#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/84/2018480.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_2018480
loop_
_publ_author_name
'Bélombé, Michel M.'
'Nenwa, Justin'
'Wankap Kouamo, Jean S. T.'
'Ponou, Siméon'
'Fischer, Andreas'
_publ_section_title
;
 catena-Poly[[[(oxamide
 dioxime-κ²N,N')copper(II)]-μ-<small>L</small>-tartrato-κ⁴O¹,O²:O³,O⁴]
 tetrahydrate]: a chiral nanochannel framework hosting solvent water
 molecules
;
_journal_coeditor_code           SF3165
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m131
_journal_page_last               m134
_journal_paper_doi               10.1107/S0108270112016435
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu (C4 H4 O6) (C2 H6 N4 O2)] , 4H2 O'
_chemical_formula_moiety         'C6 H10 Cu N4 O8, 4(H2 O)'
_chemical_formula_sum            'C6 H18 Cu N4 O12'
_chemical_formula_weight         401.772
_chemical_name_systematic
;
catena-Poly[[[(oxamide
dioxime-κ²N,N')copper(II)]-μ-L-tartrato-
κ⁴O¹,O²:O³,O⁴] tetrahydrate]
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6316(9)
_cell_length_b                   14.6316(9)
_cell_length_c                   6.6239(4)
_cell_measurement_reflns_used    171
_cell_measurement_temperature    299
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      3.7
_cell_volume                     1418.07(15)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      299
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10357
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         5.00
_exptl_absorpt_coefficient_mu    1.616
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.204
_refine_ls_abs_structure_details 'Flack (1983), with 644 Friedel pairs'
_refine_ls_abs_structure_Flack   0.021(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_shift/su_mean_lt      0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0277P)²+0.0841P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0525
_reflns_number_gt                1426
_reflns_number_total             1624
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sf3165.cif
_cod_data_source_block           I
_cod_original_cell_volume        1418.1(2)
_cod_database_code               2018480
_cod_database_fobs_code          2018480
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'-y, -x, -z+1/2'
'y, x, -z'
'y+1/2, -x+1/2, z+1/4'
'-y+1/2, x+1/2, z+3/4'
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
_atom_site_symmetry_multiplicity
Cu Cu1 0.1408 0.1408 0.0000 0.01952(10) Uani d S 1 2
C C1 -0.02603(11) 0.04600(12) 0.0037(3) 0.0173(4) Uani d . 1 1
C C2 0.18881(12) 0.29030(12) 0.2560(3) 0.0193(4) Uani d . 1 1
C C3 0.23919(13) 0.22103(12) 0.3889(3) 0.0185(4) Uani d . 1 1
N N1 0.00707(11) 0.12625(11) 0.0363(3) 0.0213(4) Uani d . 1 1
N N2 -0.11351(11) 0.02580(12) -0.0238(3) 0.0261(4) Uani d . 1 1
O O1 -0.05969(10) 0.19413(10) 0.0267(3) 0.0369(4) Uani d . 1 1
O O2 0.14398(11) 0.26419(9) 0.1051(2) 0.0269(3) Uani d . 1 1
O O3 0.19637(12) 0.37216(10) 0.3041(2) 0.0352(4) Uani d . 1 1
O O4 0.21444(9) 0.13028(9) 0.3343(2) 0.0205(3) Uani d . 1 1
O O5 0.37291(12) 0.04366(11) 0.3020(3) 0.0394(4) Uani d . 1 1
O O6 0.14712(11) 0.47039(10) -0.0276(3) 0.0387(4) Uani d . 1 1
H H3 0.3030 0.2315 0.3653 0.022 Uiso d R 1 1
H H2A -0.1482 0.0701 -0.0205 0.031 Uiso d R 1 1
H H2B -0.1263 -0.0272 -0.0471 0.031 Uiso d R 1 1
H H1 -0.0340 0.2413 0.0999 0.044 Uiso d R 1 1
H H4 0.2583 0.0999 0.3124 0.025 Uiso d R 1 1
H H5A 0.3680 -0.0132 0.2643 0.047 Uiso d R 1 1
H H5B 0.3978 0.0629 0.2158 0.047 Uiso d R 1 1
H H6A 0.1379 0.5193 -0.0020 0.046 Uiso d R 1 1
H H6B 0.1588 0.4414 0.0919 0.046 Uiso d R 1 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'
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'
loop_
_diffrn_radiation_wavelength
0.71073
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
O2 Cu1 O2 6 . 94.85(9) y
O2 Cu1 N1 6 6 94.61(6) n
O2 Cu1 N1 . 6 165.16(6) y
O2 Cu1 N1 6 . 165.16(6) ?
O2 Cu1 N1 . . 94.61(6) y
N1 Cu1 N1 6 . 78.62(9) y
N1 C1 N2 . . 126.09(16) ?
N1 C1 C1 . 6 112.58(11) ?
N2 C1 C1 . 6 121.32(12) ?
O3 C2 O2 . . 122.90(19) ?
O3 C2 C3 . . 116.56(18) ?
O2 C2 C3 . . 120.53(16) ?
O4 C3 C3 . 6_556 111.41(11) ?
O4 C3 C2 . . 110.42(14) ?
C3 C3 C2 6_556 . 110.9(2) ?
C1 N1 O1 . . 112.22(15) ?
C1 N1 Cu1 . . 116.66(12) ?
O1 N1 Cu1 . . 127.53(12) ?
C2 O2 Cu1 . . 125.65(12) ?
O4 C3 H3 . . 110.8 ?
C3 C3 H3 6_556 . 107.5 ?
C2 C3 H3 . . 105.6 ?
C1 N2 H2A . . 114.6 ?
C1 N2 H2B . . 117.5 ?
H2A N2 H2B . . 127.9 ?
N1 O1 H1 . . 103.0 ?
C3 O4 H4 . . 111.4 ?
H5A O5 H5B . . 100.6 ?
H6A O6 H6B . . 106.3 ?
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 O2 6 1.9355(14) ?
Cu1 O2 . 1.9356(14) y
Cu1 N1 6 1.9829(16) ?
Cu1 N1 . 1.9829(16) y
C1 N1 . 1.288(2) ?
C1 N2 . 1.326(2) ?
C1 C1 6 1.491(3) ?
C2 O3 . 1.244(2) ?
C2 O2 . 1.255(3) ?
C2 C3 . 1.531(3) ?
C3 O4 . 1.423(2) ?
C3 C3 6_556 1.519(4) ?
N1 O1 . 1.395(2) ?
C3 H3 . 0.9587 ?
N2 H2A . 0.8230 ?
N2 H2B . 0.8126 ?
O1 H1 . 0.9237 ?
O4 H4 . 0.7939 ?
O5 H5A . 0.8711 ?
O5 H5B . 0.7327 ?
O6 H6A . 0.7473 ?
O6 H6B . 0.9147 ?
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
N2 H2A O3 3_455 0.82 2.44 3.164(2) 148 y
N2 H2B O4 2_554 0.81 2.13 2.878(2) 152 y
O1 H1 O6 7_455 0.92 1.82 2.696(2) 157 y
O4 H4 O5 . 0.79 1.87 2.651(2) 168 y
O5 H5A O3 4_545 0.87 2.27 2.869(2) 126 y
O5 H5A O5 8_544 0.87 2.53 3.236(2) 138 y
O5 H5B O6 6 0.73 2.05 2.762(2) 164 y
O6 H6A O2 8_554 0.75 2.51 2.956(2) 121 y
O6 H6A O3 8_554 0.75 2.62 3.362(2) 171 y
