#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:50:34 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180451 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/20/7212066.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_7212066
loop_
_publ_author_name
'Basu, Tannistha'
'Mondal, Raju'
_publ_section_title
;
 Construction of first anion-assisted helix inside a helix network
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              366
_journal_paper_doi               10.1039/b919235m
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C11 H18 Cl2 N4 O8'
_chemical_formula_weight         405.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.7440(3)
_cell_length_b                   13.7417(3)
_cell_length_c                   16.8120(4)
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.36
_cell_volume                     3406.24(13)
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_collection       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47448
_diffrn_reflns_theta_full        30.62
_diffrn_reflns_theta_max         30.62
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.857938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.03 (Bruker, 2001), R(int)=0.0706 before correction'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         5200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0764P)²+2.6376P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                3863
_reflns_number_total             5200
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b919235m.txt
_cod_data_source_block           rm7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7212066
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cl2 Cl 0.23504(3) 0.46850(4) 0.14983(3) 0.02630(14) Uani 1 1 d .
N1 N 0.46187(12) 0.56247(12) 0.10793(10) 0.0218(3) Uani 1 1 d .
C2 C 0.57723(12) 0.65458(13) 0.14448(10) 0.0170(3) Uani 1 1 d .
C3 C 0.60998(13) 0.56471(14) 0.11950(11) 0.0198(4) Uani 1 1 d .
N3 N 0.57714(14) 0.97412(15) 0.08183(15) 0.0357(5) Uani 1 1 d .
C8 C 0.41156(13) 0.72341(15) 0.15408(12) 0.0233(4) Uani 1 1 d .
H8A H 0.3531 0.6967 0.1416 0.035 Uiso 1 1 calc R
H8B H 0.4218 0.7806 0.1225 0.035 Uiso 1 1 calc R
H8C H 0.4137 0.7403 0.2095 0.035 Uiso 1 1 calc R
C4 C 0.57689(14) 0.91541(15) 0.14559(13) 0.0265(4) Uani 1 1 d .
N2 N 0.53853(12) 0.51083(13) 0.09724(10) 0.0238(4) Uani 1 1 d .
C7 C 0.63145(13) 0.73972(14) 0.17331(12) 0.0198(4) Uani 1 1 d .
C5 C 0.61778(12) 0.82834(13) 0.12275(12) 0.0196(4) Uani 1 1 d .
O5 O 0.14406(11) 0.46853(13) 0.11801(11) 0.0388(4) Uani 1 1 d .
C9 C 0.70428(15) 0.52668(16) 0.11436(14) 0.0288(4) Uani 1 1 d .
H9A H 0.7032 0.4612 0.0944 0.043 Uiso 1 1 calc R
H9B H 0.7314 0.5274 0.1663 0.043 Uiso 1 1 calc R
H9C H 0.7391 0.5669 0.0791 0.043 Uiso 1 1 calc R
C6 C 0.64268(13) 0.84025(15) 0.04329(12) 0.0247(4) Uani 1 1 d .
C1 C 0.48281(12) 0.65035(14) 0.13655(11) 0.0182(4) Uani 1 1 d .
O6 O 0.29733(12) 0.47038(15) 0.08329(11) 0.0448(5) Uani 1 1 d .
N4 N 0.61717(13) 0.92929(15) 0.02085(13) 0.0338(5) Uani 1 1 d .
C11 C 0.69015(15) 0.7733(2) -0.01217(13) 0.0343(5) Uani 1 1 d .
H11A H 0.6968 0.8042 -0.0630 0.051 Uiso 1 1 calc R
H11B H 0.6554 0.7147 -0.0181 0.051 Uiso 1 1 calc R
H11C H 0.7489 0.7577 0.0088 0.051 Uiso 1 1 calc R
O7 O 0.24934(16) 0.55447(15) 0.19545(12) 0.0541(6) Uani 1 1 d .
O8 O 0.24743(14) 0.38461(15) 0.19700(14) 0.0582(6) Uani 1 1 d .
C10 C 0.53856(18) 0.94633(19) 0.22330(16) 0.0414(6) Uani 1 1 d .
H10A H 0.5153 1.0114 0.2188 0.062 Uiso 1 1 calc R
H10B H 0.5852 0.9446 0.2631 0.062 Uiso 1 1 calc R
H10C H 0.4904 0.9030 0.2382 0.062 Uiso 1 1 calc R
Cl1 Cl 0.05761(3) 0.24081(3) 0.40529(3) 0.02306(13) Uani 1 1 d .
O1 O 0.01124(14) 0.31780(12) 0.44753(12) 0.0427(5) Uani 1 1 d .
O2 O 0.13180(13) 0.28053(15) 0.36263(12) 0.0458(5) Uani 1 1 d .
O3 O -0.00414(15) 0.19211(17) 0.35333(12) 0.0545(6) Uani 1 1 d .
O4 O 0.08795(16) 0.17156(13) 0.46363(12) 0.0495(5) Uani 1 1 d .
H7A H 0.6174(19) 0.7516(19) 0.2271(17) 0.035(7) Uiso 1 1 d .
H7B H 0.6967(18) 0.7232(18) 0.1726(15) 0.027(6) Uiso 1 1 d .
H222 H 0.5372(19) 0.454(2) 0.0866(16) 0.031(7) Uiso 1 1 d .
H111 H 0.4112(18) 0.5358(18) 0.0981(15) 0.027(7) Uiso 1 1 d .
H444 H 0.626(2) 0.960(2) -0.020(2) 0.058(10) Uiso 1 1 d .
H333 H 0.567(2) 1.024(2) 0.075(2) 0.046(9) Uiso 1 1 d .
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O8 Cl2 O7 110.85(14)
O8 Cl2 O5 109.19(11)
O7 Cl2 O5 109.68(13)
O8 Cl2 O6 111.51(15)
O7 Cl2 O6 107.90(11)
O5 Cl2 O6 107.64(11)
C1 N1 N2 109.29(16)
C1 N1 H111 131.6(17)
N2 N1 H111 119.1(17)
C3 C2 C1 106.24(17)
C3 C2 C7 127.30(17)
C1 C2 C7 126.46(17)
N2 C3 C2 107.56(17)
N2 C3 C9 121.60(18)
C2 C3 C9 130.83(19)
N4 N3 C4 109.7(2)
N4 N3 H333 114(3)
C4 N3 H333 135(3)
C1 C8 H8A 109.5
C1 C8 H8B 109.5
H8A C8 H8B 109.5
C1 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
N3 C4 C5 107.2(2)
N3 C4 C10 122.1(2)
C5 C4 C10 130.7(2)
C3 N2 N1 109.34(16)
C3 N2 H222 128(2)
N1 N2 H222 122(2)
C2 C7 C5 112.30(16)
C2 C7 H7A 109.2(16)
C5 C7 H7A 112.0(16)
C2 C7 H7B 109.6(14)
C5 C7 H7B 108.1(15)
H7A C7 H7B 105(2)
C4 C5 C6 106.08(18)
C4 C5 C7 126.84(19)
C6 C5 C7 127.08(18)
C3 C9 H9A 109.5
C3 C9 H9B 109.5
H9A C9 H9B 109.5
C3 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
N4 C6 C5 107.7(2)
N4 C6 C11 121.6(2)
C5 C6 C11 130.7(2)
N1 C1 C2 107.56(17)
N1 C1 C8 121.32(17)
C2 C1 C8 131.12(18)
N3 N4 C6 109.3(2)
N3 N4 H444 119(2)
C6 N4 H444 132(2)
C6 C11 H11A 109.5
C6 C11 H11B 109.5
H11A C11 H11B 109.5
C6 C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
C4 C10 H10A 109.5
C4 C10 H10B 109.5
H10A C10 H10B 109.5
C4 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
O2 Cl1 O3 111.27(13)
O2 Cl1 O4 111.10(13)
O3 Cl1 O4 107.78(13)
O2 Cl1 O1 109.37(11)
O3 Cl1 O1 109.98(13)
O4 Cl1 O1 107.24(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cl2 O8 1.4112(19)
Cl2 O7 1.4242(19)
Cl2 O5 1.4441(17)
Cl2 O6 1.4477(18)
N1 C1 1.336(2)
N1 N2 1.347(2)
N1 H111 0.85(3)
C2 C3 1.391(3)
C2 C1 1.400(2)
C2 C7 1.498(3)
C3 N2 1.341(3)
C3 C9 1.488(3)
N3 N4 1.334(3)
N3 C4 1.342(3)
N3 H333 0.71(3)
C8 C1 1.483(3)
C8 H8A 0.9600
C8 H8B 0.9600
C8 H8C 0.9600
C4 C5 1.394(3)
C4 C10 1.486(3)
N2 H222 0.80(3)
C7 C5 1.499(3)
C7 H7A 0.94(3)
C7 H7B 0.99(3)
C5 C6 1.395(3)
C9 H9A 0.9600
C9 H9B 0.9600
C9 H9C 0.9600
C6 N4 1.334(3)
C6 C11 1.485(3)
N4 H444 0.82(3)
C11 H11A 0.9600
C11 H11B 0.9600
C11 H11C 0.9600
C10 H10A 0.9600
C10 H10B 0.9600
C10 H10C 0.9600
Cl1 O2 1.4173(18)
Cl1 O3 1.4283(19)
Cl1 O4 1.4379(18)
Cl1 O1 1.4461(17)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H111 O6 0.85(3) 1.92(3) 2.767(2) 176(3) .
N2 H222 O1 0.80(3) 1.99(3) 2.786(3) 169(3) 6_656
N3 H333 O4 0.71(3) 2.15(3) 2.823(3) 159(4) 6_666
N4 H444 O5 0.82(3) 1.94(4) 2.753(3) 178(4) 4_565
