#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/59/2105980.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_2105980
loop_
_publ_author_name
'Lamberts, Kevin'
'Möller, Andreas'
'Englert, Ulli'
_publ_section_title
;
 Enantiopure and racemic alanine as bridging ligands in Ca and Mn chain
 polymers
;
_journal_coeditor_code           GP5078
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              989
_journal_page_last               998
_journal_paper_doi               10.1107/S2052520614021398
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C6 H18 Ca N2 O6, 2(Cl), H2 O'
_chemical_formula_sum            'C6 H20 Ca Cl2 N2 O7'
_chemical_formula_weight         343.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.347(7)
_cell_length_b                   8.702(3)
_cell_length_c                   7.391(2)
_cell_measurement_temperature    100(2)
_cell_volume                     1501.6(8)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1285
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16504
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.414
_diffrn_reflns_theta_min         2.498
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       needle
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.313
_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     102
_refine_ls_number_reflns         1545
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0250P)²+0.6000P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                1164
_reflns_number_total             1545
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            gp5078sup1.cif
_cod_data_source_block           5
_cod_original_cell_volume        1501.5(8)
_cod_database_code               2105980
_cod_database_fobs_code          2105980
#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   0.857
_shelx_estimated_absorpt_t_max   0.969
_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+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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 0.5000 0.59494(8) 0.2500 0.01290(19) Uani d 1
Cl Cl1 0.68892(3) 0.73248(7) 0.05715(9) 0.01771(18) Uani d 1
O O1 0.59104(7) 0.4699(2) 0.2517(3) 0.0224(5) Uani d 1
O O2 0.53781(8) 0.3579(2) 0.0429(2) 0.0208(4) Uani d 1
C C1 0.58538(11) 0.3843(3) 0.1180(4) 0.0160(6) Uani d 1
C C2 0.63906(11) 0.3070(3) 0.0425(4) 0.0164(6) Uani d 1
H H2 0.6427 0.3342 -0.0885 0.020 Uiso calc 1
C C3 0.63797(12) 0.1331(3) 0.0599(4) 0.0225(6) Uani d 1
H H3A 0.6727 0.0899 0.0053 0.034 Uiso calc 1
H H3B 0.6042 0.0924 -0.0025 0.034 Uiso calc 1
H H3C 0.6364 0.1047 0.1881 0.034 Uiso calc 1
N N1 0.68928(9) 0.3709(3) 0.1413(3) 0.0165(5) Uani d 1
H H1A 0.6865(11) 0.353(3) 0.264(2) 0.020 Uiso d 1
H H1B 0.6908(11) 0.475(2) 0.125(4) 0.020 Uiso d 1
H H1C 0.7220(9) 0.324(3) 0.096(4) 0.020 Uiso d 1
O O1W 0.55648(8) 0.8059(2) 0.1368(3) 0.0250(5) Uani d 1
H H3E 0.5900(8) 0.793(3) 0.117(4) 0.030 Uiso d 1
H H3D 0.5480(13) 0.892(2) 0.175(4) 0.030 Uiso d 1
O O2W 0.5000 1.0793(3) 0.2500 0.0352(8) Uani d 1
H H4 0.4958(15) 1.137(3) 0.160(3) 0.042 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Ca1 O2 7_566 5_665 160.10(10)
O2 Ca1 O1 7_566 3_655 114.50(7)
O2 Ca1 O1 5_665 3_655 75.10(6)
O2 Ca1 O1 7_566 . 75.10(6)
O2 Ca1 O1 5_665 . 114.50(7)
O1 Ca1 O1 3_655 . 125.78(9)
O2 Ca1 O1W 7_566 . 88.93(7)
O2 Ca1 O1W 5_665 . 75.84(7)
O1 Ca1 O1W 3_655 . 146.33(7)
O1 Ca1 O1W . . 82.07(7)
O2 Ca1 O1W 7_566 3_655 75.84(7)
O2 Ca1 O1W 5_665 3_655 88.93(7)
O1 Ca1 O1W 3_655 3_655 82.07(7)
O1 Ca1 O1W . 3_655 146.33(7)
O1W Ca1 O1W . 3_655 80.77(10)
O2 Ca1 O2 7_566 . 121.63(6)
O2 Ca1 O2 5_665 . 74.81(7)
O1 Ca1 O2 3_655 . 86.58(6)
O1 Ca1 O2 . . 50.77(6)
O1W Ca1 O2 . . 101.83(7)
O1W Ca1 O2 3_655 . 162.15(7)
O2 Ca1 O2 7_566 3_655 74.81(7)
O2 Ca1 O2 5_665 3_655 121.63(6)
O1 Ca1 O2 3_655 3_655 50.77(6)
O1 Ca1 O2 . 3_655 86.58(6)
O1W Ca1 O2 . 3_655 162.15(7)
O1W Ca1 O2 3_655 3_655 101.83(7)
O2 Ca1 O2 . 3_655 81.18(8)
O2 Ca1 C1 7_566 3_655 93.36(7)
O2 Ca1 C1 5_665 3_655 99.30(7)
O1 Ca1 C1 3_655 3_655 25.20(7)
O1 Ca1 C1 . 3_655 108.93(8)
O1W Ca1 C1 . 3_655 168.99(7)
O1W Ca1 C1 3_655 3_655 89.35(7)
O2 Ca1 C1 . 3_655 86.13(7)
O2 Ca1 C1 3_655 3_655 25.88(6)
O2 Ca1 C1 7_566 . 99.30(7)
O2 Ca1 C1 5_665 . 93.36(7)
O1 Ca1 C1 3_655 . 108.93(8)
O1 Ca1 C1 . . 25.20(7)
O1W Ca1 C1 . . 89.35(7)
O1W Ca1 C1 3_655 . 168.99(7)
O2 Ca1 C1 . . 25.88(6)
O2 Ca1 C1 3_655 . 86.13(7)
C1 Ca1 C1 3_655 . 100.88(11)
O2 Ca1 Ca1 7_566 5_665 154.57(5)
O2 Ca1 Ca1 5_665 5_665 40.36(5)
O1 Ca1 Ca1 3_655 5_665 79.00(5)
O1 Ca1 Ca1 . 5_665 79.56(5)
O1W Ca1 Ca1 . 5_665 89.66(6)
O1W Ca1 Ca1 3_655 5_665 128.89(6)
O2 Ca1 Ca1 . 5_665 34.46(4)
O2 Ca1 Ca1 3_655 5_665 101.81(5)
C1 Ca1 Ca1 3_655 5_665 92.83(6)
C1 Ca1 Ca1 . 5_665 55.29(6)
O2 Ca1 Ca1 7_566 5_666 40.36(5)
O2 Ca1 Ca1 5_665 5_666 154.57(5)
O1 Ca1 Ca1 3_655 5_666 79.56(5)
O1 Ca1 Ca1 . 5_666 79.00(5)
O1W Ca1 Ca1 . 5_666 128.89(6)
O1W Ca1 Ca1 3_655 5_666 89.66(6)
O2 Ca1 Ca1 . 5_666 101.81(5)
O2 Ca1 Ca1 3_655 5_666 34.46(4)
C1 Ca1 Ca1 3_655 5_666 55.29(6)
C1 Ca1 Ca1 . 5_666 92.83(6)
Ca1 Ca1 Ca1 5_665 5_666 131.82(4)
C1 O1 Ca1 . . 100.03(16)
C1 O2 Ca1 . 5_665 134.18(17)
C1 O2 Ca1 . . 84.27(16)
Ca1 O2 Ca1 5_665 . 105.19(7)
O1 C1 O2 . . 123.5(2)
O1 C1 C2 . . 117.8(2)
O2 C1 C2 . . 118.8(2)
O1 C1 Ca1 . . 54.78(13)
O2 C1 Ca1 . . 69.85(15)
C2 C1 Ca1 . . 166.44(18)
N1 C2 C3 . . 110.1(2)
N1 C2 C1 . . 107.6(2)
C3 C2 C1 . . 113.2(2)
N1 C2 H2 . . 108.6
C3 C2 H2 . . 108.6
C1 C2 H2 . . 108.6
C2 C3 H3A . . 109.5
C2 C3 H3B . . 109.5
H3A C3 H3B . . 109.5
C2 C3 H3C . . 109.5
H3A C3 H3C . . 109.5
H3B C3 H3C . . 109.5
C2 N1 H1A . . 111.4(17)
C2 N1 H1B . . 109.5(16)
H1A N1 H1B . . 107(2)
C2 N1 H1C . . 107.9(18)
H1A N1 H1C . . 110(2)
H1B N1 H1C . . 111(2)
Ca1 O1W H3E . . 119(2)
Ca1 O1W H3D . . 116(2)
H3E O1W H3D . . 115(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ca1 O2 7_566 2.3732(19)
Ca1 O2 5_665 2.3732(19)
Ca1 O1 3_655 2.3880(18)
Ca1 O1 . 2.3880(18)
Ca1 O1W . 2.410(2)
Ca1 O1W 3_655 2.410(2)
Ca1 O2 . 2.716(2)
Ca1 O2 3_655 2.716(2)
Ca1 C1 3_655 2.879(3)
Ca1 C1 . 2.879(3)
Ca1 Ca1 5_665 4.0479(12)
Ca1 Ca1 5_666 4.0479(12)
O1 C1 . 1.245(3)
O2 C1 . 1.263(3)
O2 Ca1 5_665 2.3732(19)
C1 C2 . 1.528(4)
C2 N1 . 1.489(3)
C2 C3 . 1.519(3)
C2 H2 . 1.0000
C3 H3A . 0.9800
C3 H3B . 0.9800
C3 H3C . 0.9800
N1 H1A . 0.922(17)
N1 H1B . 0.917(17)
N1 H1C . 0.927(17)
O1W H3E . 0.805(17)
O1W H3D . 0.825(17)
O2W H4 . 0.840(17)
