#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:24:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179842 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/38/7013822.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_7013822
loop_
_publ_author_name
'King, Philippa'
'Clérac, Rodolphe'
'Anson, Christopher E.'
'Powell, Annie K.'
_publ_section_title
;
 The building block approach to extended solids:
 3,5-pyrazoledicarboxylate coordination compounds of increasing
 dimensionality.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              852
_journal_page_last               861
_journal_paper_doi               10.1039/b315067d
_journal_year                    2004
_chemical_formula_sum            'C10 H24 Mn2 N4 O18'
_chemical_formula_weight         598.21
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.890(8)
_cell_angle_beta                 92.257(7)
_cell_angle_gamma                112.480(7)
_cell_formula_units_Z            1
_cell_length_a                   7.2808(7)
_cell_length_b                   7.3579(10)
_cell_length_c                   12.0107(11)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.73
_cell_measurement_theta_min      5.18
_cell_volume                     570.95(12)
_computing_cell_refinement       'XSCANS 2.2 (Siemens, 1996)'
_computing_data_collection       'XSCANS 2.2 (Siemens, 1996)'
_computing_data_reduction        'XSCANS 2.2 (Siemens, 1996)'
_computing_molecular_graphics    'XP: SHELXTL/PC 5.03 (Siemens, 1995)'
_computing_publication_material  'XCIF: SHELXTL/PC 5.03 (Siemens, 1995)'
_computing_structure_refinement  'XL: SHELXTL/PC 5.03 (Siemens, 1995)'
_computing_structure_solution    'XS: SHELXTL/PC 5.03 (Siemens, 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       ω-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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2513
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'multi-faceted block'
_exptl_crystal_F_000             306
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.067(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         1998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0263
_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)+(0.0374P)²+0.2177P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                1853
_reflns_number_total             1998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b315067d.txt
_cod_data_source_block           pk1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        570.95(11)
_cod_database_code               7013822
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 0.5000 0.5000 0.02409(15) Uani 1 2 d S . .
N1 N 0.7596(2) 0.6803(2) 0.42645(12) 0.0230(3) Uani 1 1 d . . .
C1 C 0.9371(3) 0.7264(2) 0.48719(14) 0.0202(4) Uani 1 1 d . . .
C2 C 1.0931(3) 0.8081(3) 0.42610(14) 0.0213(4) Uani 1 1 d . . .
H21 H 1.226(4) 0.851(3) 0.4502(19) 0.031(5) Uiso 1 1 d . . .
C3 C 0.9991(3) 0.8080(3) 0.32409(15) 0.0213(4) Uani 1 1 d . . .
N2 N 0.8003(2) 0.7307(2) 0.32811(13) 0.0238(3) Uani 1 1 d . . .
H22 H 0.703(4) 0.720(3) 0.279(2) 0.039(6) Uiso 1 1 d . . .
C4 C 0.9342(3) 0.6831(3) 0.60314(14) 0.0206(4) Uani 1 1 d . . .
O1 O 0.76239(19) 0.5964(2) 0.62984(11) 0.0279(3) Uani 1 1 d . . .
O2 O 1.09683(18) 0.7344(2) 0.66502(10) 0.0291(3) Uani 1 1 d . . .
C5 C 1.0809(3) 0.8756(3) 0.22266(15) 0.0215(4) Uani 1 1 d . . .
O3 O 0.95493(18) 0.8538(2) 0.14003(10) 0.0275(3) Uani 1 1 d . . .
O4 O 1.26767(19) 0.9482(2) 0.22662(11) 0.0307(3) Uani 1 1 d . . .
O5 O 0.5467(2) 0.2263(2) 0.41222(14) 0.0336(3) Uani 1 1 d . . .
H51 H 0.649(4) 0.235(4) 0.386(2) 0.040(7) Uiso 1 1 d . . .
H52 H 0.464(4) 0.153(4) 0.364(2) 0.039(7) Uiso 1 1 d . . .
Mn2 Mn 1.0000 1.0000 0.0000 0.02597(15) Uani 1 2 d S . .
O6 O 0.6803(3) 0.8347(3) -0.06903(19) 0.0581(6) Uani 1 1 d . . .
H61 H 0.591(5) 0.760(5) -0.058(3) 0.054(9) Uiso 1 1 d . . .
H62 H 0.660(5) 0.878(5) -0.120(3) 0.079(11) Uiso 1 1 d . . .
O7 O 0.9452(3) 1.2549(3) 0.10585(15) 0.0476(4) Uani 1 1 d . . .
H71 H 0.871(5) 1.291(5) 0.079(3) 0.056(9) Uiso 1 1 d . . .
H72 H 0.925(5) 1.258(5) 0.174(3) 0.075(10) Uiso 1 1 d . . .
O8 O 0.5822(2) 0.3561(3) 0.78374(14) 0.0368(4) Uani 1 1 d . . .
H81 H 0.612(5) 0.260(5) 0.762(3) 0.070(10) Uiso 1 1 d . . .
H82 H 0.656(4) 0.440(4) 0.753(3) 0.052(8) Uiso 1 1 d . . .
O9 O 0.6924(2) 0.4249(3) 0.02464(15) 0.0399(4) Uani 1 1 d . . .
H91 H 0.754(6) 0.558(6) 0.058(3) 0.097(12) Uiso 1 1 d . . .
H92 H 0.673(5) 0.413(5) -0.044(3) 0.060(9) Uiso 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'
Mn Mn 0.3368 0.7283 '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
_geom_angle_publ_flag
O1 Mn1 O1 180.0 2_666 . ?
O1 Mn1 O5 90.63(6) 2_666 2_666 ?
O1 Mn1 O5 89.37(6) . 2_666 ?
O1 Mn1 O5 89.37(6) 2_666 . ?
O1 Mn1 O5 90.63(6) . . ?
O5 Mn1 O5 180.0 2_666 . ?
O1 Mn1 N1 105.55(5) 2_666 . ?
O1 Mn1 N1 74.45(5) . . ?
O5 Mn1 N1 92.17(6) 2_666 . ?
O5 Mn1 N1 87.83(6) . . ?
O1 Mn1 N1 74.45(5) 2_666 2_666 ?
O1 Mn1 N1 105.55(5) . 2_666 ?
O5 Mn1 N1 87.83(6) 2_666 2_666 ?
O5 Mn1 N1 92.17(6) . 2_666 ?
N1 Mn1 N1 180.0 . 2_666 ?
N2 N1 C1 106.03(14) . . ?
N2 N1 Mn1 139.21(11) . . ?
C1 N1 Mn1 113.47(11) . . ?
N1 C1 C2 110.44(15) . . ?
N1 C1 C4 117.04(15) . . ?
C2 C1 C4 132.52(16) . . ?
C3 C2 C1 104.75(15) . . ?
C3 C2 H21 129.1(14) . . ?
C1 C2 H21 126.2(14) . . ?
N2 C3 C2 107.16(15) . . ?
N2 C3 C5 121.41(15) . . ?
C2 C3 C5 131.43(16) . . ?
N1 N2 C3 111.62(14) . . ?
N1 N2 H22 119.6(17) . . ?
C3 N2 H22 128.6(17) . . ?
O2 C4 O1 125.25(16) . . ?
O2 C4 C1 118.90(15) . . ?
O1 C4 C1 115.85(15) . . ?
C4 O1 Mn1 118.08(11) . . ?
O4 C5 O3 125.90(16) . . ?
O4 C5 C3 117.30(15) . . ?
O3 C5 C3 116.80(15) . . ?
C5 O3 Mn2 129.26(11) . . ?
Mn1 O5 H51 121.2(18) . . ?
Mn1 O5 H52 114(2) . . ?
H51 O5 H52 105(3) . . ?
O3 Mn2 O3 180.00(6) . 2_775 ?
O3 Mn2 O7 90.77(6) . . ?
O3 Mn2 O7 89.23(6) 2_775 . ?
O3 Mn2 O7 89.23(6) . 2_775 ?
O3 Mn2 O7 90.77(6) 2_775 2_775 ?
O7 Mn2 O7 180.00(9) . 2_775 ?
O3 Mn2 O6 89.86(6) . 2_775 ?
O3 Mn2 O6 90.14(6) 2_775 2_775 ?
O7 Mn2 O6 89.10(8) . 2_775 ?
O7 Mn2 O6 90.90(9) 2_775 2_775 ?
O3 Mn2 O6 90.14(6) . . ?
O3 Mn2 O6 89.86(6) 2_775 . ?
O7 Mn2 O6 90.90(8) . . ?
O7 Mn2 O6 89.10(8) 2_775 . ?
O6 Mn2 O6 180.0 2_775 . ?
Mn2 O6 H61 140(2) . . ?
Mn2 O6 H62 107(3) . . ?
H61 O6 H62 113(3) . . ?
Mn2 O7 H71 119(2) . . ?
Mn2 O7 H72 120(2) . . ?
H71 O7 H72 107(3) . . ?
H81 O8 H82 103(3) . . ?
H91 O9 H92 106(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.1870(13) 2_666 ?
Mn1 O1 2.1870(13) . ?
Mn1 O5 2.1944(15) 2_666 ?
Mn1 O5 2.1944(15) . ?
Mn1 N1 2.2114(14) . ?
Mn1 N1 2.2114(14) 2_666 ?
N1 N2 1.332(2) . ?
N1 C1 1.338(2) . ?
C1 C2 1.395(2) . ?
C1 C4 1.501(2) . ?
C2 C3 1.379(2) . ?
C2 H21 0.91(2) . ?
C3 N2 1.345(2) . ?
C3 C5 1.486(2) . ?
N2 H22 0.87(2) . ?
C4 O2 1.246(2) . ?
C4 O1 1.263(2) . ?
C5 O4 1.251(2) . ?
C5 O3 1.261(2) . ?
O3 Mn2 2.1761(12) . ?
O5 H51 0.80(3) . ?
O5 H52 0.75(3) . ?
Mn2 O3 2.1761(12) 2_775 ?
Mn2 O7 2.1819(17) . ?
Mn2 O7 2.1819(17) 2_775 ?
Mn2 O6 2.1872(18) 2_775 ?
Mn2 O6 2.1872(18) . ?
O6 H61 0.71(3) . ?
O6 H62 0.79(4) . ?
O7 H71 0.77(3) . ?
O7 H72 0.83(4) . ?
O8 H81 0.81(3) . ?
O8 H82 0.83(3) . ?
O9 H91 0.88(4) . ?
O9 H92 0.81(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H22 O8 0.87(2) 2.00(2) 2.811(2) 156(2) 2_666
O5 H51 O2 0.80(3) 1.92(3) 2.725(2) 176(3) 2_766
O5 H52 O4 0.75(3) 2.01(3) 2.749(2) 173(3) 1_445
O6 H61 O9 0.71(3) 2.11(3) 2.817(2) 171(3) 2_665
O6 H62 O4 0.79(4) 1.97(4) 2.706(2) 155(3) 2_775
O7 H71 O9 0.77(3) 2.08(3) 2.847(2) 172(3) 1_565
O7 H72 O2 0.83(4) 1.94(4) 2.767(2) 174(3) 2_776
O8 H81 O4 0.81(3) 2.06(4) 2.824(2) 158(3) 2_766
O8 H82 O1 0.83(3) 2.08(3) 2.872(2) 161(3) .
O9 H91 O3 0.88(4) 2.07(4) 2.935(2) 167(4) .
O9 H92 O8 0.81(3) 2.04(3) 2.842(2) 172(3) 1_554
