#------------------------------------------------------------------------------
#$Date: 2018-05-15 18:58:00 +0300 (Tue, 15 May 2018) $
#$Revision: 207789 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/94/1549412.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_1549412
loop_
_publ_author_name
'Yang, Annabeth P.'
'LaDuca, Robert L.'
_publ_contact_author             'LaDuca, Robert L.'
_publ_section_title
;
 Poly[diaquabis(μ-hydrogen
 benzene-1,2,4-tricarboxylato)copper(II)disodium]: a novel 4,5,6-connected
 trinodal net
;
_journal_coeditor_code           LH4034
_journal_issue                   5
_journal_name_full               IUCrData
_journal_page_first              x180676
_journal_paper_doi               10.1107/S2414314618006764
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac          '[Cu Na2 (C9 H4 O6)2 (H2 O)4]'
_chemical_formula_moiety         'C18 H16 Cu Na2 O16'
_chemical_formula_sum            'C18 H16 Cu Na2 O16'
_chemical_formula_weight         597.83
_chemical_name_systematic
;
Poly[diaquabis(μ-hydrogen benzene-1,2,4-tricarboxylato)copper(II)disodium]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
 Olex2 1.2 (compiled
 2017.03.02 svn.r3394 for
 OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                105.071(2)
_cell_angle_beta                 93.073(2)
_cell_angle_gamma                109.955(2)
_cell_formula_units_Z            1
_cell_length_a                   6.9048(9)
_cell_length_b                   7.0555(9)
_cell_length_c                   11.8449(15)
_cell_measurement_reflns_used    2453
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      3.18
_cell_volume                     517.26(12)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
COSMO (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
Crystal Maker (Palmer, 2018)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b) within OLEX2 (Dolomanov et al.,
2009)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4640
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             301
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1906
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0395
_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)+(0.0511P)²+0.2450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                1606
_reflns_number_total             1906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            lh4034sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        517.26(11)
_cod_database_code               1549412
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-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_occupancy
Cu Cu1 0.0000 0.5000 0.0000 0.01725(19) Uani d 1
Na Na1 0.38930(19) 0.8360(2) 0.87662(11) 0.0247(3) Uani d 1
O O1 0.2019(3) 0.5155(3) 0.12631(18) 0.0188(5) Uani d 1
O O2 0.4758(4) 0.7631(4) 0.09054(19) 0.0265(6) Uani d 1
O O3 0.8109(3) 0.5155(3) 0.11767(18) 0.0181(5) Uani d 1
O O4 0.9730(4) 0.8616(4) 0.1695(2) 0.0322(6) Uani d 1
O O5 0.4966(4) 0.7908(4) 0.68605(19) 0.0248(6) Uani d 1
O O6 0.2072(4) 0.7132(4) 0.5602(2) 0.0242(6) Uani d 1
H H6 0.167(7) 0.722(7) 0.614(4) 0.039(13) Uiso d 1
O O7 0.0503(4) 0.7544(5) 0.7571(2) 0.0221(6) Uani d 1
H H7A 0.032(6) 0.846(6) 0.770(3) 0.021(12) Uiso d 1
H H7B -0.036(7) 0.673(7) 0.783(4) 0.038(12) Uiso d 1
O O8 0.7418(4) 0.9752(4) 0.9649(2) 0.0264(6) Uani d 1
H H8A 0.836(5) 1.038(5) 0.931(3) 0.028 Uiso d 1
H H8B 0.770(5) 0.877(4) 0.973(3) 0.028 Uiso d 1
C C1 0.5084(5) 0.6815(5) 0.2697(3) 0.0143(6) Uani d 1
C C2 0.7216(5) 0.7167(5) 0.2844(3) 0.0162(7) Uani d 1
C C3 0.8280(5) 0.7616(5) 0.3969(3) 0.0188(7) Uani d 1
H H3 0.965(6) 0.780(5) 0.411(3) 0.020(9) Uiso d 1
C C4 0.7268(5) 0.7724(5) 0.4942(3) 0.0192(7) Uani d 1
H H4 0.806(5) 0.811(5) 0.574(3) 0.027(10) Uiso d 1
C C5 0.5150(5) 0.7383(5) 0.4802(3) 0.0166(7) Uani d 1
C C6 0.4076(5) 0.6917(5) 0.3678(3) 0.0170(7) Uani d 1
H H6A 0.259(5) 0.667(5) 0.358(2) 0.011(8) Uiso d 1
C C7 0.3906(5) 0.6523(5) 0.1510(3) 0.0170(7) Uani d 1
C C8 0.8432(5) 0.7000(5) 0.1818(3) 0.0168(7) Uani d 1
C C9 0.4075(5) 0.7501(5) 0.5861(3) 0.0185(7) Uani 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'
Cu Cu 0.3201 1.2651 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cu1 O1 . 2_565 180.0 y
O1 Cu1 O3 2_565 2_665 87.13(9) y
O1 Cu1 O3 2_565 1_455 92.88(9) y
O1 Cu1 O3 . 2_665 92.87(9) y
O1 Cu1 O3 . 1_455 87.13(9) y
O3 Cu1 O3 2_665 1_455 180.00(14) y
O3 Na1 O2 2_666 2_676 162.81(9) y
O3 Na1 O7 2_666 . 77.27(10) y
O5 Na1 O2 . 2_676 89.20(8) y
O5 Na1 O3 . 2_666 105.37(9) y
O5 Na1 O7 . . 81.70(9) y
O5 Na1 O8 . 2_677 150.41(10) y
O7 Na1 O2 . 2_676 96.31(10) y
O8 Na1 O2 2_677 2_676 66.08(9) y
O8 Na1 O2 . 2_676 72.51(9) y
O8 Na1 O3 . 2_666 115.87(9) y
O8 Na1 O3 2_677 2_666 97.25(9) y
O8 Na1 O5 . . 89.37(9) y
O8 Na1 O7 . . 165.87(11) y
O8 Na1 O7 2_677 . 85.02(9) y
O8 Na1 O8 . 2_677 97.79(8) y
C7 O1 Cu1 . . 122.27(19) ?
Na1 O2 Na1 2_676 1_554 71.48(7) ?
C7 O2 Na1 . 2_676 132.9(2) ?
C7 O2 Na1 . 1_554 139.5(2) ?
Cu1 O3 Na1 1_655 2_666 109.41(9) ?
C8 O3 Cu1 . 1_655 114.38(19) ?
C8 O3 Na1 . 2_666 135.22(19) ?
C9 O5 Na1 . . 133.8(2) ?
C9 O6 H6 . . 107(4) ?
Na1 O7 H7A . . 106(3) ?
Na1 O7 H7B . . 106(3) ?
H7A O7 H7B . . 107(4) ?
Na1 O8 Na1 . 2_677 82.21(8) ?
Na1 O8 H8A 2_677 . 122(2) ?
Na1 O8 H8A . . 121(3) ?
Na1 O8 H8B . . 107(3) ?
Na1 O8 H8B 2_677 . 118(3) ?
H8A O8 H8B . . 105(3) ?
C2 C1 C7 . . 121.4(3) ?
C6 C1 C2 . . 119.1(3) ?
C6 C1 C7 . . 119.3(3) ?
C1 C2 C8 . . 122.9(3) ?
C3 C2 C1 . . 119.5(3) ?
C3 C2 C8 . . 117.5(3) ?
C2 C3 H3 . . 123(2) ?
C4 C3 C2 . . 121.0(3) ?
C4 C3 H3 . . 116(2) ?
C3 C4 H4 . . 120(2) ?
C3 C4 C5 . . 119.8(3) ?
C5 C4 H4 . . 120(2) ?
C4 C5 C9 . . 119.2(3) ?
C6 C5 C4 . . 119.4(3) ?
C6 C5 C9 . . 121.3(3) ?
C1 C6 C5 . . 121.1(3) ?
C1 C6 H6A . . 119.4(17) ?
C5 C6 H6A . . 119.5(17) ?
O1 C7 C1 . . 115.1(3) ?
O2 C7 O1 . . 126.2(3) ?
O2 C7 C1 . . 118.6(3) ?
O3 C8 C2 . . 116.0(3) ?
O4 C8 O3 . . 124.3(3) ?
O4 C8 C2 . . 119.6(3) ?
O5 C9 O6 . . 123.9(3) ?
O5 C9 C5 . . 123.1(3) ?
O6 C9 C5 . . 113.0(3) ?
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
Cu1 O1 . 1.944(2) y
Cu1 O1 2_565 1.944(2) y
Cu1 O3 1_455 1.9681(19) y
Cu1 O3 2_665 1.9681(19) y
Na1 O2 2_676 2.571(3) y
Na1 O3 2_666 2.413(3) y
Na1 O5 . 2.390(2) y
Na1 O7 . 2.473(3) y
Na1 O8 . 2.354(3) y
Na1 O8 2_677 2.413(3) y
O1 C7 . 1.292(4) ?
O2 Na1 1_554 2.787(3) ?
O2 Na1 2_676 2.571(3) ?
O2 C7 . 1.222(4) ?
O3 Cu1 1_655 1.9681(19) ?
O3 Na1 2_666 2.413(3) ?
O3 C8 . 1.261(4) ?
O4 C8 . 1.236(4) ?
O5 C9 . 1.219(4) ?
O6 H6 . 0.70(4) ?
O6 C9 . 1.320(4) ?
O7 H7A . 0.68(4) ?
O7 H7B . 0.81(5) ?
O8 Na1 2_677 2.413(3) ?
O8 H8A . 0.842(18) ?
O8 H8B . 0.808(18) ?
C1 C2 . 1.400(4) ?
C1 C6 . 1.385(4) ?
C1 C7 . 1.514(4) ?
C2 C3 . 1.389(4) ?
C2 C8 . 1.516(4) ?
C3 H3 . 0.91(4) ?
C3 C4 . 1.379(4) ?
C4 H4 . 0.99(4) ?
C4 C5 . 1.392(4) ?
C5 C6 . 1.390(4) ?
C5 C9 . 1.489(4) ?
C6 H6A . 0.98(3) ?
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
_geom_hbond_publ_flag
O6 H6 O7 . 0.70(4) 1.91(4) 2.613(3) 177(5) y
O7 H7A O4 2_676 0.68(4) 2.01(4) 2.685(4) 169(4) y
O7 H7B O1 2_566 0.81(5) 2.02(5) 2.816(4) 168(4) y
O8 H8A O4 2_776 0.842(18) 1.902(19) 2.736(3) 170(4) y
O8 H8B O2 1_556 0.808(18) 2.54(3) 2.720(3) 94(3) y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
Cu1 Na1 O5 C9 1_556 . 59.0(3)
Cu1 Na1 O8 Na1 1_556 2_677 -66.87(8)
Cu1 O1 C7 O2 . . -12.0(4)
Cu1 O1 C7 C1 . . 164.65(18)
Cu1 O3 C8 O4 1_655 . 4.1(4)
Cu1 O3 C8 C2 1_655 . -171.8(2)
Na1 Cu1 O1 C7 1_554 . 12.9(2)
Na1 Cu1 O1 C7 2_566 . -167.1(2)
Na1 Na1 O5 C9 2_677 . -138.8(3)
Na1 O2 C7 O1 2_676 . 114.2(3)
Na1 O2 C7 O1 1_554 . -0.6(5)
Na1 O2 C7 C1 2_676 . -62.4(4)
Na1 O2 C7 C1 1_554 . -177.12(19)
Na1 O3 C8 O4 2_666 . 171.2(2)
Na1 O3 C8 C2 2_666 . -4.7(4)
Na1 O5 C9 O6 . . -2.0(5)
Na1 O5 C9 C5 . . 177.6(2)
O1 Cu1 O1 C7 2_565 . 23(9)
O2 Na1 O5 C9 1_556 . 146.4(3)
O2 Na1 O5 C9 2_676 . -95.6(3)
O2 Na1 O8 Na1 2_676 2_677 61.83(8)
O2 Na1 O8 Na1 1_556 2_677 -60.30(8)
O3 Cu1 O1 C7 2_665 . 52.4(2)
O3 Cu1 O1 C7 1_455 . -127.6(2)
O3 Na1 O5 C9 2_666 . 75.2(3)
O3 Na1 O8 Na1 2_666 2_677 -102.00(10)
O5 Na1 O8 Na1 . 2_677 151.19(10)
O7 Na1 O5 C9 . . 0.9(3)
O7 Na1 O8 Na1 . 2_677 100.6(4)
O8 Na1 O5 C9 . . -168.1(3)
O8 Na1 O5 C9 2_677 . -63.3(4)
O8 Na1 O8 Na1 2_677 2_677 0.0
C1 C2 C3 C4 . . -0.1(5)
C1 C2 C8 O3 . . -74.2(4)
C1 C2 C8 O4 . . 109.7(4)
C2 C1 C6 C5 . . 0.7(5)
C2 C1 C7 O1 . . 143.0(3)
C2 C1 C7 O2 . . -40.1(4)
C2 C3 C4 C5 . . -0.1(5)
C3 C2 C8 O3 . . 103.4(3)
C3 C2 C8 O4 . . -72.7(4)
C3 C4 C5 C6 . . 0.6(5)
C3 C4 C5 C9 . . 179.9(3)
C4 C5 C6 C1 . . -1.0(5)
C4 C5 C9 O5 . . 0.8(5)
C4 C5 C9 O6 . . -179.6(3)
C6 C1 C2 C3 . . -0.2(4)
C6 C1 C2 C8 . . 177.4(3)
C6 C1 C7 O1 . . -42.6(4)
C6 C1 C7 O2 . . 134.3(3)
C6 C5 C9 O5 . . -179.9(3)
C6 C5 C9 O6 . . -0.3(4)
C7 C1 C2 C3 . . 174.2(3)
C7 C1 C2 C8 . . -8.2(4)
C7 C1 C6 C5 . . -173.8(3)
C8 C2 C3 C4 . . -177.8(3)
C9 C5 C6 C1 . . 179.8(3)

_cod_database_fobs_code 1549412
