#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:53:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180453 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/22/7212214.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_7212214
loop_
_publ_author_name
'Xiao, Weiming'
'Chen, Chao'
'Deng, Shengjun'
'Mao, Xuejin'
'Sun, Bin'
'Zhang, Ning'
_publ_section_title
;
 Supramolecular assembly of [H(4−n)BPTC]n− with pipzH22+: 1D
 negatively charged rectangular tubes and a 2D neutral fes 4·82
 network
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              2011
_journal_paper_doi               10.1039/b922188c
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C20 H24 N2 O10'
_chemical_formula_sum            'C20 H24 N2 O10'
_chemical_formula_weight         452.41
_chemical_melting_point          ?
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.155(2)
_cell_angle_beta                 93.378(2)
_cell_angle_gamma                94.221(2)
_cell_formula_units_Z            1
_cell_length_a                   6.2017(9)
_cell_length_b                   8.3441(13)
_cell_length_c                   9.6508(14)
_cell_measurement_reflns_used    2409
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.45
_cell_volume                     497.04(13)
_computing_cell_refinement       Process-auto
_computing_data_collection       Process-auto
_computing_data_reduction        Process-auto
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       ω/2θ
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4756
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             238
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2409
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0966P)²+0.4355P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2184
_reflns_number_gt                1516
_reflns_number_total             2409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b922188c.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' 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 'none' 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      P-1
_cod_database_code               7212214
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
C1 C 0.7433(5) 0.1346(4) 0.5675(3) 0.0286(7) Uani 1 1 d .
C2 C 0.5989(5) 0.0442(4) 0.4760(3) 0.0255(6) Uani 1 1 d .
C3 C 0.6501(5) 0.0378(4) 0.3374(3) 0.0324(7) Uani 1 1 d .
C4 C 0.8370(5) 0.1194(4) 0.2961(3) 0.0319(7) Uani 1 1 d .
C5 C 0.9797(5) 0.2123(3) 0.3876(3) 0.0262(7) Uani 1 1 d .
C6 C 0.9313(5) 0.2203(3) 0.5285(3) 0.0261(7) Uani 1 1 d .
C7 C 1.0578(5) 0.3113(4) 0.6480(3) 0.0299(7) Uani 1 1 d .
C8 C 1.1718(5) 0.2930(4) 0.3190(3) 0.0324(7) Uani 1 1 d .
C9 C 0.5571(6) 0.3898(4) 0.8952(4) 0.0378(8) Uani 1 1 d .
C10 C 0.3051(6) 0.5791(5) 0.9726(4) 0.0381(8) Uani 1 1 d .
H1 H 0.874(6) 0.109(5) 0.198(4) 0.045(10) Uiso 1 1 d .
H2 H 0.559(6) -0.031(5) 0.266(4) 0.046(11) Uiso 1 1 d .
H3 H 0.706(5) 0.139(4) 0.661(4) 0.030(9) Uiso 1 1 d .
H4 H 1.249(9) 0.413(6) 0.513(3) 0.096(18) Uiso 1 1 d D
H5 H 0.232(7) 0.673(5) 0.952(4) 0.049(11) Uiso 1 1 d .
H6 H 0.209(7) 0.481(5) 0.975(4) 0.056(12) Uiso 1 1 d .
H7 H 0.643(7) 0.370(5) 0.824(5) 0.058(12) Uiso 1 1 d .
H8 H 0.447(6) 0.297(4) 0.903(4) 0.032(9) Uiso 1 1 d .
H9 H 0.354(5) 0.987(5) 0.017(4) 0.039 Uiso 1 1 d D
H10 H 0.196(6) 1.059(5) 0.107(4) 0.039 Uiso 1 1 d .
H11 H 0.535(7) 0.623(5) 0.840(4) 0.054(12) Uiso 1 1 d .
H12 H 0.341(8) 0.506(6) 0.771(5) 0.072(14) Uiso 1 1 d .
N1 N 0.4388(5) 0.5332(4) 0.8589(3) 0.0344(7) Uani 1 1 d .
O1 O 1.2108(4) 0.4160(3) 0.6220(3) 0.0489(8) Uani 1 1 d D
O2 O 1.0121(4) 0.2876(3) 0.7674(3) 0.0468(7) Uani 1 1 d .
O3 O 1.2027(4) 0.2567(3) 0.1978(3) 0.0482(7) Uani 1 1 d .
O4 O 1.2984(4) 0.4001(3) 0.3852(3) 0.0500(8) Uani 1 1 d .
O5 O 0.2295(10) 0.9471(6) 0.0632(5) 0.1211(19) Uani 1 1 d 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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 C1 C6 124.2(3) . .
C2 C1 H3 116(2) . .
C6 C1 H3 120(2) . .
C1 C2 C3 116.9(3) . .
C1 C2 C2 121.6(3) . 2_656
C3 C2 C2 121.5(3) . 2_656
C4 C3 C2 120.2(3) . .
C4 C3 H2 118(2) . .
C2 C3 H2 122(2) . .
C3 C4 C5 122.8(3) . .
C3 C4 H1 119(2) . .
C5 C4 H1 118(2) . .
C4 C5 C6 118.0(3) . .
C4 C5 C8 113.7(3) . .
C6 C5 C8 128.3(3) . .
C1 C6 C5 117.9(3) . .
C1 C6 C7 113.5(3) . .
C5 C6 C7 128.5(3) . .
O2 C7 O1 120.3(3) . .
O2 C7 C6 120.5(3) . .
O1 C7 C6 119.2(3) . .
O3 C8 O4 120.1(3) . .
O3 C8 C5 119.4(3) . .
O4 C8 C5 120.5(3) . .
N1 C9 C10 110.5(3) . 2_667
N1 C9 H7 107(3) . .
C10 C9 H7 110(3) 2_667 .
N1 C9 H8 108(2) . .
C10 C9 H8 112(2) 2_667 .
H7 C9 H8 110(3) . .
N1 C10 C9 110.5(3) . 2_667
N1 C10 H5 112(2) . .
C9 C10 H5 109(2) 2_667 .
N1 C10 H6 99(3) . .
C9 C10 H6 113(3) 2_667 .
H5 C10 H6 114(4) . .
C10 N1 C9 110.9(3) . .
C10 N1 H11 108(3) . .
C9 N1 H11 112(3) . .
C10 N1 H12 109(3) . .
C9 N1 H12 109(3) . .
H11 N1 H12 108(4) . .
C7 O1 H4 112(3) . .
C8 O4 H4 111(2) . .
H9 O5 H10 96(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.390(4) .
C1 C6 1.398(4) .
C1 H3 0.94(3) .
C2 C3 1.394(4) .
C2 C2 1.487(6) 2_656
C3 C4 1.384(4) .
C3 H2 1.00(4) .
C4 C5 1.394(4) .
C4 H1 0.99(4) .
C5 C6 1.411(4) .
C5 C8 1.518(4) .
C6 C7 1.514(4) .
C7 O2 1.220(4) .
C7 O1 1.281(4) .
C8 O3 1.231(4) .
C8 O4 1.280(4) .
C9 N1 1.486(5) .
C9 C10 1.501(5) 2_667
C9 H7 0.91(4) .
C9 H8 1.00(4) .
C10 N1 1.475(4) .
C10 C9 1.501(5) 2_667
C10 H5 0.95(4) .
C10 H6 0.98(4) .
N1 H11 0.95(4) .
N1 H12 1.02(5) .
O1 H4 1.10(2) .
O4 H4 1.29(2) .
O5 H9 0.957(19) .
O5 H10 1.06(4) .
