#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/95/2219542.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_2219542
loop_
_publ_author_name
'Wu, YanLi'
'Wang, XingCong'
'You, XiuLi'
_publ_section_title
;
 Di-μ-sulfato-bis{[bis(3,5-dimethylpyrazol-1-yl)methane]copper(II)}
;
_journal_coeditor_code           CS2085
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1242
_journal_paper_doi               10.1107/S1600536808027840
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu2 (S O4)2 (C11 H16 N4)2]'
_chemical_formula_moiety         'C22 H32 Cu2 N8 O8 S2'
_chemical_formula_sum            'C22 H32 Cu2 N8 O8 S2'
_chemical_formula_weight         727.76
_chemical_name_systematic
;
Di-μ-sulfato-bis{[bis(3,5-dimethylpyrazol-1-yl)methane]copper(II)}
;
_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
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.5293(15)
_cell_length_b                   10.734(2)
_cell_length_c                   17.740(4)
_cell_measurement_reflns_used    4573
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.0043
_cell_volume                     1413.1(5)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2001)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13344
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.714
_exptl_absorpt_correction_T_max  0.7365
_exptl_absorpt_correction_T_min  0.7042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.418
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0451
_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)+(0.0540P)²+2.0475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1124
_reflns_number_gt                2253
_reflns_number_total             2580
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cs2085.cif
_cod_data_source_block           I
_cod_original_cell_volume        1413.2(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2219542
_cod_database_fobs_code          2219542
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_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
Cu Cu1 -0.00166(6) 0.33244(4) 0.03099(2) 0.03196(18) Uani d . 1
S S1 -0.08737(12) 0.41689(8) -0.10738(5) 0.0301(2) Uani d . 1
O O1 -0.2040(4) 0.3437(3) -0.06474(16) 0.0422(7) Uani d . 1
O O2 0.0920(3) 0.4113(3) -0.05419(15) 0.0431(7) Uani d . 1
O O3 -0.0756(4) 0.3645(3) -0.18102(15) 0.0461(7) Uani d . 1
O O4 -0.1457(4) 0.5477(3) -0.11429(16) 0.0444(7) Uani d . 1
N N1 -0.1409(4) 0.2717(3) 0.10764(17) 0.0316(7) Uani d . 1
N N2 -0.0581(4) 0.1991(3) 0.16697(17) 0.0330(7) Uani d . 1
N N3 0.1848(4) 0.1141(3) 0.11191(17) 0.0316(7) Uani d . 1
N N4 0.1593(4) 0.1722(3) 0.04242(17) 0.0315(7) Uani d . 1
C C1 -0.3116(5) 0.2839(4) 0.1176(2) 0.0343(9) Uani d . 1
C C2 -0.3360(6) 0.2205(4) 0.1837(2) 0.0411(10) Uani d . 1
H H2 -0.4423 0.2152 0.2036 0.049 Uiso calc R 1
C C3 -0.1745(6) 0.1674(4) 0.2137(2) 0.0365(9) Uani d . 1
C C4 -0.1213(7) 0.0889(5) 0.2836(3) 0.0557(13) Uani d . 1
H H4A -0.0814 0.0089 0.2691 0.084 Uiso calc R 1
H H4B -0.2230 0.0785 0.3092 0.084 Uiso calc R 1
H H4C -0.0253 0.1291 0.3175 0.084 Uiso calc R 1
C C5 -0.4425(5) 0.3586(4) 0.0638(2) 0.0433(10) Uani d . 1
H H5A -0.3832 0.4307 0.0478 0.065 Uiso calc R 1
H H5B -0.5399 0.3843 0.0888 0.065 Uiso calc R 1
H H5C -0.4889 0.3089 0.0198 0.065 Uiso calc R 1
C C6 0.1344(5) 0.1810(4) 0.1760(2) 0.0331(8) Uani d . 1
H H6A 0.1751 0.1348 0.2228 0.040 Uiso calc R 1
H H6B 0.1939 0.2615 0.1807 0.040 Uiso calc R 1
C C7 0.2597(5) -0.0001(4) 0.1088(2) 0.0360(9) Uani d . 1
C C8 0.2818(6) -0.0156(4) 0.0345(2) 0.0418(10) Uani d . 1
H H8 0.3300 -0.0851 0.0140 0.050 Uiso calc R 1
C C9 0.2187(5) 0.0921(4) -0.0045(2) 0.0340(9) Uani d . 1
C C10 0.3072(7) -0.0825(4) 0.1768(3) 0.0509(11) Uani d . 1
H H10A 0.4025 -0.0449 0.2123 0.076 Uiso calc R 1
H H10B 0.3462 -0.1619 0.1609 0.076 Uiso calc R 1
H H10C 0.2034 -0.0936 0.2009 0.076 Uiso calc R 1
C C11 0.2141(6) 0.1216(5) -0.0874(2) 0.0495(11) Uani d . 1
H H11A 0.0912 0.1305 -0.1123 0.074 Uiso calc R 1
H H11B 0.2701 0.0552 -0.1111 0.074 Uiso calc R 1
H H11C 0.2779 0.1979 -0.0920 0.074 Uiso calc R 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'
S S 0.1246 0.1234 '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
N1 Cu1 O2 . . 168.29(12)
N1 Cu1 O1 . . 100.44(11)
O2 Cu1 O1 . . 69.90(11)
N1 Cu1 N4 . . 91.60(12)
O2 Cu1 N4 . . 98.70(12)
O1 Cu1 N4 . . 117.24(12)
N1 Cu1 O4 . 3_565 89.80(12)
O2 Cu1 O4 . 3_565 93.50(11)
O1 Cu1 O4 . 3_565 139.06(11)
N4 Cu1 O4 . 3_565 101.80(12)
N1 Cu1 S1 . . 134.03(9)
O2 Cu1 S1 . . 35.47(8)
O1 Cu1 S1 . . 34.73(8)
N4 Cu1 S1 . . 115.22(9)
O4 Cu1 S1 3_565 . 117.63(8)
O3 S1 O4 . . 111.17(17)
O3 S1 O1 . . 112.93(18)
O4 S1 O1 . . 110.82(18)
O3 S1 O2 . . 111.43(17)
O4 S1 O2 . . 108.23(17)
O1 S1 O2 . . 101.81(16)
O3 S1 Cu1 . . 132.76(13)
O4 S1 Cu1 . . 115.83(12)
O1 S1 Cu1 . . 53.44(11)
O2 S1 Cu1 . . 48.89(11)
S1 O1 Cu1 . . 91.83(14)
S1 O2 Cu1 . . 95.64(14)
S1 O4 Cu1 . 3_565 114.00(17)
C1 N1 N2 . . 106.1(3)
C1 N1 Cu1 . . 134.3(3)
N2 N1 Cu1 . . 119.6(2)
C3 N2 N1 . . 110.9(3)
C3 N2 C6 . . 129.9(3)
N1 N2 C6 . . 118.6(3)
C7 N3 N4 . . 111.8(3)
C7 N3 C6 . . 130.3(3)
N4 N3 C6 . . 117.8(3)
C9 N4 N3 . . 105.1(3)
C9 N4 Cu1 . . 136.3(3)
N3 N4 Cu1 . . 117.0(2)
N1 C1 C2 . . 109.3(3)
N1 C1 C5 . . 121.1(3)
C2 C1 C5 . . 129.6(4)
C3 C2 C1 . . 107.3(3)
C3 C2 H2 . . 126.4
C1 C2 H2 . . 126.4
N2 C3 C2 . . 106.4(3)
N2 C3 C4 . . 122.8(4)
C2 C3 C4 . . 130.8(4)
C3 C4 H4A . . 109.5
C3 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C3 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
C1 C5 H5A . . 109.5
C1 C5 H5B . . 109.5
H5A C5 H5B . . 109.5
C1 C5 H5C . . 109.5
H5A C5 H5C . . 109.5
H5B C5 H5C . . 109.5
N2 C6 N3 . . 111.7(3)
N2 C6 H6A . . 109.3
N3 C6 H6A . . 109.3
N2 C6 H6B . . 109.3
N3 C6 H6B . . 109.3
H6A C6 H6B . . 107.9
N3 C7 C8 . . 105.6(3)
N3 C7 C10 . . 123.2(4)
C8 C7 C10 . . 131.1(4)
C7 C8 C9 . . 107.0(4)
C7 C8 H8 . . 126.5
C9 C8 H8 . . 126.5
N4 C9 C8 . . 110.4(3)
N4 C9 C11 . . 121.7(4)
C8 C9 C11 . . 127.9(4)
C7 C10 H10A . . 109.5
C7 C10 H10B . . 109.5
H10A C10 H10B . . 109.5
C7 C10 H10C . . 109.5
H10A C10 H10C . . 109.5
H10B C10 H10C . . 109.5
C9 C11 H11A . . 109.5
C9 C11 H11B . . 109.5
H11A C11 H11B . . 109.5
C9 C11 H11C . . 109.5
H11A C11 H11C . . 109.5
H11B C11 H11C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 N1 . 1.963(3)
Cu1 O2 . 1.964(3)
Cu1 O1 . 2.085(3)
Cu1 N4 . 2.094(3)
Cu1 O4 3_565 2.125(3)
Cu1 S1 . 2.5939(11)
S1 O3 . 1.439(3)
S1 O4 . 1.470(3)
S1 O1 . 1.479(3)
S1 O2 . 1.513(3)
O4 Cu1 3_565 2.125(3)
N1 C1 . 1.333(5)
N1 N2 . 1.372(4)
N2 C3 . 1.348(5)
N2 C6 . 1.444(5)
N3 C7 . 1.354(5)
N3 N4 . 1.366(4)
N3 C6 . 1.449(5)
N4 C9 . 1.326(5)
C1 C2 . 1.394(5)
C1 C5 . 1.486(6)
C2 C3 . 1.367(6)
C2 H2 . 0.9300
C3 C4 . 1.497(6)
C4 H4A . 0.9600
C4 H4B . 0.9600
C4 H4C . 0.9600
C5 H5A . 0.9600
C5 H5B . 0.9600
C5 H5C . 0.9600
C6 H6A . 0.9700
C6 H6B . 0.9700
C7 C8 . 1.365(5)
C7 C10 . 1.489(6)
C8 C9 . 1.390(6)
C8 H8 . 0.9300
C9 C11 . 1.499(5)
C10 H10A . 0.9600
C10 H10B . 0.9600
C10 H10C . 0.9600
C11 H11A . 0.9600
C11 H11B . 0.9600
C11 H11C . 0.9600
