#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/27/1512735.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_1512735
loop_
_publ_author_name
'Eleonora Freire'
'Mariano Quintero'
'Daniel Vega'
'Ricardo Baggio'
_publ_section_title
;
 Crystal structure and magnetic properties of two new zoledronate
 complexes: A Mn dimer [Mn(II)(H3Zol)2(H2O)2] and a Fe15 molecular cluster
 [Fe(III)15(HZol)10(H2Zol)2 (H2O)12(Cl4:(H2O)2)Cl7(H2O)65] (where H4Zol:
 C5H10N2O7P2 is zoledronic acid)
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              229
_journal_page_last               236
_journal_volume                  393
_journal_year                    2012
_chemical_formula_iupac          'Mn (P2 O7 N2 C5 H9)2 (H2 O)2'
_chemical_formula_moiety         'C10 H22 Mn N4 O16 P4'
_chemical_formula_sum            'C10 H22 Mn N4 O16 P4'
_chemical_formula_weight         633.14
_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
_cell_angle_alpha                105.32(3)
_cell_angle_beta                 110.90(3)
_cell_angle_gamma                97.48(3)
_cell_formula_units_Z            1
_cell_length_a                   7.4810(15)
_cell_length_b                   8.6030(17)
_cell_length_c                   9.7300(19)
_cell_measurement_reflns_used    1244
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.87
_cell_volume                     546.4(3)
_computing_cell_refinement       'CrysAlisPro '
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro '
_computing_molecular_graphics    'SHELXTL   (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97, PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (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  'CCD Oxford Diffraction Gemini S Ultra'
_diffrn_measurement_method       'ω scans, thick slices'
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5594
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, Oxford Diffraction (2009) '
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             323
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2142
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0342
_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)+(0.0513P)²+0.1793P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                1692
_reflns_number_total             2142
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ICA-2013-394-229-236-1.cif
_cod_data_source_block           (I)
_cod_original_cell_volume        546.39(27)
_cod_database_code               1512735
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
Mn1 Mn 0.5000 0.5000 0.5000 0.01907(17) Uani 1 2 d S
P1 P 0.15028(10) 0.22033(9) 0.16614(8) 0.02028(19) Uani 1 1 d .
P2 P 0.12152(10) 0.22430(9) 0.47741(8) 0.01765(18) Uani 1 1 d .
O1 O 0.3015(3) 0.3847(2) 0.2550(2) 0.0263(5) Uani 1 1 d .
O2 O 0.2628(3) 0.0792(3) 0.1829(2) 0.0272(5) Uani 1 1 d D
H2O H 0.180(5) -0.014(3) 0.130(4) 0.068(15) Uiso 1 1 d D
O3 O 0.0265(3) 0.1932(2) -0.0029(2) 0.0256(4) Uani 1 1 d .
O4 O 0.2784(3) 0.3844(2) 0.5558(2) 0.0231(4) Uani 1 1 d .
O5 O 0.2223(3) 0.0750(3) 0.4758(2) 0.0256(4) Uani 1 1 d D
H5O H 0.150(5) -0.013(3) 0.469(5) 0.056(12) Uiso 1 1 d D
O6 O -0.0295(3) 0.2084(2) 0.5462(2) 0.0228(4) Uani 1 1 d .
O7 O -0.1597(3) 0.0459(3) 0.1924(2) 0.0259(4) Uani 1 1 d D
H7O H -0.116(5) -0.034(3) 0.156(4) 0.039 Uiso 1 1 d D
N1 N -0.2487(3) 0.3450(3) 0.1185(3) 0.0244(5) Uani 1 1 d .
N2 N -0.3440(5) 0.4172(4) -0.0862(3) 0.0402(7) Uani 1 1 d D
H2N H -0.345(6) 0.472(5) -0.148(4) 0.059(12) Uiso 1 1 d D
C1 C -0.0146(4) 0.2023(3) 0.2686(3) 0.0191(5) Uani 1 1 d .
C2 C -0.1267(4) 0.3406(4) 0.2730(3) 0.0258(6) Uani 1 1 d .
H2B H -0.2109 0.3253 0.3269 0.031 Uiso 1 1 calc R
H2A H -0.0315 0.4474 0.3330 0.031 Uiso 1 1 calc R
C3 C -0.2059(5) 0.4591(4) 0.0572(4) 0.0331(7) Uani 1 1 d .
H3 H -0.0984 0.5514 0.1065 0.040 Uiso 1 1 calc R
C4 C -0.4784(5) 0.2756(5) -0.1171(4) 0.0419(8) Uani 1 1 d .
H4 H -0.5897 0.2205 -0.2096 0.050 Uiso 1 1 calc R
C5 C -0.4197(5) 0.2306(4) 0.0114(4) 0.0348(7) Uani 1 1 d .
H5 H -0.4835 0.1391 0.0247 0.042 Uiso 1 1 calc R
O1W O 0.3866(3) 0.7250(3) 0.4906(3) 0.0424(6) Uani 1 1 d D
H1WB H 0.280(4) 0.749(6) 0.488(6) 0.074(15) Uiso 1 1 d D
H1WA H 0.465(6) 0.817(4) 0.512(8) 0.15(3) Uiso 1 1 d 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'
P P 0.1023 0.0942 '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
O4 Mn1 O4 180.0 . 2_666
O4 Mn1 O1 88.27(8) . .
O4 Mn1 O1 91.73(8) 2_666 .
O4 Mn1 O1 91.73(8) . 2_666
O4 Mn1 O1 88.27(8) 2_666 2_666
O1 Mn1 O1 180.0 . 2_666
O4 Mn1 O1W 84.53(9) . 2_666
O4 Mn1 O1W 95.47(9) 2_666 2_666
O1 Mn1 O1W 92.94(10) . 2_666
O1 Mn1 O1W 87.06(10) 2_666 2_666
O4 Mn1 O1W 95.47(9) . .
O4 Mn1 O1W 84.53(9) 2_666 .
O1 Mn1 O1W 87.06(10) . .
O1 Mn1 O1W 92.94(10) 2_666 .
O1W Mn1 O1W 180.000(1) 2_666 .
O1 P1 O3 115.50(12) . .
O1 P1 O2 107.39(12) . .
O3 P1 O2 111.09(12) . .
O1 P1 C1 107.97(12) . .
O3 P1 C1 109.17(12) . .
O2 P1 C1 105.17(12) . .
O4 P2 O6 115.32(11) . .
O4 P2 O5 109.09(11) . .
O6 P2 O5 110.22(11) . .
O4 P2 C1 108.56(12) . .
O6 P2 C1 107.45(12) . .
O5 P2 C1 105.74(12) . .
P1 O1 Mn1 131.97(12) . .
P1 O2 H2O 108(3) . .
P2 O4 Mn1 134.30(12) . .
P2 O5 H5O 114(3) . .
C1 O7 H7O 113(2) . .
C3 N1 C5 108.7(3) . .
C3 N1 C2 125.2(3) . .
C5 N1 C2 126.0(3) . .
C3 N2 C4 109.3(3) . .
C3 N2 H2N 124(3) . .
C4 N2 H2N 127(3) . .
O7 C1 C2 107.3(2) . .
O7 C1 P1 111.02(18) . .
C2 C1 P1 111.98(19) . .
O7 C1 P2 108.44(18) . .
C2 C1 P2 104.66(18) . .
P1 C1 P2 113.10(14) . .
N1 C2 C1 114.2(2) . .
N1 C2 H2B 108.7 . .
C1 C2 H2B 108.7 . .
N1 C2 H2A 108.7 . .
C1 C2 H2A 108.7 . .
H2B C2 H2A 107.6 . .
N2 C3 N1 107.8(3) . .
N2 C3 H3 126.1 . .
N1 C3 H3 126.1 . .
C5 C4 N2 107.1(3) . .
C5 C4 H4 126.4 . .
N2 C4 H4 126.4 . .
C4 C5 N1 107.0(3) . .
C4 C5 H5 126.5 . .
N1 C5 H5 126.5 . .
Mn1 O1W H1WB 133(3) . .
Mn1 O1W H1WA 120(4) . .
H1WB O1W H1WA 105(4) . .
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 O4 2.1281(19) . y
Mn1 O4 2.1281(19) 2_666 ?
Mn1 O1 2.171(2) . y
Mn1 O1 2.171(2) 2_666 ?
Mn1 O1W 2.222(2) 2_666 ?
Mn1 O1W 2.222(2) . y
P1 O1 1.506(2) . ?
P1 O3 1.507(2) . ?
P1 O2 1.576(2) . ?
P1 C1 1.857(3) . ?
P2 O4 1.497(2) . ?
P2 O6 1.5138(19) . ?
P2 O5 1.571(2) . ?
P2 C1 1.863(3) . ?
O2 H2O 0.846(10) . ?
O5 H5O 0.843(10) . ?
O7 C1 1.434(3) . ?
O7 H7O 0.846(10) . ?
N1 C3 1.336(4) . ?
N1 C5 1.368(4) . ?
N1 C2 1.467(3) . ?
N2 C3 1.324(4) . ?
N2 C4 1.362(5) . ?
N2 H2N 0.853(10) . ?
C1 C2 1.543(4) . ?
C2 H2B 0.9700 . ?
C2 H2A 0.9700 . ?
C3 H3 0.9300 . ?
C4 C5 1.347(5) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
O1W H1WB 0.843(10) . ?
O1W H1WA 0.846(10) . ?
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
O1W H1WA O5 0.846(10) 2.35(3) 3.056(3) 141(5) 2_666
O1W H1WB O6 0.843(10) 1.885(12) 2.724(3) 173(5) 2_566
O2 H2O O3 0.846(10) 1.817(13) 2.655(3) 170(4) 2
O7 H7O O3 0.846(10) 2.102(16) 2.909(3) 159(3) 2
O5 H5O O6 0.843(10) 1.743(12) 2.580(3) 172(4) 2_556
N2 H2N O1 0.853(10) 1.880(13) 2.723(3) 169(4) 2_565
