#------------------------------------------------------------------------------
#$Date: 2017-01-21 04:01:30 +0200 (Sat, 21 Jan 2017) $
#$Revision: 190798 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/20/2242031.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_2242031
loop_
_publ_author_name
'van der Horn, Jitschaq A.'
'Lutz, Martin'
_publ_section_title
;
 Crystal structure of
 catena-poly[[copper(II)-μ₂-salicylato-[diaquacopper(II)]-μ₂-salicylato]
 dihydrate]
;
_journal_coeditor_code           WM5360
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              235
_journal_page_last               238
_journal_paper_doi               10.1107/S2056989017000883
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Cu2 (C7 H4 O3)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C14 H12 Cu2 O8, 2(H2 O)'
_chemical_formula_sum            'C14 H16 Cu2 O10'
_chemical_formula_weight         471.34
_chemical_name_systematic
'catena-Poly[[copper(II)-μ₂-salicylato-[diaquacopper(II)]-μ₂-salicylato] dihydrate]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5028(17)
_cell_length_b                   5.0553(4)
_cell_length_c                   15.7573(13)
_cell_measurement_reflns_used    6768
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.07
_cell_volume                     1553.6(2)
_computing_cell_refinement
;
PEAKREF (Schreurs, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
Eval15 (Schreurs et al.,  2010) and SADABS (Sheldrick,
2014)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and DRAWxtl (Finger et al.,
2007)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14169
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.088
_exptl_absorpt_coefficient_mu    2.795
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2014)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.584
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0424P)²+2.4851P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                1186
_reflns_number_total             1799
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5360sup1.cif
_cod_data_source_block           I
_cod_database_code               2242031
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
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 0.500000 0.18416(12) 0.250000 0.01968(19) Uani d 1
Cu Cu2 0.500000 0.000000 0.500000 0.00951(16) Uani d 1
O O1 0.56220(14) 0.4466(5) 0.30330(15) 0.0123(6) Uani d 1
O O2 0.52168(14) 0.1699(5) 0.39545(15) 0.0124(6) Uani d 1
O O3 0.55744(13) 0.2318(5) 0.56341(15) 0.0116(6) Uani d 1
C C1 0.56041(19) 0.3678(7) 0.3812(2) 0.0091(7) Uani d 1
C C2 0.60045(18) 0.4988(7) 0.4466(2) 0.0087(7) Uani d 1
C C3 0.59722(19) 0.4210(7) 0.5328(2) 0.0095(7) Uani d 1
C C4 0.6396(2) 0.5632(7) 0.5908(2) 0.0139(8) Uani d 1
H H4 0.639097 0.515779 0.649085 0.017 Uiso calc 1
C C5 0.6809(2) 0.7660(8) 0.5647(2) 0.0135(8) Uani d 1
H H5 0.708139 0.857335 0.605141 0.016 Uiso calc 1
C C6 0.6837(2) 0.8409(7) 0.4794(2) 0.0128(8) Uani d 1
H H6 0.712306 0.982514 0.461553 0.015 Uiso calc 1
C C7 0.64451(19) 0.7064(7) 0.4224(2) 0.0117(8) Uani d 1
H H7 0.646947 0.754349 0.364212 0.014 Uiso calc 1
O O4 0.57447(14) -0.0767(5) 0.22503(15) 0.0121(6) Uani d 1
H H4A 0.568654 -0.200793 0.252177 0.018 Uiso d 1
H H4B 0.571466 -0.118039 0.180993 0.018 Uiso d 1
O O5 0.71893(16) 0.1128(6) 0.2774(2) 0.0314(8) Uani d 1
H H5A 0.730462 0.264763 0.277138 0.047 Uiso d 1
H H5B 0.684633 0.112719 0.262689 0.047 Uiso 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'
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 . 4_655 96.07(14) y
O1 Cu1 O4 . 4_655 143.25(10) ?
O1 Cu1 O4 4_655 4_655 94.60(11) ?
O1 Cu1 O4 . . 94.60(11) y
O1 Cu1 O4 4_655 . 143.25(10) ?
O4 Cu1 O4 4_655 . 97.54(15) y
O1 Cu1 O2 . . 59.59(9) ?
O1 Cu1 O2 4_655 . 123.20(9) ?
O4 Cu1 O2 4_655 . 85.29(9) ?
O4 Cu1 O2 . . 92.36(9) ?
O1 Cu1 O2 . 4_655 123.20(9) ?
O1 Cu1 O2 4_655 4_655 59.59(9) ?
O4 Cu1 O2 4_655 4_655 92.37(9) ?
O4 Cu1 O2 . 4_655 85.29(9) ?
O2 Cu1 O2 . 4_655 176.45(12) y
O3 Cu2 O3 5_656 . 180.0 ?
O3 Cu2 O2 5_656 5_656 92.62(10) ?
O3 Cu2 O2 . 5_656 87.38(10) ?
O3 Cu2 O2 5_656 . 87.38(10) ?
O3 Cu2 O2 . . 92.62(10) y
O2 Cu2 O2 5_656 . 180.0 ?
C1 O1 Cu1 . . 100.4(2) ?
C1 O2 Cu2 . . 129.6(2) y
C1 O2 Cu1 . . 84.86(19) y
Cu2 O2 Cu1 . . 145.44(13) y
C3 O3 Cu2 . . 126.8(2) ?
O2 C1 O1 . . 115.2(3) ?
O2 C1 C2 . . 123.5(3) ?
O1 C1 C2 . . 121.3(3) ?
C7 C2 C3 . . 119.5(3) ?
C7 C2 C1 . . 118.4(3) ?
C3 C2 C1 . . 122.0(3) ?
O3 C3 C2 . . 125.2(3) ?
O3 C3 C4 . . 118.1(3) ?
C2 C3 C4 . . 116.7(3) ?
C5 C4 C3 . . 121.8(3) ?
C5 C4 H4 . . 119.1 ?
C3 C4 H4 . . 119.1 ?
C4 C5 C6 . . 121.0(4) ?
C4 C5 H5 . . 119.5 ?
C6 C5 H5 . . 119.5 ?
C7 C6 C5 . . 118.5(3) ?
C7 C6 H6 . . 120.8 ?
C5 C6 H6 . . 120.8 ?
C6 C7 C2 . . 122.5(3) ?
C6 C7 H7 . . 118.8 ?
C2 C7 H7 . . 118.8 ?
Cu1 O4 H4A . . 108.8 ?
Cu1 O4 H4B . . 108.6 ?
H4A O4 H4B . . 106.5 ?
H5A O5 H5B . . 105.3 ?
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 . 1.984(2) y
Cu1 O1 4_655 1.984(2) ?
Cu1 O4 4_655 2.001(3) ?
Cu1 O4 . 2.001(3) y
Cu1 O2 . 2.332(2) y
Cu1 O2 4_655 2.332(2) ?
Cu2 O3 5_656 1.905(2) ?
Cu2 O3 . 1.905(2) y
Cu2 O2 5_656 1.905(2) ?
Cu2 O2 . 1.905(2) y
O1 C1 . 1.292(4) y
O2 C1 . 1.274(4) y
O3 C3 . 1.322(4) y
C1 C2 . 1.452(5) ?
C2 C7 . 1.409(5) ?
C2 C3 . 1.416(5) ?
C3 C4 . 1.426(5) ?
C4 C5 . 1.367(5) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.397(5) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.361(5) ?
C6 H6 . 0.9500 ?
C7 H7 . 0.9500 ?
O4 H4A . 0.7679 ?
O4 H4B . 0.7271 ?
O5 H5A . 0.8007 ?
O5 H5B . 0.7079 ?
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
O4 H4A O1 1_545 0.77 1.96 2.718(3) 169
O4 H4B O3 8 0.73 1.96 2.685(3) 177
O5 H5A O5 7_765 0.80 2.02 2.803(3) 167
O5 H5B O4 . 0.71 2.43 3.088(4) 157
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
_geom_torsion_publ_flag
Cu2 O2 C1 O1 -176.6(2) ?
Cu1 O2 C1 O1 1.0(3) ?
Cu2 O2 C1 C2 3.7(5) ?
Cu1 O2 C1 C2 -178.8(3) ?
Cu1 O1 C1 O2 -1.2(3) ?
Cu1 O1 C1 C2 178.6(3) ?
O2 C1 C2 C7 176.4(3) ?
O1 C1 C2 C7 -3.4(5) y
O2 C1 C2 C3 -2.5(6) y
O1 C1 C2 C3 177.7(3) ?
Cu2 O3 C3 C2 4.9(5) ?
Cu2 O3 C3 C4 -176.3(2) ?
C7 C2 C3 O3 179.2(3) ?
C1 C2 C3 O3 -1.9(6) ?
C7 C2 C3 C4 0.4(5) ?
C1 C2 C3 C4 179.3(3) ?
O3 C3 C4 C5 -178.3(4) ?
C2 C3 C4 C5 0.5(5) ?
C3 C4 C5 C6 -0.6(6) ?
C4 C5 C6 C7 -0.3(6) ?
C5 C6 C7 C2 1.3(6) ?
C3 C2 C7 C6 -1.3(5) ?
C1 C2 C7 C6 179.7(4) ?

_cod_database_fobs_code 2242031
