#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/27/2202757.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_2202757
loop_
_publ_author_name
'Borkowski, Lauren A.'
'Cahill, Christopher L.'
_publ_section_title
;
 Poly[diaquabis(3-pyridylpropionato)copper(II)]
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1127
_journal_page_last               m1128
_journal_paper_doi               10.1107/S160053680302484X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cu (C8 H8 N O2)2 (H2 O)2]'
_chemical_formula_moiety         'C16 H20 Cu N2 O6'
_chemical_formula_sum            'C16 H20 Cu N2 O6'
_chemical_formula_weight         399.88
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.872(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4199(5)
_cell_length_b                   8.6557(5)
_cell_length_c                   10.1261(7)
_cell_measurement_reflns_used    17349
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.5
_cell_volume                     813.41(9)
_computing_cell_refinement       'HKL (Otwinowski & Minor, 1997)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2003)'
_computing_data_reduction        HKL
_computing_molecular_graphics    'CrystalMaker (CrystalMaker, 2003)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9977
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_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  0.048
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13951
_diffrn_reflns_theta_full        28.3
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    1.380
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC, 2003)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.308
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0323
_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)+(0.022P)²+0.74P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                1654
_reflns_number_total             2020
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            na6261.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2202757
_cod_database_fobs_code          2202757
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu1 1.0000 0.0000 0.5000 0.02558(10) Uani d S 1 . . Cu
O1 0.95412(15) 0.21538(16) 0.54973(14) 0.0305(3) Uani d . 1 . . O
O2 0.78469(17) 0.27134(19) 0.37361(16) 0.0392(4) Uani d . 1 . . O
O3 1.1056(2) -0.0229(2) 0.74057(18) 0.0419(4) Uani d . 1 . . O
N1 0.68873(18) 0.4264(2) 0.95299(16) 0.0269(4) Uani d . 1 . . N
C1 0.8565(2) 0.3002(2) 0.4861(2) 0.0274(4) Uani d . 1 . . C
C2 0.8247(3) 0.4528(3) 0.5501(2) 0.0355(5) Uani d . 1 . . C
C3 0.9140(2) 0.4975(3) 0.6846(2) 0.0355(5) Uani d . 1 . . C
C4 0.8647(2) 0.4302(2) 0.8067(2) 0.0283(4) Uani d . 1 . . C
C5 0.7347(2) 0.4762(2) 0.8419(2) 0.0286(4) Uani d . 1 . . C
C6 0.7727(2) 0.3287(3) 1.0339(2) 0.0316(5) Uani d . 1 . . C
C7 0.9031(2) 0.2776(3) 1.0061(2) 0.0381(5) Uani d . 1 . . C
C8 0.9489(2) 0.3283(3) 0.8912(2) 0.0367(5) Uani d . 1 . . C
H1 1.159(3) -0.106(4) 0.712(3) 0.072(10) Uiso d . 1 . . H
H2 1.163(4) 0.044(4) 0.775(3) 0.073(11) Uiso d . 1 . . H
H3 0.839(3) 0.534(3) 0.483(3) 0.043(7) Uiso d . 1 . . H
H4 0.724(3) 0.452(3) 0.553(3) 0.048(8) Uiso d . 1 . . H
H5 0.910(3) 0.610(3) 0.693(3) 0.047(7) Uiso d . 1 . . H
H6 1.014(3) 0.464(3) 0.686(3) 0.043(7) Uiso d . 1 . . H
H7 0.670(3) 0.541(3) 0.786(2) 0.038(7) Uiso d . 1 . . H
H8 0.740(3) 0.295(3) 1.113(2) 0.034(6) Uiso d . 1 . . H
H9 0.960(3) 0.210(3) 1.064(3) 0.049(8) Uiso d . 1 . . H
H10 1.039(3) 0.294(3) 0.870(3) 0.050(8) Uiso d . 1 . . H
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'
Cu Cu 0.3201 1.2651 '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'
N N 0.0061 0.0033 '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
O1 Cu1 O1 3_756 . 180.0000(10)
O1 Cu1 N1 3_756 4_665 89.88(6)
O1 Cu1 N1 . 4_665 90.12(6)
O1 Cu1 N1 3_756 2_646 90.12(6)
O1 Cu1 N1 . 2_646 89.88(6)
N1 Cu1 N1 4_665 2_646 180.0
O1 Cu1 O3 3_756 . 96.06(6)
O1 Cu1 O3 . . 83.94(6)
N1 Cu1 O3 4_665 . 92.05(6)
N1 Cu1 O3 2_646 . 87.95(6)
C1 O1 Cu1 . . 125.70(14)
Cu1 O3 H1 . . 84(2)
Cu1 O3 H2 . . 119(2)
H1 O3 H2 . . 109(3)
C6 N1 C5 . . 118.29(18)
C6 N1 Cu1 . 2_656 120.45(14)
C5 N1 Cu1 . 2_656 121.25(14)
O2 C1 O1 . . 125.7(2)
O2 C1 C2 . . 116.58(19)
O1 C1 C2 . . 117.74(19)
C3 C2 C1 . . 118.8(2)
C3 C2 H3 . . 108.0(15)
C1 C2 H3 . . 105.1(15)
C3 C2 H4 . . 111.9(16)
C1 C2 H4 . . 106.1(17)
H3 C2 H4 . . 106(2)
C4 C3 C2 . . 115.74(19)
C4 C3 H5 . . 106.8(16)
C2 C3 H5 . . 107.8(16)
C4 C3 H6 . . 107.8(15)
C2 C3 H6 . . 108.5(15)
H5 C3 H6 . . 110(2)
C8 C4 C5 . . 117.48(19)
C8 C4 C3 . . 122.0(2)
C5 C4 C3 . . 120.5(2)
N1 C5 C4 . . 123.14(19)
N1 C5 H7 . . 115.2(15)
C4 C5 H7 . . 121.6(15)
N1 C6 C7 . . 122.1(2)
N1 C6 H8 . . 118.0(15)
C7 C6 H8 . . 119.9(14)
C8 C7 C6 . . 119.2(2)
C8 C7 H9 . . 120.2(17)
C6 C7 H9 . . 120.6(17)
C7 C8 C4 . . 119.8(2)
C7 C8 H10 . . 120.5(17)
C4 C8 H10 . . 119.7(17)
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 3_756 1.9976(14) ?
Cu1 O1 . 1.9976(14) yes
Cu1 N1 4_665 2.0207(17) yes
Cu1 N1 2_646 2.0207(17) ?
Cu1 O3 . 2.4763(17) yes
O1 C1 . 1.264(2) ?
O2 C1 . 1.246(3) ?
O3 H1 . 0.95(3) ?
O3 H2 . 0.83(4) ?
N1 C6 . 1.337(3) ?
N1 C5 . 1.344(3) ?
N1 Cu1 2_656 2.0207(17) ?
C1 C2 . 1.523(3) ?
C2 C3 . 1.523(3) ?
C2 H3 . 1.01(3) ?
C2 H4 . 0.95(3) ?
C3 C4 . 1.510(3) ?
C3 H5 . 0.98(3) ?
C3 H6 . 0.98(3) ?
C4 C8 . 1.381(3) ?
C4 C5 . 1.391(3) ?
C5 H7 . 0.94(3) ?
C6 C7 . 1.380(3) ?
C6 H8 . 0.95(2) ?
C7 C8 . 1.379(3) ?
C7 H9 . 0.93(3) ?
C8 H10 . 0.95(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
O3 H1 O2 3_756 0.95(3) 1.80(3) 2.727(2) 164(3) yes
O3 H2 O2 4_666 0.83(4) 2.11(4) 2.936(2) 172(3) yes
