#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/28/2212843.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_2212843
loop_
_publ_author_name
'Feng, Xiao-Jun'
'Dong, Hua-Ze'
'Huang, Wei'
_publ_section_title
Tetra-μ-acetato-κ⁸O:O'-bis[(4-dimethylaminopyridine-κN)copper(II)]
_journal_coeditor_code           CV2213
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1105
_journal_page_last               m1106
_journal_paper_doi               10.1107/S160053680701183X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu2 (C2 H3 O2)4 (C7 H10 N2)2]'
_chemical_formula_moiety         'C22 H32 Cu2 N4 O8'
_chemical_formula_sum            'C22 H32 Cu2 N4 O8'
_chemical_formula_weight         607.6
_chemical_name_systematic
;
Tetra-μ₂-acetato-κ⁸O:O'-bis[(4-dimethylaminopyridine-\kN)copper(II)]
;
_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                 96.944(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.615(3)
_cell_length_b                   8.233(3)
_cell_length_c                   14.618(5)
_cell_measurement_reflns_used    846
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.474
_cell_measurement_theta_min      3.140
_cell_volume                     1268.1(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6513
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.730
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628.0
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0305
_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)+(0.047P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                2072
_reflns_number_total             2481
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2213.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212843
_cod_database_fobs_code          2212843
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_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
C C1 0.8596(2) 0.0298(3) 0.17930(17) 0.0467(6) Uani d . 1
H H1 0.8785 -0.0405 0.1331 0.056 Uiso calc R 1
C C2 0.9481(2) 0.0455(3) 0.25555(17) 0.0466(6) Uani d . 1
H H2 1.0244 -0.0109 0.2592 0.056 Uiso calc R 1
C C3 0.9221(2) 0.1471(3) 0.32757(15) 0.0402(5) Uani d . 1
C C4 0.8063(2) 0.2291(3) 0.31424(16) 0.0452(5) Uani d . 1
H H4 0.7837 0.2998 0.3592 0.054 Uiso calc R 1
C C5 0.7263(2) 0.2053(3) 0.23506(17) 0.0461(6) Uani d . 1
H H5 0.6499 0.2619 0.2285 0.055 Uiso calc R 1
C C6 1.1311(3) 0.0968(4) 0.4144(2) 0.0702(8) Uani d . 1
H H6A 1.1261 -0.0190 0.4072 0.105 Uiso calc R 1
H H6B 1.1743 0.1225 0.4742 0.105 Uiso calc R 1
H H6C 1.1770 0.1422 0.3678 0.105 Uiso calc R 1
C C7 0.9722(3) 0.2669(4) 0.4801(2) 0.0745(9) Uani d . 1
H H7A 0.9819 0.3789 0.4640 0.112 Uiso calc R 1
H H7B 1.0277 0.2425 0.5352 0.112 Uiso calc R 1
H H7C 0.8859 0.2473 0.4905 0.112 Uiso calc R 1
C C8 0.5093(2) 0.2743(3) -0.07678(15) 0.0422(5) Uani d . 1
C C9 0.5096(3) 0.4409(3) -0.1191(2) 0.0572(7) Uani d . 1
H H9A 0.4941 0.4319 -0.1850 0.086 Uiso calc R 1
H H9B 0.5906 0.4912 -0.1021 0.086 Uiso calc R 1
H H9C 0.4443 0.5058 -0.0973 0.086 Uiso calc R 1
C C10 0.3495(2) 0.1214(3) 0.10420(15) 0.0388(5) Uani d . 1
C C11 0.2676(2) 0.1984(4) 0.16883(17) 0.0579(7) Uani d . 1
H H11A 0.3194 0.2314 0.2241 0.087 Uiso calc R 1
H H11B 0.2054 0.1214 0.1839 0.087 Uiso calc R 1
H H11C 0.2256 0.2915 0.1398 0.087 Uiso calc R 1
Cu Cu1 0.60135(2) 0.03965(3) 0.058164(16) 0.03512(12) Uani d . 1
N N1 0.74915(17) 0.1075(2) 0.16651(13) 0.0419(4) Uani d . 1
N N2 1.00392(19) 0.1645(3) 0.40560(14) 0.0558(5) Uani d . 1
O O1 0.59537(15) 0.24327(18) -0.01282(11) 0.0475(4) Uani d . 1
O O2 0.46614(14) 0.1250(2) 0.12739(10) 0.0479(4) Uani d . 1
O O3 0.70478(15) -0.0584(2) -0.03185(11) 0.0458(4) Uani d . 1
O O4 0.57775(17) -0.1792(2) 0.10703(12) 0.0539(4) 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 125.0(2) ?
N1 C1 H1 . . 117.5 ?
C2 C1 H1 . . 117.5 ?
C1 C2 C3 . . 119.3(2) ?
C1 C2 H2 . . 120.3 ?
C3 C2 H2 . . 120.3 ?
N2 C3 C4 . . 122.0(2) ?
N2 C3 C2 . . 122.2(2) ?
C4 C3 C2 . . 115.8(2) ?
C5 C4 C3 . . 119.8(2) ?
C5 C4 H4 . . 120.1 ?
C3 C4 H4 . . 120.1 ?
N1 C5 C4 . . 125.1(2) ?
N1 C5 H5 . . 117.5 ?
C4 C5 H5 . . 117.5 ?
N2 C6 H6A . . 109.5 ?
N2 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
N2 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
N2 C7 H7A . . 109.5 ?
N2 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
N2 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
O4 C8 O1 3_655 . 125.3(2) ?
O4 C8 C9 3_655 . 117.6(2) ?
O1 C8 C9 . . 117.1(2) ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C8 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
O2 C10 O3 . 3_655 125.5(2) ?
O2 C10 C11 . . 116.9(2) ?
O3 C10 C11 3_655 . 117.6(2) ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
O4 Cu1 O1 . . 167.13(7) ?
O4 Cu1 O2 . . 90.43(8) y
O1 Cu1 O2 . . 89.31(7) y
O4 Cu1 O3 . . 88.45(7) y
O1 Cu1 O3 . . 88.98(7) y
O2 Cu1 O3 . . 167.31(6) ?
O4 Cu1 N1 . . 94.79(7) y
O1 Cu1 N1 . . 98.07(7) y
O2 Cu1 N1 . . 92.32(7) y
O3 Cu1 N1 . . 100.37(7) y
O4 Cu1 Cu1 . 3_655 83.02(5) ?
O1 Cu1 Cu1 . 3_655 84.26(5) ?
O2 Cu1 Cu1 . 3_655 80.42(5) ?
O3 Cu1 Cu1 . 3_655 86.89(5) ?
N1 Cu1 Cu1 . 3_655 172.38(5) y
C1 N1 C5 . . 115.1(2) ?
C1 N1 Cu1 . . 121.89(16) ?
C5 N1 Cu1 . . 121.70(15) ?
C3 N2 C7 . . 120.7(2) ?
C3 N2 C6 . . 121.9(2) ?
C7 N2 C6 . . 117.1(2) ?
C8 O1 Cu1 . . 122.78(15) ?
C10 O2 Cu1 . . 127.63(15) ?
C10 O3 Cu1 3_655 . 119.53(14) ?
C8 O4 Cu1 3_655 . 124.52(15) ?
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
C1 N1 . 1.329(3) ?
C1 C2 . 1.374(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.398(3) ?
C2 H2 . 0.9300 ?
C3 N2 . 1.355(3) ?
C3 C4 . 1.396(3) ?
C4 C5 . 1.364(3) ?
C4 H4 . 0.9300 ?
C5 N1 . 1.331(3) ?
C5 H5 . 0.9300 ?
C6 N2 . 1.452(3) ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9600 ?
C6 H6C . 0.9600 ?
C7 N2 . 1.449(3) ?
C7 H7A . 0.9600 ?
C7 H7B . 0.9600 ?
C7 H7C . 0.9600 ?
C8 O4 3_655 1.250(3) ?
C8 O1 . 1.252(3) ?
C8 C9 . 1.505(3) ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C10 O2 . 1.244(3) ?
C10 O3 3_655 1.254(3) ?
C10 C11 . 1.500(3) ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
Cu1 O4 . 1.9657(18) y
Cu1 O1 . 1.9686(16) y
Cu1 O2 . 1.9821(15) y
Cu1 O3 . 1.9844(16) y
Cu1 N1 . 2.1635(19) y
Cu1 Cu1 3_655 2.6575(7) y
O3 C10 3_655 1.254(3) ?
O4 C8 3_655 1.250(3) ?
