . 2_554 132.9(7)
C2 N1 C5 . . 108.9(10)
C2 N1 H1A . . 109.9
C5 N1 H1A . . 109.9
C2 N1 H1B . . 109.9
C5 N1 H1B . . 109.9
H1A N1 H1B . . 108.3
O2 C1 O1 . . 126.0(8)
O2 C1 C2 . . 119.0(10)
O1 C1 C2 . . 114.9(9)
C1 C2 N1 . . 109.9(9)
C1 C2 C3 . . 112.4(10)
N1 C2 C3 . . 103.9(10)
C1 C2 H2 . . 110.1
N1 C2 H2 . . 110.1
C3 C2 H2 . . 110.1
C4 C3 C2 . . 104.5(11)
C4 C3 H3A . . 110.9
C2 C3 H3A . . 110.9
C4 C3 H3B . . 110.9
C2 C3 H3B . . 110.9
H3A C3 H3B . . 108.9
C3 C4 C5 . . 106.0(12)
C3 C4 H4A . . 110.5
C5 C4 H4A . . 110.5
C3 C4 H4B . . 110.5
C5 C4 H4B . . 110.5
H4A C4 H4B . . 108.7
C4 C5 N1 . . 102.3(10)
C4 C5 H5A . . 111.3
N1 C5 H5A . . 111.3
C4 C5 H5B . . 111.3
N1 C5 H5B . . 111.3
H5A C5 H5B . . 109.2
H1W O1W H2W . . 106(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cd1 O1 . 2.312(8)
Cd1 O2 2 2.318(8)
Cd1 Br2 2_554 2.7236(13)
Cd1 Br1 2 2.7285(11)
Cd1 Br2 . 2.7421(13)
Cd1 Br1 . 2.7737(12)
Br1 Cd1 2_554 2.7285(11)
Br2 Cd1 2 2.7236(13)
O1 C1 . 1.276(12)
O2 C1 . 1.237(12)
O2 Cd1 2_554 2.318(8)
N1 C2 . 1.499(13)
N1 C5 . 1.537(17)
N1 H1A . 0.8900
N1 H1B . 0.8900
C1 C2 . 1.491(13)
C2 C3 . 1.517(19)
C2 H2 . 0.9800
C3 C4 . 1.47(2)
C3 H3A . 0.9700
C3 H3B . 0.9700
C4 C5 . 1.52(2)
C4 H4A . 0.9700
C4 H4B . 0.9700
C5 H5A . 0.9700
C5 H5B . 0.9700
O1W H1W . 0.87(3)
O1W H2W . 0.87(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
N1 H1A O2 . 0.89 2.16 2.626(12) 112.1
O1W H2W O1 . 0.84(17) 2.6(2) 3.175(19) 132
O1W H2W Br2 . 0.84(17) 2.8(3) 3.311(19) 123
N1 H1A O1W 1_554 0.89 2.05 2.90(2) 159
N1 H1B Br1 3_455 0.89 2.69 3.416(11) 140
O1W H1W Br2 3_456 0.88(16) 2.7(3) 3.197(19) 116
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_site_symmetry_1
_geom_torsion
Cd1 O2 C1 O1 2_554 44.5(15)
Cd1 O2 C1 C2 2_554 -132.7(9)
Cd1 O1 C1 O2 . -40.4(15)
Cd1 O1 C1 C2 . 136.8(8)
O2 C1 C2 N1 . -6.1(15)
O1 C1 C2 N1 . 176.4(9)
O2 C1 C2 C3 . 109.1(12)
O1 C1 C2 C3 . -68.3(13)
C5 N1 C2 C1 . 107.4(11)
C5 N1 C2 C3 . -13.1(11)
C1 C2 C3 C4 . -87.0(14)
N1 C2 C3 C4 . 31.8(13)
C2 C3 C4 C5 . -39.1(15)
C3 C4 C5 N1 . 29.9(14)
C2 N1 C5 C4 . -9.7(12)
