#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:20:24 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179573 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/38/4503867.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_4503867
loop_
_publ_author_name
'Martin, David P.'
'Supkowski, Ronald M.'
'LaDuca, Robert L.'
_publ_section_title
;
 A Three-Dimensional Mixed-Ligand Coordination Polymer Featuring Strongly
 Antiferromagnetically Coupled Dinuclear Copper Paddlewheels Linked into a
 6-Connected Self-Penetrated Network
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3518
_journal_paper_doi               10.1021/cg800743a
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C13 H20 Cu N2 O6'
_chemical_formula_weight         363.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.184(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.054(3)
_cell_length_b                   13.568(3)
_cell_length_c                   8.7130(18)
_cell_measurement_temperature    173(2)
_cell_volume                     1543.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16780
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.445
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0261P)²+1.3436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                2536
_reflns_number_total             3531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg800743a_si_002.cif
_cod_data_source_block           mono
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1543.3(6)
_cod_original_sg_symbol_H-M      P2(1)/C
_cod_database_code               4503867
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Cu1 Cu 0.58762(2) 0.04017(2) 0.04517(4) 0.01238(9) Uani 1 1 d .
O1 O 0.63549(14) 0.01053(14) -0.1643(2) 0.0239(5) Uani 1 1 d .
O1W O 0.88449(19) 0.71938(17) 0.0883(3) 0.0383(6) Uani 1 1 d D
H1WA H 0.867(3) 0.694(2) 0.172(3) 0.056(13) Uiso 1 1 d D
H1WB H 0.927(2) 0.681(2) 0.045(4) 0.047(11) Uiso 1 1 d D
O2 O 0.48498(13) -0.04939(13) -0.2421(2) 0.0202(4) Uani 1 1 d .
O2W O 0.8298(2) 0.8672(2) -0.1209(3) 0.0455(6) Uani 1 1 d D
H2WA H 0.840(3) 0.829(2) -0.046(3) 0.053(13) Uiso 1 1 d D
H2WB H 0.7753(19) 0.897(2) -0.108(4) 0.054(12) Uiso 1 1 d D
O3 O 0.63522(14) -0.40791(13) -0.4000(2) 0.0226(4) Uani 1 1 d .
O4 O 0.48633(14) -0.34126(13) -0.4716(2) 0.0238(5) Uani 1 1 d .
N1 N 0.71506(16) 0.13226(15) 0.1203(2) 0.0160(5) Uani 1 1 d .
N2 N 0.98154(16) 0.40763(16) 0.0801(3) 0.0181(5) Uani 1 1 d .
C1 C 0.6900(2) 0.2177(2) 0.1870(3) 0.0233(6) Uani 1 1 d .
H1 H 0.6219 0.2279 0.2143 0.028 Uiso 1 1 calc R
C2 C 0.7595(2) 0.2914(2) 0.2173(3) 0.0219(6) Uani 1 1 d .
H2 H 0.7380 0.3498 0.2629 0.026 Uiso 1 1 calc R
C3 C 0.8618(2) 0.27833(19) 0.1798(3) 0.0176(6) Uani 1 1 d .
C4 C 0.8886(2) 0.18941(19) 0.1125(3) 0.0186(6) Uani 1 1 d .
H4 H 0.9563 0.1771 0.0860 0.022 Uiso 1 1 calc R
C5 C 0.8142(2) 0.11939(19) 0.0852(3) 0.0169(6) Uani 1 1 d .
H5 H 0.8337 0.0602 0.0402 0.020 Uiso 1 1 calc R
C6 C 0.9400(2) 0.3571(2) 0.2168(3) 0.0227(6) Uani 1 1 d .
H6A H 0.9087 0.4058 0.2833 0.027 Uiso 1 1 calc R
H6B H 0.9963 0.3272 0.2730 0.027 Uiso 1 1 calc R
C7 C 1.0573(2) 0.4808(2) 0.1342(3) 0.0225(6) Uani 1 1 d .
H7A H 1.1127 0.4471 0.1870 0.027 Uiso 1 1 calc R
H7B H 1.0249 0.5251 0.2066 0.027 Uiso 1 1 calc R
C8 C 0.89972(19) 0.4605(2) -0.0026(3) 0.0203(6) Uani 1 1 d .
H8A H 0.8648 0.5045 0.0677 0.024 Uiso 1 1 calc R
H8B H 0.8501 0.4135 -0.0414 0.024 Uiso 1 1 calc R
C11 C 0.5774(2) -0.02817(17) -0.2628(3) 0.0148(5) Uani 1 1 d .
C12 C 0.6224(2) -0.05281(18) -0.4181(3) 0.0174(6) Uani 1 1 d .
H12A H 0.6966 -0.0537 -0.4097 0.021 Uiso 1 1 calc R
H12B H 0.6038 -0.0015 -0.4905 0.021 Uiso 1 1 calc R
C13 C 0.5862(2) -0.15162(18) -0.4800(3) 0.0179(6) Uani 1 1 d .
H13A H 0.6175 -0.1636 -0.5790 0.021 Uiso 1 1 calc R
H13B H 0.5125 -0.1499 -0.4944 0.021 Uiso 1 1 calc R
C14 C 0.6140(2) -0.23520(18) -0.3702(3) 0.0188(6) Uani 1 1 d .
H14A H 0.6880 -0.2380 -0.3603 0.023 Uiso 1 1 calc R
H14B H 0.5863 -0.2200 -0.2698 0.023 Uiso 1 1 calc R
C15 C 0.5757(2) -0.33539(18) -0.4186(3) 0.0151(6) Uani 1 1 d .
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'
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'
Cu Cu 0.3201 1.2651 '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
O3 Cu1 O2 89.94(8) 4_556 3_655
O3 Cu1 O1 86.41(8) 4_556 .
O2 Cu1 O1 167.21(7) 3_655 .
O3 Cu1 O4 167.68(8) 4_556 2_654
O2 Cu1 O4 89.72(8) 3_655 2_654
O1 Cu1 O4 91.24(8) . 2_654
O3 Cu1 N1 102.18(8) 4_556 .
O2 Cu1 N1 94.07(8) 3_655 .
O1 Cu1 N1 98.68(8) . .
O4 Cu1 N1 90.13(8) 2_654 .
O3 Cu1 Cu1 88.19(6) 4_556 3_655
O2 Cu1 Cu1 82.39(5) 3_655 3_655
O1 Cu1 Cu1 85.25(6) . 3_655
O4 Cu1 Cu1 79.56(6) 2_654 3_655
N1 Cu1 Cu1 169.08(6) . 3_655
C11 O1 Cu1 121.63(17) . .
C11 O2 Cu1 125.26(17) . 3_655
C15 O3 Cu1 119.20(17) . 4
C15 O4 Cu1 128.43(17) . 2_644
C1 N1 C5 116.7(2) . .
C1 N1 Cu1 116.07(18) . .
C5 N1 Cu1 126.37(17) . .
C8 N2 C7 108.2(2) . .
C8 N2 C6 110.7(2) . .
C7 N2 C6 107.5(2) . .
N1 C1 C2 123.4(3) . .
C1 C2 C3 119.9(2) . .
C2 C3 C4 117.1(2) . .
C2 C3 C6 120.6(2) . .
C4 C3 C6 122.2(2) . .
C5 C4 C3 119.6(3) . .
N1 C5 C4 123.4(2) . .
N2 C6 C3 113.9(2) . .
N2 C7 C8 111.3(2) . 3_765
N2 C8 C7 111.0(2) . 3_765
O2 C11 O1 125.1(2) . .
O2 C11 C12 117.0(2) . .
O1 C11 C12 117.8(2) . .
C11 C12 C13 113.0(2) . .
C12 C13 C14 111.1(2) . .
C15 C14 C13 114.6(2) . .
O4 C15 O3 124.6(2) . .
O4 C15 C14 117.8(2) . .
O3 C15 C14 117.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O3 1.9576(18) 4_556
Cu1 O2 1.9671(18) 3_655
Cu1 O1 1.9723(19) .
Cu1 O4 1.9817(18) 2_654
Cu1 N1 2.179(2) .
Cu1 Cu1 2.6513(7) 3_655
O1 C11 1.258(3) .
O2 C11 1.254(3) .
O2 Cu1 1.9671(18) 3_655
O3 C15 1.264(3) .
O3 Cu1 1.9576(18) 4
O4 C15 1.256(3) .
O4 Cu1 1.9817(18) 2_644
N1 C1 1.339(3) .
N1 C5 1.342(3) .
N2 C8 1.473(3) .
N2 C7 1.477(3) .
N2 C6 1.479(3) .
C1 C2 1.375(4) .
C2 C3 1.386(4) .
C3 C4 1.387(4) .
C3 C6 1.513(4) .
C4 C5 1.379(4) .
C7 C8 1.506(4) 3_765
C8 C7 1.506(4) 3_765
C11 C12 1.514(3) .
C12 C13 1.520(3) .
C13 C14 1.527(4) .
C14 C15 1.508(3) .
