#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/74/2227420.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_2227420
loop_
_publ_author_name
'Zhou, Xin-Hui'
_publ_section_title
;
 catena-Poly[hexaaqua-1κO,2κO,3κ⁴O-(μ₄-3,5-dicarboxylatopyrazol-1-ido-3':1:2:3κ⁶O⁵:N¹,O^5'^:N²,O³:O^3'^)(μ₂-3,5-dicarboxylatopyrazol-1-ido-1:2κ⁴N²,O³:N¹,O⁵)-1,2-dicopper(II)-3-manganese(II)]
;
_journal_coeditor_code           FJ2333
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1309
_journal_paper_doi               10.1107/S1600536810037542
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cu2 Mn (C5 H N2 O4)2 (H2 O)6]'
_chemical_formula_moiety         'C10 H14 Cu2 Mn N4 O14'
_chemical_formula_sum            'C10 H14 Cu2 Mn N4 O14'
_chemical_formula_weight         596.27
_chemical_name_systematic
;
catena-Poly[hexaaqua-1κO,2κO,3κ⁴O-(μ₄-
3,5-dicarboxylatopyrazol-1-ido-3':1:2:3κ⁶O⁵:N¹,
O^5'^:N²,O³:O^3'^)(μ₂-3,5-
dicarboxylatopyrazol-1-ido-1:2κ⁴N²,O³:N¹,
O⁵)-1,2-dicopper(II)-3-manganese(II)]
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.778(3)
_cell_length_b                   13.0387(19)
_cell_length_c                   12.3800(18)
_cell_measurement_reflns_used    2617
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.5
_cell_volume                     3515.4(9)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8862
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    3.194
_exptl_absorpt_correction_T_max  0.7004
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.641
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0567
_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)+(0.0422P)²+21.9067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                1562
_reflns_number_total             1779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            fj2333.cif
_cod_data_source_block           I
_cod_original_cell_volume        3515.3(9)
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2227420
_cod_database_fobs_code          2227420
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'
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_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.41085(3) 0.14426(5) 1.06815(5) 0.0203(2) Uani d . 1 A .
Mn Mn1 0.2500 0.12380(9) 0.7500 0.0246(3) Uani d S 1 . .
C C1 0.5000 0.1141(6) 1.3514(6) 0.0224(16) Uani d S 1 . .
H H1 0.5000 0.1054 1.4259 0.027 Uiso calc SR 1 . .
C C2 0.4501(2) 0.1221(4) 1.2832(4) 0.0191(11) Uani d . 1 . .
C C3 0.3821(2) 0.1194(4) 1.2885(4) 0.0205(11) Uani d . 1 A .
C C4 0.5000 0.1212(5) 0.7831(6) 0.0172(15) Uani d S 1 . .
H H4 0.5000 0.1178 0.7081 0.021 Uiso calc SR 1 . .
C C5 0.4497(2) 0.1244(4) 0.8532(4) 0.0171(10) Uani d . 1 A .
C C6 0.3809(2) 0.1249(4) 0.8491(4) 0.0183(10) Uani d . 1 . .
N N1 0.47006(19) 0.1342(3) 1.1814(3) 0.0202(9) Uani d . 1 . .
N N2 0.46982(19) 0.1290(4) 0.9544(3) 0.0210(10) Uani d . 1 . .
O O1 0.35447(17) 0.1124(3) 1.3755(3) 0.0298(10) Uani d . 1 . .
O O2 0.35551(16) 0.1236(3) 1.1967(3) 0.0230(8) Uani d . 1 . .
O O3 0.35519(16) 0.1275(3) 0.9417(3) 0.0256(9) Uani d . 1 A .
O O4 0.35220(16) 0.1236(3) 0.7623(3) 0.0229(8) Uani d . 1 A .
O O5W 0.4030(2) 0.3139(3) 1.0671(3) 0.0364(10) Uani d . 1 . .
H H2 0.3857 0.3342 1.1248 0.055 Uiso d R 1 A .
H H3 0.3823 0.3398 1.0157 0.055 Uiso d R 1 . .
O O6W 0.2501(4) -0.0125(11) 0.6497(12) 0.033(3) Uani d P 0.50(3) A 1
H H5 0.2677 -0.0653 0.6755 0.049 Uiso d PR 0.50(3) A 1
H H6 0.2121 -0.0259 0.6433 0.049 Uiso d PR 0.50(3) A 1
O O6W' 0.2644(7) 0.0351(14) 0.6051(12) 0.042(5) Uani d P 0.50(3) A 2
H H7 0.2464 0.0563 0.5484 0.063 Uiso d PR 0.50(3) A 2
H H8 0.3028 0.0420 0.5955 0.063 Uiso d PR 0.50(3) A 2
O O7W 0.2436(4) 0.2640(9) 0.8425(12) 0.032(3) Uani d P 0.50(2) A 3
H H9 0.2115 0.2976 0.8258 0.048 Uiso d PR 0.50(2) A 3
H H10 0.2752 0.3015 0.8513 0.048 Uiso d PR 0.50(2) A 3
O O7W' 0.2415(5) 0.2143(15) 0.8986(13) 0.050(5) Uani d P 0.50(2) A 4
H H11 0.2152 0.1755 0.9287 0.076 Uiso d PR 0.50(2) A 4
H H12 0.2703 0.1978 0.9416 0.076 Uiso d PR 0.50(2) A 4
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'
Mn Mn 0.3368 0.7283 '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 Cu1 N2 . . 94.59(18) ?
N1 Cu1 O3 . . 168.67(18) ?
N2 Cu1 O3 . . 79.57(16) ?
N1 Cu1 O2 . . 79.32(16) ?
N2 Cu1 O2 . . 165.40(18) ?
O3 Cu1 O2 . . 104.02(14) ?
N1 Cu1 O5W . . 97.17(17) ?
N2 Cu1 O5W . . 98.69(18) ?
O3 Cu1 O5W . . 93.33(16) ?
O2 Cu1 O5W . . 95.25(15) ?
O6W' Mn1 O6W' . 7_546 115.2(12) ?
O6W' Mn1 O7W . . 154.6(8) ?
O6W' Mn1 O7W 7_546 . 90.2(7) ?
O6W' Mn1 O7W . 7_546 90.2(7) ?
O6W' Mn1 O7W 7_546 7_546 154.6(8) ?
O7W Mn1 O7W . 7_546 64.5(9) ?
O6W' Mn1 O6W . . 23.7(3) ?
O6W' Mn1 O6W 7_546 . 92.1(11) ?
O7W Mn1 O6W . . 175.4(5) ?
O7W Mn1 O6W 7_546 . 112.9(6) ?
O6W' Mn1 O6W . 7_546 92.1(11) ?
O6W' Mn1 O6W 7_546 7_546 23.7(3) ?
O7W Mn1 O6W . 7_546 112.9(6) ?
O7W Mn1 O6W 7_546 7_546 175.4(5) ?
O6W Mn1 O6W . 7_546 69.9(10) ?
O6W' Mn1 O7W' . . 176.5(5) ?
O6W' Mn1 O7W' 7_546 . 65.1(8) ?
O7W Mn1 O7W' . . 25.2(3) ?
O7W Mn1 O7W' 7_546 . 89.7(10) ?
O6W Mn1 O7W' . . 157.2(8) ?
O6W Mn1 O7W' 7_546 . 87.7(8) ?
O6W' Mn1 O7W' . 7_546 65.1(8) ?
O6W' Mn1 O7W' 7_546 7_546 176.5(5) ?
O7W Mn1 O7W' . 7_546 89.7(10) ?
O7W Mn1 O7W' 7_546 7_546 25.2(3) ?
O6W Mn1 O7W' . 7_546 87.7(8) ?
O6W Mn1 O7W' 7_546 7_546 157.2(8) ?
O7W' Mn1 O7W' . 7_546 114.9(13) ?
O6W' Mn1 O4 . . 84.9(4) ?
O6W' Mn1 O4 7_546 . 95.0(4) ?
O7W Mn1 O4 . . 91.7(2) ?
O7W Mn1 O4 7_546 . 88.5(2) ?
O6W Mn1 O4 . . 92.1(3) ?
O6W Mn1 O4 7_546 . 87.8(3) ?
O7W' Mn1 O4 . . 91.6(3) ?
O7W' Mn1 O4 7_546 . 88.5(3) ?
O6W' Mn1 O4 . 7_546 95.0(4) ?
O6W' Mn1 O4 7_546 7_546 84.9(4) ?
O7W Mn1 O4 . 7_546 88.5(2) ?
O7W Mn1 O4 7_546 7_546 91.7(2) ?
O6W Mn1 O4 . 7_546 87.8(3) ?
O6W Mn1 O4 7_546 7_546 92.1(3) ?
O7W' Mn1 O4 . 7_546 88.5(3) ?
O7W' Mn1 O4 7_546 7_546 91.6(3) ?
O4 Mn1 O4 . 7_546 179.8(2) ?
C2 C1 C2 12_655 . 103.9(7) ?
C2 C1 H1 12_655 . 128.1 ?
C2 C1 H1 . . 128.1 ?
N1 C2 C1 . . 109.2(5) ?
N1 C2 C3 . . 111.5(4) ?
C1 C2 C3 . . 139.3(5) ?
O1 C3 O2 . . 124.0(5) ?
O1 C3 C2 . . 121.7(5) ?
O2 C3 C2 . . 114.4(4) ?
C5 C4 C5 12_655 . 103.2(6) ?
C5 C4 H4 12_655 . 128.4 ?
C5 C4 H4 . . 128.4 ?
N2 C5 C4 . . 109.2(4) ?
N2 C5 C6 . . 111.2(4) ?
C4 C5 C6 . . 139.6(5) ?
O4 C6 O3 . . 123.8(5) ?
O4 C6 C5 . . 122.1(5) ?
O3 C6 C5 . . 114.0(4) ?
N1 N1 C2 12_655 . 108.9(3) ?
N1 N1 Cu1 12_655 . 132.47(12) ?
C2 N1 Cu1 . . 118.6(3) ?
N2 N2 C5 12_655 . 109.3(3) ?
N2 N2 Cu1 12_655 . 132.09(12) ?
C5 N2 Cu1 . . 118.5(3) ?
C3 O2 Cu1 . . 116.0(3) ?
C6 O3 Cu1 . . 116.3(3) ?
C6 O4 Mn1 . . 124.1(3) ?
Cu1 O5W H2 . . 109.9 ?
Cu1 O5W H3 . . 116.2 ?
H2 O5W H3 . . 105.7 ?
Mn1 O6W H5 . . 116.8 ?
Mn1 O6W H6 . . 102.7 ?
H5 O6W H6 . . 107.7 ?
Mn1 O6W' H6 . . 84.8 ?
Mn1 O6W' H7 . . 116.4 ?
H6 O6W' H7 . . 94.9 ?
Mn1 O7W H9 . . 111.1 ?
Mn1 O7W H10 . . 120.1 ?
H9 O7W H10 . . 113.6 ?
Mn1 O7W' H11 . . 96.0 ?
Mn1 O7W' H12 . . 109.1 ?
H11 O7W' H12 . . 94.1 ?
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 N1 . 1.910(4) ?
Cu1 N2 . 1.916(4) ?
Cu1 O3 . 1.992(4) ?
Cu1 O2 . 2.014(4) ?
Cu1 O5W . 2.219(4) ?
Mn1 O6W' . 2.157(10) ?
Mn1 O6W' 7_546 2.157(10) ?
Mn1 O7W . 2.162(9) ?
Mn1 O7W 7_546 2.162(9) ?
Mn1 O6W . 2.168(10) ?
Mn1 O6W 7_546 2.168(10) ?
Mn1 O7W' . 2.193(10) ?
Mn1 O7W' 7_546 2.193(10) ?
Mn1 O4 . 2.231(3) ?
Mn1 O4 7_546 2.231(3) ?
C1 C2 12_655 1.379(7) ?
C1 C2 . 1.379(7) ?
C1 H1 . 0.9300 ?
C2 N1 . 1.342(6) ?
C2 C3 . 1.484(7) ?
C3 O1 . 1.238(6) ?
C3 O2 . 1.276(6) ?
C4 C5 12_655 1.398(6) ?
C4 C5 . 1.398(6) ?
C4 H4 . 0.9300 ?
C5 N2 . 1.329(6) ?
C5 C6 . 1.500(7) ?
C6 O4 . 1.243(6) ?
C6 O3 . 1.276(6) ?
N1 N1 12_655 1.304(8) ?
N2 N2 12_655 1.315(8) ?
O5W H2 . 0.8500 ?
O5W H3 . 0.8500 ?
O6W H5 . 0.8500 ?
O6W H6 . 0.8500 ?
O6W' H7 . 0.8500 ?
O6W' H8 . 0.8499 ?
O7W H9 . 0.8500 ?
O7W H10 . 0.8500 ?
O7W' H11 . 0.8499 ?
O7W' H12 . 0.8500 ?
