#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:55:11 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179870 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/66/7016645.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_7016645
loop_
_publ_author_name
'Drahoš, Bohuslav'
'Pniok, Miroslav'
'Havlíčková, Jana'
'Kotek, Jan'
'Císařová, Ivana'
'Hermann, Petr'
'Lukeš, Ivan'
'Tóth, Eva'
_publ_section_title
;
 Mn(2+) complexes of 1-oxa-4,7-diazacyclononane based ligands with
 acetic, phosphonic and phosphinic acid pendant arms: Stability and
 relaxation studies.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10131
_journal_page_last               10146
_journal_paper_doi               10.1039/c1dt10543d
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C40 H52 Mn2 N4 O10 P4, 2(H2 O)'
_chemical_formula_sum            'C40 H56 Mn2 N4 O12 P4'
_chemical_formula_weight         1018.65
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.556(5)
_cell_angle_beta                 87.468(5)
_cell_angle_gamma                76.778(4)
_cell_formula_units_Z            1
_cell_length_a                   7.8641(10)
_cell_length_b                   9.9409(14)
_cell_length_c                   15.085(2)
_cell_measurement_temperature    150(1)
_cell_volume                     1132.4(3)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5122
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0383
_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)+(0.0000P)²+2.0665P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                4558
_reflns_number_total             5122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10543d.txt
_cod_data_source_block           mnphp
_cod_original_cell_volume        1132.5(3)
_cod_database_code               7016645
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 0.44895(5) 0.69422(4) 0.85748(3) 0.01250(9) Uani 1 1 d .
O1 O 0.5093(3) 0.90455(19) 0.88219(13) 0.0199(4) Uani 1 1 d .
C2 C 0.5490(4) 0.9966(3) 0.8036(2) 0.0235(6) Uani 1 1 d .
H21 H 0.6749 0.9969 0.8027 0.028 Uiso 1 1 calc R
H22 H 0.4816 1.0933 0.8056 0.028 Uiso 1 1 calc R
C3 C 0.5029(4) 0.9476(3) 0.71945(19) 0.0202(6) Uani 1 1 d .
H31 H 0.3744 0.9703 0.7127 0.024 Uiso 1 1 calc R
H32 H 0.5530 0.9978 0.6662 0.024 Uiso 1 1 calc R
N4 N 0.5709(3) 0.7943(2) 0.72357(15) 0.0162(5) Uani 1 1 d .
C5 C 0.7653(3) 0.7554(3) 0.7226(2) 0.0206(6) Uani 1 1 d .
H51 H 0.8117 0.8354 0.7342 0.025 Uiso 1 1 calc R
H52 H 0.8073 0.7336 0.6626 0.025 Uiso 1 1 calc R
C6 C 0.8322(3) 0.6291(3) 0.79377(19) 0.0196(6) Uani 1 1 d .
H61 H 0.8068 0.5449 0.7750 0.024 Uiso 1 1 calc R
H62 H 0.9606 0.6142 0.7985 0.024 Uiso 1 1 calc R
N7 N 0.7515(3) 0.6464(2) 0.88313(16) 0.0176(5) Uani 1 1 d .
C8 C 0.8034(4) 0.7624(3) 0.9192(2) 0.0254(6) Uani 1 1 d .
H81 H 0.8672 0.8134 0.8720 0.030 Uiso 1 1 calc R
H82 H 0.8828 0.7229 0.9707 0.030 Uiso 1 1 calc R
C9 C 0.6434(4) 0.8641(3) 0.9493(2) 0.0255(6) Uani 1 1 d .
H91 H 0.5963 0.8194 1.0056 0.031 Uiso 1 1 calc R
H92 H 0.6784 0.9485 0.9619 0.031 Uiso 1 1 calc R
C10 C 0.4983(4) 0.7436(3) 0.65011(18) 0.0197(6) Uani 1 1 d .
H101 H 0.5662 0.6482 0.6447 0.024 Uiso 1 1 calc R
H102 H 0.5102 0.8054 0.5927 0.024 Uiso 1 1 calc R
P1 P 0.26642(9) 0.73946(7) 0.66947(4) 0.01486(14) Uani 1 1 d .
O11 O 0.2403(2) 0.72436(19) 0.77071(12) 0.0159(4) Uani 1 1 d .
O12 O 0.1518(3) 0.8615(2) 0.61309(13) 0.0221(4) Uani 1 1 d .
C11 C 0.2487(4) 0.5796(3) 0.6324(2) 0.0213(6) Uani 1 1 d .
C12 C 0.2677(4) 0.4543(3) 0.6908(2) 0.0323(7) Uani 1 1 d .
H121 H 0.2875 0.4513 0.7528 0.039 Uiso 1 1 calc R
C13 C 0.2578(5) 0.3324(4) 0.6587(3) 0.0443(10) Uani 1 1 d .
H131 H 0.2689 0.2468 0.6991 0.053 Uiso 1 1 calc R
C14 C 0.2317(5) 0.3362(4) 0.5677(3) 0.0497(11) Uani 1 1 d .
H141 H 0.2277 0.2529 0.5455 0.060 Uiso 1 1 calc R
C15 C 0.2118(6) 0.4600(5) 0.5104(3) 0.0515(11) Uani 1 1 d .
H151 H 0.1929 0.4626 0.4483 0.062 Uiso 1 1 calc R
C16 C 0.2189(5) 0.5819(4) 0.5417(2) 0.0390(8) Uani 1 1 d .
H161 H 0.2035 0.6676 0.5012 0.047 Uiso 1 1 calc R
C20 C 0.7957(4) 0.5131(3) 0.94553(19) 0.0190(6) Uani 1 1 d .
H201 H 0.7732 0.5323 1.0078 0.023 Uiso 1 1 calc R
H202 H 0.9221 0.4718 0.9399 0.023 Uiso 1 1 calc R
P2 P 0.67201(9) 0.38530(7) 0.92549(4) 0.01337(14) Uani 1 1 d .
O21 O 0.5066(2) 0.46891(19) 0.87869(13) 0.0169(4) Uani 1 1 d .
O22 O 0.6593(3) 0.29508(19) 1.01505(12) 0.0200(4) Uani 1 1 d .
C21 C 0.7939(3) 0.2699(3) 0.85311(18) 0.0145(5) Uani 1 1 d .
C22 C 0.9290(4) 0.1580(3) 0.8886(2) 0.0221(6) Uani 1 1 d .
H221 H 0.9569 0.1444 0.9505 0.027 Uiso 1 1 calc R
C23 C 1.0223(4) 0.0669(3) 0.8337(2) 0.0293(7) Uani 1 1 d .
H231 H 1.1151 -0.0077 0.8579 0.035 Uiso 1 1 calc R
C24 C 0.9799(4) 0.0850(3) 0.7441(2) 0.0334(8) Uani 1 1 d .
H241 H 1.0433 0.0223 0.7067 0.040 Uiso 1 1 calc R
C25 C 0.8456(5) 0.1939(3) 0.7083(2) 0.0299(7) Uani 1 1 d .
H251 H 0.8168 0.2052 0.6467 0.036 Uiso 1 1 calc R
C26 C 0.7522(4) 0.2871(3) 0.76241(19) 0.0220(6) Uani 1 1 d .
H261 H 0.6606 0.3621 0.7375 0.026 Uiso 1 1 calc R
O1W O 0.2015(3) 0.0429(3) 0.45543(16) 0.0429(6) Uani 1 1 d .
H11W H 0.1008 0.0722 0.4379 0.064 Uiso 1 1 d R
H12W H 0.1942 -0.0118 0.5015 0.064 Uiso 1 1 d R
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
O22 Mn1 O11 106.17(8) 2_667 .
O22 Mn1 O21 93.03(7) 2_667 .
O11 Mn1 O21 96.59(7) . .
O22 Mn1 O1 80.14(7) 2_667 .
O11 Mn1 O1 112.72(7) . .
O21 Mn1 O1 150.67(7) . .
O22 Mn1 N7 103.46(8) 2_667 .
O11 Mn1 N7 150.32(8) . .
O21 Mn1 N7 80.07(7) . .
O1 Mn1 N7 73.99(7) . .
O22 Mn1 N4 151.77(8) 2_667 .
O11 Mn1 N4 80.19(7) . .
O21 Mn1 N4 113.86(7) . .
O1 Mn1 N4 72.19(7) . .
N7 Mn1 N4 74.50(8) . .
C9 O1 C2 114.5(2) . .
C9 O1 Mn1 104.80(15) . .
C2 O1 Mn1 116.39(16) . .
O1 C2 C3 109.8(2) . .
O1 C2 H21 109.7 . .
C3 C2 H21 109.7 . .
O1 C2 H22 109.7 . .
C3 C2 H22 109.7 . .
H21 C2 H22 108.2 . .
N4 C3 C2 111.2(2) . .
N4 C3 H31 109.4 . .
C2 C3 H31 109.4 . .
N4 C3 H32 109.4 . .
C2 C3 H32 109.4 . .
H31 C3 H32 108.0 . .
C10 N4 C3 110.7(2) . .
C10 N4 C5 111.1(2) . .
C3 N4 C5 112.0(2) . .
C10 N4 Mn1 105.59(15) . .
C3 N4 Mn1 104.35(15) . .
C5 N4 Mn1 112.75(16) . .
N4 C5 C6 110.6(2) . .
N4 C5 H51 109.5 . .
C6 C5 H51 109.5 . .
N4 C5 H52 109.5 . .
C6 C5 H52 109.5 . .
H51 C5 H52 108.1 . .
N7 C6 C5 112.2(2) . .
N7 C6 H61 109.2 . .
C5 C6 H61 109.2 . .
N7 C6 H62 109.2 . .
C5 C6 H62 109.2 . .
H61 C6 H62 107.9 . .
C20 N7 C6 110.2(2) . .
C20 N7 C8 111.9(2) . .
C6 N7 C8 111.1(2) . .
C20 N7 Mn1 106.96(16) . .
C6 N7 Mn1 104.47(16) . .
C8 N7 Mn1 111.88(16) . .
N7 C8 C9 110.9(2) . .
N7 C8 H81 109.5 . .
C9 C8 H81 109.5 . .
N7 C8 H82 109.5 . .
C9 C8 H82 109.5 . .
H81 C8 H82 108.0 . .
O1 C9 C8 111.7(2) . .
O1 C9 H91 109.3 . .
C8 C9 H91 109.3 . .
O1 C9 H92 109.3 . .
C8 C9 H92 109.3 . .
H91 C9 H92 107.9 . .
N4 C10 P1 112.00(18) . .
N4 C10 H101 109.2 . .
P1 C10 H101 109.2 . .
N4 C10 H102 109.2 . .
P1 C10 H102 109.2 . .
H101 C10 H102 107.9 . .
O12 P1 O11 117.52(11) . .
O12 P1 C11 109.47(13) . .
O11 P1 C11 109.07(13) . .
O12 P1 C10 110.58(12) . .
O11 P1 C10 105.51(12) . .
C11 P1 C10 103.76(13) . .
P1 O11 Mn1 121.57(10) . .
C12 C11 C16 119.0(3) . .
C12 C11 P1 122.1(2) . .
C16 C11 P1 118.9(2) . .
C11 C12 C13 120.1(3) . .
C11 C12 H121 119.9 . .
C13 C12 H121 119.9 . .
C14 C13 C12 120.0(4) . .
C14 C13 H131 120.0 . .
C12 C13 H131 120.0 . .
C15 C14 C13 119.7(3) . .
C15 C14 H141 120.1 . .
C13 C14 H141 120.1 . .
C14 C15 C16 120.8(4) . .
C14 C15 H151 119.6 . .
C16 C15 H151 119.6 . .
C15 C16 C11 120.3(4) . .
C15 C16 H161 119.8 . .
C11 C16 H161 119.8 . .
N7 C20 P2 113.48(18) . .
N7 C20 H201 108.9 . .
P2 C20 H201 108.9 . .
N7 C20 H202 108.9 . .
P2 C20 H202 108.9 . .
H201 C20 H202 107.7 . .
O22 P2 O21 119.18(11) . .
O22 P2 C21 105.91(11) . .
O21 P2 C21 109.12(12) . .
O22 P2 C20 106.00(12) . .
O21 P2 C20 106.14(11) . .
C21 P2 C20 110.36(13) . .
P2 O21 Mn1 120.62(10) . .
P2 O22 Mn1 141.24(12) . 2_667
C26 C21 C22 119.2(2) . .
C26 C21 P2 120.9(2) . .
C22 C21 P2 119.9(2) . .
C23 C22 C21 120.4(3) . .
C23 C22 H221 119.8 . .
C21 C22 H221 119.8 . .
C24 C23 C22 119.9(3) . .
C24 C23 H231 120.1 . .
C22 C23 H231 120.1 . .
C23 C24 C25 120.4(3) . .
C23 C24 H241 119.8 . .
C25 C24 H241 119.8 . .
C24 C25 C26 120.4(3) . .
C24 C25 H251 119.8 . .
C26 C25 H251 119.8 . .
C21 C26 C25 119.8(3) . .
C21 C26 H261 120.1 . .
C25 C26 H261 120.1 . .
H11W O1W H12W 104.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O22 2.0772(19) 2_667
Mn1 O11 2.0816(18) .
Mn1 O21 2.1535(18) .
Mn1 O1 2.3371(19) .
Mn1 N7 2.353(2) .
Mn1 N4 2.366(2) .
O1 C9 1.436(3) .
O1 C2 1.443(3) .
C2 C3 1.519(4) .
C2 H21 0.9900 .
C2 H22 0.9900 .
C3 N4 1.487(3) .
C3 H31 0.9900 .
C3 H32 0.9900 .
N4 C10 1.476(4) .
N4 C5 1.489(3) .
C5 C6 1.521(4) .
C5 H51 0.9900 .
C5 H52 0.9900 .
C6 N7 1.484(4) .
C6 H61 0.9900 .
C6 H62 0.9900 .
N7 C20 1.473(3) .
N7 C8 1.495(3) .
C8 C9 1.526(4) .
C8 H81 0.9900 .
C8 H82 0.9900 .
C9 H91 0.9900 .
C9 H92 0.9900 .
C10 P1 1.842(3) .
C10 H101 0.9900 .
C10 H102 0.9900 .
P1 O12 1.495(2) .
P1 O11 1.5194(18) .
P1 C11 1.804(3) .
C11 C12 1.384(4) .
C11 C16 1.394(4) .
C12 C13 1.396(5) .
C12 H121 0.9500 .
C13 C14 1.390(6) .
C13 H131 0.9500 .
C14 C15 1.365(6) .
C14 H141 0.9500 .
C15 C16 1.384(5) .
C15 H151 0.9500 .
C16 H161 0.9500 .
C20 P2 1.836(3) .
C20 H201 0.9900 .
C20 H202 0.9900 .
P2 O22 1.5070(19) .
P2 O21 1.5083(19) .
P2 C21 1.801(3) .
O22 Mn1 2.0772(19) 2_667
C21 C26 1.395(4) .
C21 C22 1.402(4) .
C22 C23 1.391(4) .
C22 H221 0.9500 .
C23 C24 1.380(5) .
C23 H231 0.9500 .
C24 C25 1.383(5) .
C24 H241 0.9500 .
C25 C26 1.396(4) .
C25 H251 0.9500 .
C26 H261 0.9500 .
O1W H11W 0.8178 .
O1W H12W 0.8177 .
