#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/44/2214471.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_2214471
loop_
_publ_author_name
'Rong-Hua Zeng'
'Feng Sun'
'La-Sheng Jiang'
'You-Wen Tang'
'Zhan-Qiang Fang'
_publ_section_title
Bis(μ-3-amino-5-carboxybenzoato-κ²O:O')bis[(5-aminoisophthalato)triaquasodium(I)]
_journal_coeditor_code           ZL2034
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1813
_journal_page_last               m1814
_journal_paper_doi               10.1107/S1600536807026013
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Na2 (C8 H6 N O4)2 (C8 H7 N O4)2 (H2 O)6]'
_chemical_formula_moiety         'C32 H38 N4 Na2 O22'
_chemical_formula_sum            'C32 H38 N4 Na2 O22'
_chemical_formula_weight         876.64
_chemical_name_systematic
;
Bis(μ-3-amino-5-carboxybenzoato-κ²O:O')bis[(5-
aminoisophthalato)triaquasodium(I)]
;
_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           SHELXL97
_cell_angle_alpha                95.251(2)
_cell_angle_beta                 98.649(2)
_cell_angle_gamma                95.200(2)
_cell_formula_units_Z            1
_cell_length_a                   8.1889(3)
_cell_length_b                   8.8821(3)
_cell_length_c                   12.6381(5)
_cell_measurement_reflns_used    3500
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.66
_cell_volume                     899.86(6)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11809
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0382
_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)+(0.0543P)²+0.2242P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                2714
_reflns_number_total             3506
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            zl2034.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2214471
_cod_database_fobs_code          2214471
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_refinement_flags
_atom_site_occupancy
C C1 0.1175(2) 0.2786(2) 1.00350(14) 0.0251(4) Uani d . 1
C C2 0.0923(2) 0.16994(19) 1.08453(14) 0.0233(4) Uani d . 1
C C3 0.2264(2) 0.0955(2) 1.12436(14) 0.0253(4) Uani d . 1
H H3 0.3292 0.1168 1.1031 0.030 Uiso calc R 1
C C4 0.2060(2) -0.01048(19) 1.19577(14) 0.0241(4) Uani d . 1
C C5 0.0531(2) -0.04674(19) 1.22571(14) 0.0242(4) Uani d . 1
H H5 0.0403 -0.1214 1.2717 0.029 Uiso calc R 1
C C6 -0.0814(2) 0.02815(19) 1.18715(14) 0.0230(4) Uani d . 1
C C7 -0.0614(2) 0.13772(19) 1.11621(14) 0.0237(4) Uani d . 1
H H7 -0.1507 0.1890 1.0902 0.028 Uiso calc R 1
C C8 -0.2484(2) -0.0130(2) 1.22114(14) 0.0247(4) Uani d . 1
C C9 -0.0748(2) 0.5059(2) 0.74424(15) 0.0288(4) Uani d . 1
C C10 -0.0515(2) 0.60556(19) 0.65623(14) 0.0237(4) Uani d . 1
C C11 -0.1875(2) 0.6705(2) 0.60714(14) 0.0252(4) Uani d . 1
H H11 -0.2909 0.6513 0.6279 0.030 Uiso calc R 1
C C12 -0.1679(2) 0.76336(19) 0.52771(14) 0.0228(4) Uani d . 1
C C13 -0.0155(2) 0.79463(19) 0.49608(14) 0.0242(4) Uani d . 1
H H13 -0.0042 0.8585 0.4427 0.029 Uiso calc R 1
C C14 0.12133(19) 0.72997(19) 0.54466(14) 0.0234(4) Uani d . 1
C C15 0.1019(2) 0.63570(19) 0.62487(14) 0.0246(4) Uani d . 1
H H15 0.1930 0.5924 0.6578 0.030 Uiso calc R 1
C C16 0.2881(2) 0.7633(2) 0.50918(15) 0.0258(4) Uani d . 1
N N1 0.34825(17) -0.08917(17) 1.23537(13) 0.0293(4) Uani d . 1
H H1A 0.3487 -0.1741 1.1922 0.044 Uiso calc R 1
H H1B 0.3411 -0.1124 1.3017 0.044 Uiso calc R 1
H H1C 0.4417 -0.0291 1.2364 0.044 Uiso calc R 1
N N2 -0.31119(17) 0.83326(16) 0.47749(12) 0.0264(3) Uani d . 1
H H2A -0.4044 0.7823 0.4892 0.040 Uiso calc R 1
H H2B -0.3106 0.8305 0.4070 0.040 Uiso calc R 1
H H2C -0.3056 0.9294 0.5058 0.040 Uiso calc R 1
Na Na1 0.32524(8) 0.39379(8) 0.81767(6) 0.0301(2) Uani d . 1
O O1 0.25624(15) 0.31616(16) 0.98325(11) 0.0368(4) Uani d . 1
O O2 -0.01689(14) 0.32523(15) 0.95567(11) 0.0339(3) Uani d . 1
H H2 0.0044 0.3713 0.9052 0.051 Uiso calc R 1
O O3 -0.26498(14) -0.13253(14) 1.26574(11) 0.0322(3) Uani d . 1
O O4 -0.36025(15) 0.07342(15) 1.20278(12) 0.0395(4) Uani d . 1
O O5 0.05126(15) 0.45954(16) 0.79542(11) 0.0371(4) Uani d . 1
O O6 -0.21793(16) 0.4762(2) 0.76354(14) 0.0593(5) Uani d . 1
O O7 0.40436(15) 0.69099(17) 0.54356(12) 0.0427(4) Uani d . 1
O O8 0.30116(15) 0.86535(14) 0.44630(11) 0.0314(3) Uani d . 1
O O1W 0.41376(17) 0.65365(16) 0.88767(13) 0.0410(4) Uani d D 1
O O2W 0.44720(16) 0.44095(16) 0.66516(12) 0.0386(4) Uani d D 1
O O3W 0.60029(16) 0.34300(16) 0.89387(12) 0.0373(4) Uani d D 1
H H1W 0.394(2) 0.7293(17) 0.8580(17) 0.045 Uiso d D 1
H H4W 0.5484(12) 0.447(2) 0.6801(17) 0.045 Uiso d D 1
H H6W 0.618(2) 0.342(2) 0.9601(8) 0.045 Uiso d D 1
H H3W 0.430(2) 0.5095(19) 0.6268(16) 0.045 Uiso d D 1
H H2W 0.5147(12) 0.662(2) 0.9063(17) 0.045 Uiso d D 1
H H5W 0.678(2) 0.402(2) 0.8828(15) 0.045 Uiso d 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'
Na Na 0.0362 0.0249 '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_3
_geom_angle
_geom_angle_publ_flag
O1 C1 O2 . 123.59(16) ?
O1 C1 C2 . 121.24(15) ?
O2 C1 C2 . 115.14(14) ?
C3 C2 C7 . 120.26(15) ?
C3 C2 C1 . 117.75(15) ?
C7 C2 C1 . 121.93(15) ?
C4 C3 C2 . 119.41(15) ?
C4 C3 H3 . 120.3 ?
C2 C3 H3 . 120.3 ?
C3 C4 C5 . 121.02(15) ?
C3 C4 N1 . 118.45(14) ?
C5 C4 N1 . 120.47(15) ?
C4 C5 C6 . 119.98(15) ?
C4 C5 H5 . 120.0 ?
C6 C5 H5 . 120.0 ?
C5 C6 C7 . 119.47(15) ?
C5 C6 C8 . 119.25(15) ?
C7 C6 C8 . 121.27(15) ?
C2 C7 C6 . 119.81(16) ?
C2 C7 H7 . 120.1 ?
C6 C7 H7 . 120.1 ?
O3 C8 O4 . 124.40(16) ?
O3 C8 C6 . 117.05(15) ?
O4 C8 C6 . 118.55(15) ?
O6 C9 O5 . 123.50(16) ?
O6 C9 C10 . 118.04(15) ?
O5 C9 C10 . 118.45(15) ?
C15 C10 C11 . 119.60(15) ?
C15 C10 C9 . 121.63(15) ?
C11 C10 C9 . 118.76(15) ?
C12 C11 C10 . 119.53(15) ?
C12 C11 H11 . 120.2 ?
C10 C11 H11 . 120.2 ?
C11 C12 C13 . 121.37(15) ?
C11 C12 N2 . 119.21(14) ?
C13 C12 N2 . 119.40(15) ?
C12 C13 C14 . 119.52(15) ?
C12 C13 H13 . 120.2 ?
C14 C13 H13 . 120.2 ?
C15 C14 C13 . 119.26(15) ?
C15 C14 C16 . 121.28(15) ?
C13 C14 C16 . 119.45(15) ?
C10 C15 C14 . 120.72(15) ?
C10 C15 H15 . 119.6 ?
C14 C15 H15 . 119.6 ?
O7 C16 O8 . 123.72(15) ?
O7 C16 C14 . 118.79(15) ?
O8 C16 C14 . 117.48(15) ?
C4 N1 H1A . 109.5 ?
C4 N1 H1B . 109.5 ?
H1A N1 H1B . 109.5 ?
C4 N1 H1C . 109.5 ?
H1A N1 H1C . 109.5 ?
H1B N1 H1C . 109.5 ?
C12 N2 H2A . 109.5 ?
C12 N2 H2B . 109.5 ?
H2A N2 H2B . 109.5 ?
C12 N2 H2C . 109.5 ?
H2A N2 H2C . 109.5 ?
H2B N2 H2C . 109.5 ?
O5 Na1 O2W . 110.25(5) y
O5 Na1 O1 . 82.66(5) y
O2W Na1 O1 . 166.86(6) y
O5 Na1 O1W . 87.51(5) y
O2W Na1 O1W . 87.97(6) y
O1 Na1 O1W . 95.25(6) y
O5 Na1 O3W . 163.62(6) y
O2W Na1 O3W . 84.43(5) y
O1 Na1 O3W . 83.12(5) y
O1W Na1 O3W . 85.74(5) y
O5 Na1 O3 2_557 97.80(5) y
O2W Na1 O3 2_557 85.57(5) y
O1 Na1 O3 2_557 90.33(5) y
O1W Na1 O3 2_557 172.76(6) y
O3W Na1 O3 2_557 90.36(5) y
C1 O1 Na1 . 127.35(12) ?
C1 O2 H2 . 109.5 ?
C8 O3 Na1 2_557 128.48(12) ?
C9 O5 Na1 . 154.20(12) ?
Na1 O1W H1W . 127.1(16) ?
Na1 O1W H2W . 108.1(14) ?
H1W O1W H2W . 105.5(13) ?
Na1 O2W H4W . 110.2(15) ?
Na1 O2W H3W . 126.7(15) ?
H4W O2W H3W . 104.3(13) ?
Na1 O3W H6W . 115.8(15) ?
Na1 O3W H5W . 116.8(15) ?
H6W O3W H5W . 102.8(13) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.225(2) ?
C1 O2 . 1.295(2) ?
C1 C2 . 1.494(2) ?
C2 C3 . 1.387(2) ?
C2 C7 . 1.391(2) ?
C3 C4 . 1.378(2) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.381(2) ?
C4 N1 . 1.460(2) ?
C5 C6 . 1.387(2) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.397(2) ?
C6 C8 . 1.518(2) ?
C7 H7 . 0.9300 ?
C8 O3 . 1.253(2) ?
C8 O4 . 1.256(2) ?
C9 O6 . 1.242(2) ?
C9 O5 . 1.257(2) ?
C9 C10 . 1.507(2) ?
C10 C15 . 1.384(2) ?
C10 C11 . 1.390(2) ?
C11 C12 . 1.374(2) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.379(2) ?
C12 N2 . 1.465(2) ?
C13 C14 . 1.391(2) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.391(2) ?
C14 C16 . 1.513(2) ?
C15 H15 . 0.9300 ?
C16 O7 . 1.243(2) ?
C16 O8 . 1.267(2) ?
N1 H1A . 0.8900 ?
N1 H1B . 0.8900 ?
N1 H1C . 0.8900 ?
N2 H2A . 0.8900 ?
N2 H2B . 0.8900 ?
N2 H2C . 0.8900 ?
Na1 O5 . 2.3520(14) y
Na1 O2W . 2.3535(16) y
Na1 O1 . 2.3922(14) y
Na1 O1W . 2.4011(16) y
Na1 O3W . 2.4115(15) y
Na1 O3 2_557 2.4347(15) y
O2 H2 . 0.8200 ?
O3 Na1 2_557 2.4347(15) ?
O1W H1W . 0.816(9) ?
O1W H2W . 0.819(9) ?
O2W H4W . 0.818(9) ?
O2W H3W . 0.822(9) ?
O3W H6W . 0.829(9) ?
O3W H5W . 0.824(9) ?
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 O3W 2_657 0.89 1.89 2.763(2) 167.7
N1 H1B O8 1_546 0.89 1.93 2.810(2) 170.1
N1 H1C O4 1_655 0.89 1.91 2.7808(19) 165.3
N2 H2A O7 1_455 0.89 1.94 2.8221(18) 168.6
N2 H2A O8 1_455 0.89 2.58 3.1815(18) 125.6
N2 H2B O3 1_564 0.89 1.93 2.7981(19) 165.1
N2 H2C O8 2_576 0.89 1.86 2.750(2) 175.2
O2 H2 O5 . 0.82 1.73 2.5491(17) 177.0
O1W H1W O4 2_567 0.816(9) 2.002(10) 2.8150(19) 175(2)
O2W H4W O6 1_655 0.818(9) 2.024(11) 2.8128(19) 162(2)
O3W H6W O1W 2_667 0.829(9) 1.977(10) 2.778(2) 162(2)
O2W H3W O7 . 0.822(9) 2.013(10) 2.8322(19) 174(2)
