#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:22:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180335 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/04/7200445.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_7200445
loop_
_publ_author_name
'Koner, Rajesh'
'Goldberg, Israel'
_publ_section_title
;
 Supramolecular reactivity of naphthalene-1,4,5,8-tetracarboxylic acid
 towards transition metal ions: coordination polymers and discrete
 complexes with CuII, NiII and CoII
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              367
_journal_paper_doi               10.1039/b815885a
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C14 H24 Co Na2 O18, 2(H2 O)'
_chemical_formula_sum            'C14 H28 Co Na2 O20'
_chemical_formula_weight         621.27
_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                71.3400(12)
_cell_angle_beta                 75.4362(9)
_cell_angle_gamma                78.5850(11)
_cell_formula_units_Z            1
_cell_length_a                   7.1365(2)
_cell_length_b                   8.1576(2)
_cell_length_c                   11.0316(3)
_cell_measurement_reflns_used    2033
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.66
_cell_volume                     584.06(3)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. φ and ω 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6276
_diffrn_reflns_theta_full        28.15
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         2.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.8455
_exptl_absorpt_correction_T_min  0.7509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             321
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0405
_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)+(0.0453P)²+0.4913P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                2311
_reflns_number_total             2798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815885a.txt
_cod_data_source_block           Compound-5(ra4a)
_cod_database_code               7200445
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.0000 1.0000 0.01080(13) Uani 1 2 d S . .
Na2 Na -0.06227(13) -0.07920(11) 0.80251(9) 0.0146(2) Uani 1 1 d . . .
O3 O 0.5071(2) 0.20667(19) 0.82683(15) 0.0122(3) Uani 1 1 d . . .
C4 C 0.4837(3) 0.3715(3) 0.8098(2) 0.0112(4) Uani 1 1 d . . .
O5 O 0.4386(2) 0.4457(2) 0.89811(15) 0.0144(3) Uani 1 1 d . . .
C6 C 0.5346(3) 0.4779(3) 0.6691(2) 0.0109(4) Uani 1 1 d . . .
C7 C 0.6832(3) 0.5783(3) 0.6399(2) 0.0128(4) Uani 1 1 d . . .
H7 H 0.7282 0.5949 0.7086 0.015 Uiso 1 1 calc R . .
C8 C 0.2314(3) 0.3439(3) 0.4905(2) 0.0129(4) Uani 1 1 d . . .
H8 H 0.1303 0.2739 0.5091 0.015 Uiso 1 1 calc R . .
C9 C 0.4556(3) 0.4607(3) 0.5665(2) 0.0103(4) Uani 1 1 d . . .
C10 C 0.2925(3) 0.3680(3) 0.5919(2) 0.0113(4) Uani 1 1 d . . .
C11 C 0.1648(3) 0.3090(3) 0.7258(2) 0.0113(4) Uani 1 1 d . . .
O12 O 0.1256(2) 0.15330(19) 0.76490(15) 0.0131(3) Uani 1 1 d . . .
O13 O 0.1007(2) 0.4205(2) 0.78724(15) 0.0146(3) Uani 1 1 d . . .
O14 O -0.3809(2) -0.18073(19) 0.88907(15) 0.0131(3) Uani 1 1 d . . .
H14A H -0.4430 -0.1627 0.8242 0.016 Uiso 1 1 d R . .
H14B H -0.3999 -0.2842 0.9463 0.016 Uiso 1 1 d R . .
O15 O -0.2155(2) 0.01916(19) 0.99971(15) 0.0124(3) Uani 1 1 d . . .
H15A H -0.1763 -0.0512 1.0723 0.015 Uiso 1 1 d R . .
H15B H -0.1893 0.1244 0.9945 0.015 Uiso 1 1 d R . .
O16 O 0.1145(2) -0.3002(2) 0.96388(16) 0.0167(3) Uani 1 1 d . . .
H16A H 0.2130 -0.3765 0.9401 0.020 Uiso 1 1 d R . .
H16B H 0.0489 -0.3528 1.0421 0.020 Uiso 1 1 d R . .
O17 O 0.1270(2) -0.2318(2) 0.65945(16) 0.0175(4) Uani 1 1 d . . .
H17A H 0.1383 -0.2059 0.5733 0.021 Uiso 1 1 d R . .
H17B H 0.1263 -0.3459 0.6961 0.021 Uiso 1 1 d R . .
O18 O -0.2277(2) 0.0918(2) 0.61873(16) 0.0177(4) Uani 1 1 d . . .
H18A H -0.3117 0.1631 0.6607 0.021 Uiso 1 1 d R . .
H18B H -0.3081 0.0204 0.6195 0.021 Uiso 1 1 d R . .
O19 O 0.5653(2) 0.0818(2) 0.31362(16) 0.0169(3) Uani 1 1 d . . .
H19A H 0.6565 -0.0022 0.2927 0.020 Uiso 1 1 d R . .
H19B H 0.6210 0.1547 0.3293 0.020 Uiso 1 1 d R . .
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'
Co Co 0.3494 0.9721 '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'
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
_geom_angle_publ_flag
O15 Co1 O15 180.0 2_557 1_655 ?
O15 Co1 O3 90.27(6) 2_557 2_657 ?
O15 Co1 O3 89.73(6) 1_655 2_657 ?
O15 Co1 O3 89.73(6) 2_557 . ?
O15 Co1 O3 90.27(6) 1_655 . ?
O3 Co1 O3 180.0 2_657 . ?
O15 Co1 O14 93.23(6) 2_557 1_655 ?
O15 Co1 O14 86.78(6) 1_655 1_655 ?
O3 Co1 O14 89.76(6) 2_657 1_655 ?
O3 Co1 O14 90.24(6) . 1_655 ?
O15 Co1 O14 86.77(6) 2_557 2_557 ?
O15 Co1 O14 93.22(6) 1_655 2_557 ?
O3 Co1 O14 90.24(6) 2_657 2_557 ?
O3 Co1 O14 89.76(6) . 2_557 ?
O14 Co1 O14 179.999(1) 1_655 2_557 ?
O15 Co1 Na2 133.71(4) 2_557 1_655 ?
O15 Co1 Na2 46.30(4) 1_655 1_655 ?
O3 Co1 Na2 105.88(4) 2_657 1_655 ?
O3 Co1 Na2 74.12(4) . 1_655 ?
O14 Co1 Na2 45.21(4) 1_655 1_655 ?
O14 Co1 Na2 134.79(4) 2_557 1_655 ?
O15 Co1 Na2 46.29(4) 2_557 2_557 ?
O15 Co1 Na2 133.70(4) 1_655 2_557 ?
O3 Co1 Na2 74.12(4) 2_657 2_557 ?
O3 Co1 Na2 105.88(4) . 2_557 ?
O14 Co1 Na2 134.79(4) 1_655 2_557 ?
O14 Co1 Na2 45.21(4) 2_557 2_557 ?
Na2 Co1 Na2 179.999(2) 1_655 2_557 ?
O17 Na2 O12 102.25(6) . . ?
O17 Na2 O14 110.14(6) . . ?
O12 Na2 O14 145.79(6) . . ?
O17 Na2 O15 163.81(7) . . ?
O12 Na2 O15 80.19(5) . . ?
O14 Na2 O15 71.84(5) . . ?
O17 Na2 O16 83.52(6) . . ?
O12 Na2 O16 96.55(6) . . ?
O14 Na2 O16 97.68(6) . . ?
O15 Na2 O16 80.29(6) . . ?
O17 Na2 O18 85.88(6) . . ?
O12 Na2 O18 91.38(6) . . ?
O14 Na2 O18 80.51(6) . . ?
O15 Na2 O18 110.17(6) . . ?
O16 Na2 O18 167.90(6) . . ?
O17 Na2 Co1 148.43(5) . 1_455 ?
O12 Na2 Co1 108.28(4) . 1_455 ?
O14 Na2 Co1 38.38(4) . 1_455 ?
O15 Na2 Co1 37.05(4) . 1_455 ?
O16 Na2 Co1 100.52(4) . 1_455 ?
O18 Na2 Co1 85.55(4) . 1_455 ?
C4 O3 Co1 130.03(14) . . ?
O5 C4 O3 125.8(2) . . ?
O5 C4 C6 119.62(18) . . ?
O3 C4 C6 114.29(18) . . ?
C7 C6 C9 120.5(2) . . ?
C7 C6 C4 115.55(19) . . ?
C9 C6 C4 123.43(19) . . ?
C6 C7 C8 120.6(2) . 2_666 ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 2_666 . ?
C10 C8 C7 120.8(2) . 2_666 ?
C10 C8 H8 119.6 . . ?
C7 C8 H8 119.6 2_666 . ?
C10 C9 C9 118.8(2) . 2_666 ?
C10 C9 C6 122.68(19) . . ?
C9 C9 C6 118.5(2) 2_666 . ?
C8 C10 C9 120.49(19) . . ?
C8 C10 C11 115.88(19) . . ?
C9 C10 C11 123.30(19) . . ?
O13 C11 O12 125.2(2) . . ?
O13 C11 C10 117.04(18) . . ?
O12 C11 C10 117.67(18) . . ?
C11 O12 Na2 156.64(15) . . ?
Co1 O14 Na2 96.41(6) 1_455 . ?
Co1 O14 H14A 111.6 1_455 . ?
Na2 O14 H14A 110.1 . . ?
Co1 O14 H14B 104.2 1_455 . ?
Na2 O14 H14B 123.5 . . ?
H14A O14 H14B 109.9 . . ?
Co1 O15 Na2 96.66(6) 1_455 . ?
Co1 O15 H15A 112.3 1_455 . ?
Na2 O15 H15A 113.4 . . ?
Co1 O15 H15B 116.7 1_455 . ?
Na2 O15 H15B 114.1 . . ?
H15A O15 H15B 104.1 . . ?
Na2 O16 H16A 121.8 . . ?
Na2 O16 H16B 119.9 . . ?
H16A O16 H16B 107.9 . . ?
Na2 O17 H17A 128.9 . . ?
Na2 O17 H17B 110.3 . . ?
H17A O17 H17B 110.5 . . ?
Na2 O18 H18A 97.1 . . ?
Na2 O18 H18B 102.9 . . ?
H18A O18 H18B 100.1 . . ?
H19A O19 H19B 108.5 . . ?
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
Co1 O15 2.0660(15) 2_557 ?
Co1 O15 2.0660(15) 1_655 ?
Co1 O3 2.1020(15) 2_657 ?
Co1 O3 2.1021(15) . ?
Co1 O14 2.1281(14) 1_655 ?
Co1 O14 2.1282(14) 2_557 ?
Co1 Na2 3.4060(8) 1_655 ?
Co1 Na2 3.4061(8) 2_557 ?
Na2 O17 2.3204(17) . ?
Na2 O12 2.4062(17) . ?
Na2 O14 2.4325(18) . ?
Na2 O15 2.4790(17) . ?
Na2 O16 2.4872(19) . ?
Na2 O18 2.4884(19) . ?
Na2 Co1 3.4061(8) 1_455 ?
O3 C4 1.279(3) . ?
C4 O5 1.249(3) . ?
C4 C6 1.508(3) . ?
C6 C7 1.379(3) . ?
C6 C9 1.439(3) . ?
C7 C8 1.404(3) 2_666 ?
C7 H7 0.9500 . ?
C8 C10 1.378(3) . ?
C8 C7 1.404(3) 2_666 ?
C8 H8 0.9500 . ?
C9 C10 1.433(3) . ?
C9 C9 1.434(4) 2_666 ?
C10 C11 1.511(3) . ?
C11 O13 1.253(3) . ?
C11 O12 1.268(3) . ?
O14 Co1 2.1282(14) 1_455 ?
O14 H14A 0.8928 . ?
O14 H14B 0.8890 . ?
O15 Co1 2.0660(15) 1_455 ?
O15 H15A 0.8965 . ?
O15 H15B 0.8954 . ?
O16 H16A 0.8881 . ?
O16 H16B 0.8875 . ?
O17 H17A 0.8912 . ?
O17 H17B 0.8888 . ?
O18 H18A 0.8979 . ?
O18 H18B 0.8919 . ?
O19 H19A 0.8917 . ?
O19 H19B 0.8577 . ?
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
O14 H14A O19 0.89 1.82 2.699(2) 168.9 2_556
O14 H14B O5 0.89 1.79 2.640(2) 158.4 2_557
O15 H15A O12 0.90 1.82 2.698(2) 166.8 2_557
O15 H15B O16 0.90 1.84 2.707(2) 161.1 2_557
O16 H16A O5 0.89 2.01 2.897(2) 176.4 1_545
O16 H16B O13 0.89 1.88 2.759(2) 168.8 2_557
O17 H17A O18 0.89 2.01 2.866(2) 159.6 2_556
O17 H17B O13 0.89 1.87 2.754(2) 173.5 1_545
O18 H18A O3 0.90 2.05 2.867(2) 150.7 1_455
O18 H18B O19 0.89 2.03 2.853(2) 151.9 2_556
O19 H19A O12 0.89 1.89 2.779(2) 171.3 2_656
O19 H19B O17 0.86 2.06 2.834(2) 149.2 2_656
