#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:11:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179316 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/13/4321343.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_4321343
loop_
_publ_author_name
'M. Matzapetakis'
'N. Karligiano'
'A. Bino'
'M. Dakanali'
'C. P. Raptopoulou'
'V. Tangoulis'
'A. Terzis'
'J. Giapintzakis'
'A. Salifoglou'
_publ_section_title
;
 Manganese Citrate Chemistry: Syntheses, Spectroscopic Studies, and
 Structural Characterizations of Novel Mononuclear, Water-Soluble
 Manganese Citrate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4044
_journal_page_last               4051
_journal_paper_doi               10.1021/ic9912631
_journal_volume                  39
_journal_year                    2000
_chemical_formula_analytical     '[Mn(citrate)2](NH4)5'
_chemical_formula_structural     '[Mn(C6H4O7)2](NH4)5'
_chemical_formula_sum            'C12 H32 Mn N5 O16'
_chemical_formula_weight         557.37
_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
_cell_angle_alpha                91.05(1)
_cell_angle_beta                 105.60(1)
_cell_angle_gamma                119.16(1)
_cell_formula_units_Z            1
_cell_length_a                   9.606(3)
_cell_length_b                   9.914(3)
_cell_length_c                   7.247(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      4.9
_cell_volume                     571.3(4)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
'Crystal Logic Dual Goniometer diffractometer'
_diffrn_measurement_method       'theta-2theta 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  0.0056
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2304
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        -2.7
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      1.60
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.1079(66)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_obs          0.0309
_refine_ls_shift/esd_max         -0.990
_refine_ls_shift/esd_mean        0.093
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0308P)²+0.3801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0839
_refine_ls_wR_factor_obs         0.0823
_reflns_number_observed          2048
_reflns_number_total             2140
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9912631_2.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.3801P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.3801P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        571.3(3)
_cod_database_code               4321343
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn Mn 0.0000 0.0000 0.0000 0.0185(2) Uani 1 d S .
O1 O 0.0073(2) -0.20807(15) 0.0994(2) 0.0306(3) Uani 1 d . .
O3 O -0.19000(15) -0.14217(13) -0.2099(2) 0.0212(3) Uani 1 d . .
O5 O -0.1638(2) -0.04329(15) 0.1340(2) 0.0287(3) Uani 1 d . .
C1 C -0.1116(2) -0.3502(2) 0.0517(3) 0.0247(4) Uani 1 d . .
O2 O -0.0998(2) -0.4596(2) 0.1211(2) 0.0405(4) Uani 1 d . .
C2 C -0.2775(2) -0.3927(2) -0.1000(3) 0.0241(4) Uani 1 d . .
C3 C -0.3122(2) -0.2578(2) -0.1353(2) 0.0202(4) Uani 1 d . .
C4 C -0.2952(2) -0.1812(2) 0.0632(3) 0.0235(4) Uani 1 d . .
O4 O -0.3929(2) -0.2525(2) 0.1538(2) 0.0384(4) Uani 1 d . .
C5 C -0.4879(2) -0.3253(2) -0.2824(3) 0.0270(4) Uani 1 d . .
C6 C -0.5476(2) -0.2093(2) -0.3257(3) 0.0300(4) Uani 1 d . .
O6 O -0.6488(3) -0.2376(3) -0.4931(3) 0.0626(6) Uani 1 d . .
O7 O -0.5061(2) -0.1030(2) -0.1934(3) 0.0554(5) Uani 1 d . .
N1 N 0.2957(3) -0.2311(2) 0.0983(3) 0.0361(4) Uani 1 d . .
N2 N 0.2288(3) -0.0326(3) 0.5109(3) 0.0375(4) Uani 1 d . .
N3 N 0.0000 0.5000 0.5000 0.084(2) Uani 1 d S .
OW O 0.1198(3) 0.2633(3) 0.4955(3) 0.0568(5) Uani 1 d . .
H2A H -0.2801(27) -0.4387(25) -0.2239(33) 0.027(5) Uiso 1 d . .
H2B H -0.3621(31) -0.4701(28) -0.0650(33) 0.031(6) Uiso 1 d . .
H5A H -0.4896(30) -0.3715(28) -0.4012(37) 0.035(6) Uiso 1 d . .
H5B H -0.5661(32) -0.4084(30) -0.2343(36) 0.038(6) Uiso 1 d . .
HN1A H 0.2361(37) -0.3238(37) 0.0234(43) 0.048(7) Uiso 1 d . .
HN1B H 0.3742(49) -0.1667(45) 0.0633(54) 0.075(11) Uiso 1 d . .
HN1C H 0.2190(47) -0.2080(39) 0.0844(49) 0.067(10) Uiso 1 d . .
HN1D H 0.3377(39) -0.2326(35) 0.2181(51) 0.055(8) Uiso 1 d . .
HN2A H 0.2815(42) -0.0935(39) 0.5241(47) 0.067(9) Uiso 1 d . .
HN2B H 0.2307(39) 0.0264(37) 0.4091(50) 0.061(8) Uiso 1 d . .
HN2C H 0.2785(46) 0.0351(44) 0.6081(57) 0.073(11) Uiso 1 d . .
HN2D H 0.1262(48) -0.1002(41) 0.5027(47) 0.063(10) Uiso 1 d . .
HN3A H -0.0283(85) 0.5105(88) 0.3784(111) 0.053(17) Uiso 0.50 d P .
HN3B H 0.1167(109) 0.5654(113) 0.5020(106) 0.056(20) Uiso 0.50 d P .
HN3C H -0.0346(351) 0.4412(209) 0.4502(374) 0.213(95) Uiso 0.50 d P .
HN3D H -0.0575(173) 0.5929(177) 0.4850(186) 0.195(48) Uiso 0.50 d P .
HWA H 0.1459(43) 0.2334(40) 0.4142(54) 0.065(10) Uiso 1 d . .
HWB H 0.0743(110) 0.2939(118) 0.4609(130) 0.199(45) Uiso 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
O3 Mn O3 180.0 . 2 ?
O3 Mn O5 83.98(6) . . ?
O3 Mn O5 96.02(6) 2 . ?
O3 Mn O5 96.02(6) . 2 ?
O3 Mn O5 83.98(6) 2 2 ?
O5 Mn O5 180.0 . 2 ?
O3 Mn O1 93.30(5) . 2 ?
O3 Mn O1 86.70(5) 2 2 ?
O5 Mn O1 93.13(6) . 2 ?
O5 Mn O1 86.87(6) 2 2 ?
O3 Mn O1 86.70(5) . . ?
O3 Mn O1 93.30(5) 2 . ?
O5 Mn O1 86.87(6) . . ?
O5 Mn O1 93.13(6) 2 . ?
O1 Mn O1 180.0 2 . ?
C1 O1 Mn 127.30(12) . . ?
C3 O3 Mn 109.05(10) . . ?
C4 O5 Mn 110.85(11) . . ?
O2 C1 O1 123.4(2) . . ?
O2 C1 C2 117.1(2) . . ?
O1 C1 C2 119.5(2) . . ?
C1 C2 C3 116.25(14) . . ?
O3 C3 C5 109.81(14) . . ?
O3 C3 C2 110.07(14) . . ?
C5 C3 C2 108.38(14) . . ?
O3 C3 C4 108.35(13) . . ?
C5 C3 C4 112.59(15) . . ?
C2 C3 C4 107.61(14) . . ?
O4 C4 O5 122.6(2) . . ?
O4 C4 C3 121.8(2) . . ?
O5 C4 C3 115.30(15) . . ?
C6 C5 C3 115.6(2) . . ?
O7 C6 O6 124.5(2) . . ?
O7 C6 C5 119.3(2) . . ?
O6 C6 C5 115.9(2) . . ?
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
Mn O3 1.8849(13) . ?
Mn O3 1.8849(13) 2 ?
Mn O5 1.9451(14) . ?
Mn O5 1.9451(14) 2 ?
Mn O1 2.2242(14) 2 ?
Mn O1 2.2242(14) . ?
O1 C1 1.269(2) . ?
O3 C3 1.427(2) . ?
O5 C4 1.292(2) . ?
C1 O2 1.246(2) . ?
C1 C2 1.520(3) . ?
C2 C3 1.539(2) . ?
C3 C5 1.529(2) . ?
C3 C4 1.544(2) . ?
C4 O4 1.230(2) . ?
C5 C6 1.520(3) . ?
C6 O7 1.240(3) . ?
C6 O6 1.258(3) . ?
