#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:55:42 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180363 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/32/7203231.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_7203231
loop_
_publ_author_name
'Oscar Fabelo'
'Laura Cañadillas-Delgado'
'Jorge Pasán'
'Catalina Ruiz-Pérez'
'Miguel Julve'
_publ_section_title
;
 Influence of the presence of divalent first-row transition metal ions
 on the structure of sodium(<small>I</small>) salts of
 1,2,3,4-benzenetetracarboxylic acid (H<small>₄</small>bta)
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              338
_journal_paper_doi               10.1039/b516806f
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C20 H28 Mn Na2 O26'
_chemical_formula_weight         785.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.466(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3778(4)
_cell_length_b                   20.1493(6)
_cell_length_c                   10.4963(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1517.46(12)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3703
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         5.29
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.98
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0230
_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)+(0.0392P)²+0.6374P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0642
_reflns_number_gt                1051
_reflns_number_total             1115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b516806f.txt
_cod_data_source_block           COMPOUND2
_cod_original_cell_volume        1517.46(11)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7203231
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn01 Mn 0.5000 0.5000 0.0000 0.02255(18) Uani 1 4 d S . .
Na1 Na 0.81907(12) 0.5000 0.32904(8) 0.0335(3) Uani 1 2 d S . .
C1 C 1.0000 0.68708(11) 0.5000 0.0206(5) Uani 1 2 d S . .
C2 C 0.89696(18) 0.71889(7) 0.38969(13) 0.0200(3) Uani 1 1 d . . .
C3 C 0.89691(18) 0.78888(7) 0.38962(13) 0.0194(3) Uani 1 1 d . . .
C4 C 1.0000 0.82045(11) 0.5000 0.0199(4) Uani 1 2 d S . .
C5 C 0.79634(19) 0.83573(8) 0.28282(14) 0.0239(4) Uani 1 1 d . . .
C6 C 0.7958(2) 0.67128(8) 0.28416(14) 0.0262(4) Uani 1 1 d . . .
O1W O 0.5000 0.39484(8) 0.0000 0.0369(4) Uani 1 2 d S . .
O2W O 0.4718(3) 0.5000 0.20455(16) 0.0334(4) Uani 1 2 d S . .
O3W O 0.1977(2) 0.5000 -0.08794(15) 0.0292(4) Uani 1 2 d S . .
O4W O 0.5000 0.90288(8) 0.0000 0.0305(4) Uani 1 2 d S . .
O5W O 1.1657(3) 0.5000 0.43590(19) 0.0457(5) Uani 1 2 d S . .
O1 O 0.70336(19) 0.81249(6) 0.17551(11) 0.0477(4) Uani 1 1 d . . .
O2 O 0.80807(15) 0.89580(6) 0.30398(10) 0.0328(3) Uani 1 1 d . . .
O3 O 0.70201(19) 0.69423(7) 0.17501(11) 0.0495(4) Uani 1 1 d . . .
O4 O 0.80460(17) 0.61216(6) 0.30505(12) 0.0446(4) Uani 1 1 d . . .
H1 H 1.0000 0.8646(12) 0.5000 0.022(6) Uiso 1 2 d S . .
H2 H 1.0000 0.6433(12) 0.5000 0.023(6) Uiso 1 2 d S . .
H3 H 0.699(4) 0.7484(15) 0.177(3) 0.091(9) Uiso 1 1 d . . .
H4 H 1.211(4) 0.4685(12) 0.409(3) 0.085(9) Uiso 1 1 d . . .
H5 H 0.419(3) 0.4694(10) 0.2254(19) 0.053(6) Uiso 1 1 d . . .
H6 H 0.439(3) 0.3677(10) -0.053(2) 0.067(7) Uiso 1 1 d . . .
H7 H 0.142(3) 0.4683(9) -0.0680(19) 0.045(6) Uiso 1 1 d . . .
H8 H 0.564(3) 0.8755(11) 0.054(2) 0.069(7) 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'
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'
Mn Mn 0.3368 0.7283 '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
_geom_angle_publ_flag
O1W Mn01 O1W 180.0 5_665 . ?
O1W Mn01 O2W 90.0 5_665 . ?
O1W Mn01 O2W 90.0 . . ?
O1W Mn01 O2W 90.0 5_665 5_665 ?
O1W Mn01 O2W 90.0 . 5_665 ?
O2W Mn01 O2W 180.0 . 5_665 ?
O1W Mn01 O3W 90.0 5_665 . ?
O1W Mn01 O3W 90.0 . . ?
O2W Mn01 O3W 95.28(7) . . ?
O2W Mn01 O3W 84.72(7) 5_665 . ?
O1W Mn01 O3W 90.0 5_665 5_665 ?
O1W Mn01 O3W 90.0 . 5_665 ?
O2W Mn01 O3W 84.72(7) . 5_665 ?
O2W Mn01 O3W 95.28(7) 5_665 5_665 ?
O3W Mn01 O3W 180.0 . 5_665 ?
O1W Mn01 Na1 90.0 5_665 . ?
O1W Mn01 Na1 90.0 . . ?
O2W Mn01 Na1 43.50(5) . . ?
O2W Mn01 Na1 136.50(5) 5_665 . ?
O3W Mn01 Na1 138.78(4) . . ?
O3W Mn01 Na1 41.22(4) 5_665 . ?
O1W Mn01 Na1 90.0 5_665 5_665 ?
O1W Mn01 Na1 90.0 . 5_665 ?
O2W Mn01 Na1 136.50(5) . 5_665 ?
O2W Mn01 Na1 43.50(5) 5_665 5_665 ?
O3W Mn01 Na1 41.22(4) . 5_665 ?
O3W Mn01 Na1 138.78(4) 5_665 5_665 ?
Na1 Mn01 Na1 180.0 . 5_665 ?
O4 Na1 O4 167.40(7) . 6_565 ?
O4 Na1 O5W 95.84(4) . 5_766 ?
O4 Na1 O5W 95.84(4) 6_565 5_766 ?
O4 Na1 O3W 84.15(4) . 5_665 ?
O4 Na1 O3W 84.15(4) 6_565 5_665 ?
O5W Na1 O3W 179.82(7) 5_766 5_665 ?
O4 Na1 O5W 93.75(4) . . ?
O4 Na1 O5W 93.75(4) 6_565 . ?
O5W Na1 O5W 75.48(7) 5_766 . ?
O3W Na1 O5W 104.70(6) 5_665 . ?
O4 Na1 O2W 85.91(4) . . ?
O4 Na1 O2W 85.91(4) 6_565 . ?
O5W Na1 O2W 108.48(7) 5_766 . ?
O3W Na1 O2W 71.34(6) 5_665 . ?
O5W Na1 O2W 176.04(6) . . ?
O4 Na1 Mn01 83.88(3) . . ?
O4 Na1 Mn01 83.88(3) 6_565 . ?
O5W Na1 Mn01 144.33(6) 5_766 . ?
O3W Na1 Mn01 35.49(4) 5_665 . ?
O5W Na1 Mn01 140.18(5) . . ?
O2W Na1 Mn01 35.86(4) . . ?
O4 Na1 Na1 96.04(3) . 5_766 ?
O4 Na1 Na1 96.04(3) 6_565 5_766 ?
O5W Na1 Na1 38.62(5) 5_766 5_766 ?
O3W Na1 Na1 141.56(5) 5_665 5_766 ?
O5W Na1 Na1 36.87(4) . 5_766 ?
O2W Na1 Na1 147.09(5) . 5_766 ?
Mn01 Na1 Na1 177.05(4) . 5_766 ?
C2 C1 C2 124.9(2) 2_756 . ?
C1 C2 C3 117.59(14) . . ?
C1 C2 C6 113.38(15) . . ?
C3 C2 C6 129.02(13) . . ?
C4 C3 C2 117.34(13) . . ?
C4 C3 C5 114.24(14) . . ?
C2 C3 C5 128.42(12) . . ?
C3 C4 C3 125.3(2) . 2_756 ?
O2 C5 O1 121.74(14) . . ?
O2 C5 C3 118.44(13) . . ?
O1 C5 C3 119.82(14) . . ?
O4 C6 O3 120.87(14) . . ?
O4 C6 C2 119.46(14) . . ?
O3 C6 C2 119.66(14) . . ?
Mn01 O2W Na1 100.64(7) . . ?
Mn01 O3W Na1 103.29(6) . 5_665 ?
Na1 O5W Na1 104.52(7) 5_766 . ?
C6 O4 Na1 176.00(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn01 O1W 2.1189(17) 5_665 ?
Mn01 O1W 2.1189(17) . ?
Mn01 O2W 2.2047(16) . ?
Mn01 O2W 2.2047(16) 5_665 ?
Mn01 O3W 2.2064(15) . ?
Mn01 O3W 2.2064(15) 5_665 ?
Mn01 Na1 3.6990(9) . ?
Mn01 Na1 3.6990(9) 5_665 ?
Na1 O4 2.2736(12) . ?
Na1 O4 2.2736(12) 6_565 ?
Na1 O5W 2.444(2) 5_766 ?
Na1 O3W 2.5048(18) 5_665 ?
Na1 O5W 2.542(2) . ?
Na1 O2W 2.591(2) . ?
Na1 Na1 3.9428(17) 5_766 ?
C1 C2 1.3855(18) 2_756 ?
C1 C2 1.3855(18) . ?
C2 C3 1.410(2) . ?
C2 C6 1.523(2) . ?
C3 C4 1.3839(18) . ?
C3 C5 1.520(2) . ?
C4 C3 1.3839(18) 2_756 ?
C5 O2 1.2300(19) . ?
C5 O1 1.2644(19) . ?
C6 O4 1.210(2) . ?
C6 O3 1.2791(19) . ?
O3W Na1 2.5048(18) 5_665 ?
O5W Na1 2.444(2) 5_766 ?
