#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179861 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/57/7015706.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_7015706
loop_
_publ_author_name
'Türkoglu, Gazi'
'Heinemann, Frank W.'
'Burzlaff, Nicolai'
_publ_section_title
;
 Transition metal complexes bearing a
 2,2-bis(3,5-dimethylpyrazol-1-yl)propionate ligand: one methyl more
 matters.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4678
_journal_page_last               4686
_journal_paper_doi               10.1039/c1dt00022e
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H17 Mn1 N4 O5'
_chemical_formula_sum            'C16 H17 Mn N4 O5'
_chemical_formula_weight         400.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2010-04-23T14:09:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                105.882(4)
_cell_angle_beta                 99.171(6)
_cell_angle_gamma                104.865(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2964(6)
_cell_length_b                   9.6530(3)
_cell_length_c                   11.393
_cell_measurement_reflns_used    152
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      6
_cell_measurement_wavelength     0.71073
_cell_volume                     821.94(7)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
φ- and ω-rotations with 2.00 ° and 40 sec per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20009
_diffrn_reflns_theta_full        28.5
_diffrn_reflns_theta_max         28.5
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.893648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[σ²(Fo²)+(0.0210P)²+0.5353P] where
P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                3168
_reflns_number_total             4148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt00022e.txt
_cod_data_source_block           gtbu07
_cod_original_cell_volume        821.92(6)
_cod_database_code               7015706
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
C1 C 0.5234(2) 0.4110(2) 0.22359(16) 0.0131(4) Uani 1 1 d . . .
C2 C 0.3244(2) 0.3430(2) 0.15332(16) 0.0119(4) Uani 1 1 d . . .
C3 C 0.2900(3) 0.4333(2) 0.06794(18) 0.0182(4) Uani 1 1 d . . .
H3A H 0.3618 0.4266 0.0097 0.027 Uiso 1 1 calc R . .
H3B H 0.3151 0.5377 0.1178 0.027 Uiso 1 1 calc R . .
H3C H 0.1713 0.393 0.0222 0.027 Uiso 1 1 calc R . .
C11 C 0.1230(3) 0.2396(2) 0.51302(18) 0.0210(4) Uani 1 1 d . . .
H11A H 0.1251 0.1368 0.4899 0.031 Uiso 1 1 calc R . .
H11B H 0.0185 0.2437 0.5376 0.031 Uiso 1 1 calc R . .
H11C H 0.2199 0.3028 0.5821 0.031 Uiso 1 1 calc R . .
C12 C 0.1318(2) 0.2952(2) 0.40292(17) 0.0150(4) Uani 1 1 d . . .
C13 C 0.0302(2) 0.3745(2) 0.35910(17) 0.0166(4) Uani 1 1 d . . .
H13 H -0.0588 0.3994 0.3911 0.02 Uiso 1 1 calc R . .
C14 C 0.0854(2) 0.4088(2) 0.26081(17) 0.0141(4) Uani 1 1 d . . .
C15 C 0.0129(3) 0.4970(2) 0.1887(2) 0.0217(4) Uani 1 1 d . . .
H15A H -0.085 0.516 0.2166 0.033 Uiso 1 1 calc R . .
H15B H -0.0217 0.4397 0.1005 0.033 Uiso 1 1 calc R . .
H15C H 0.099 0.5919 0.2029 0.033 Uiso 1 1 calc R . .
C21 C 0.3590(3) -0.1716(2) 0.08751(19) 0.0200(4) Uani 1 1 d . . .
H21A H 0.4779 -0.1364 0.1324 0.03 Uiso 1 1 calc R . .
H21B H 0.3415 -0.2519 0.0105 0.03 Uiso 1 1 calc R . .
H21C H 0.2885 -0.2088 0.1384 0.03 Uiso 1 1 calc R . .
C22 C 0.3110(2) -0.0436(2) 0.05830(17) 0.0149(4) Uani 1 1 d . . .
C23 C 0.2221(2) -0.0469(2) -0.05778(17) 0.0169(4) Uani 1 1 d . . .
H23 H 0.1805 -0.1298 -0.1316 0.02 Uiso 1 1 calc R . .
C24 C 0.2074(2) 0.0950(2) -0.04275(16) 0.0151(4) Uani 1 1 d . . .
C25 C 0.1168(3) 0.1418(2) -0.14268(18) 0.0240(5) Uani 1 1 d . . .
H25A H 0.0286 0.1796 -0.1142 0.036 Uiso 1 1 calc R . .
H25B H 0.0658 0.0559 -0.2182 0.036 Uiso 1 1 calc R . .
H25C H 0.198 0.2201 -0.1596 0.036 Uiso 1 1 calc R . .
C31 C 0.5138(2) 0.2635(2) 0.50765(18) 0.0167(4) Uani 1 1 d . . .
C41 C 0.3037(2) 0.0093(2) 0.35604(17) 0.0150(4) Uani 1 1 d . . .
C51 C 0.6095(2) 0.0969(2) 0.34128(17) 0.0164(4) Uani 1 1 d . . .
Mn1 Mn 0.43479(4) 0.17730(3) 0.33767(3) 0.01206(8) Uani 1 1 d . . .
N11 N 0.24501(19) 0.27814(17) 0.33289(14) 0.0128(3) Uani 1 1 d . . .
N12 N 0.21755(19) 0.34945(16) 0.24531(13) 0.0118(3) Uani 1 1 d . . .
N21 N 0.34967(19) 0.09433(16) 0.14369(14) 0.0120(3) Uani 1 1 d . . .
N22 N 0.28811(19) 0.18105(17) 0.08071(13) 0.0117(3) Uani 1 1 d . . .
O1 O 0.57696(16) 0.36249(14) 0.31048(12) 0.0166(3) Uani 1 1 d . . .
O2 O 0.61310(17) 0.50645(15) 0.18845(13) 0.0213(3) Uani 1 1 d . . .
O31 O 0.56657(19) 0.31374(17) 0.61490(13) 0.0267(3) Uani 1 1 d . . .
O41 O 0.22161(19) -0.10098(16) 0.36651(13) 0.0243(3) Uani 1 1 d . . .
O51 O 0.71802(19) 0.04402(17) 0.34889(13) 0.0269(3) Uani 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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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
O2 C1 O1 125.32(17) . . ?
O2 C1 C2 116.69(16) . . ?
O1 C1 C2 117.98(15) . . ?
N12 C2 N22 107.37(13) . . ?
N12 C2 C3 111.91(14) . . ?
N22 C2 C3 111.54(14) . . ?
N12 C2 C1 110.58(14) . . ?
N22 C2 C1 107.94(14) . . ?
C3 C2 C1 107.46(14) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N11 C12 C13 109.57(16) . . ?
N11 C12 C11 123.73(17) . . ?
C13 C12 C11 126.67(17) . . ?
C14 C13 C12 107.54(16) . . ?
C14 C13 H13 126.2 . . ?
C12 C13 H13 126.2 . . ?
C13 C14 N12 106.50(16) . . ?
C13 C14 C15 124.72(17) . . ?
N12 C14 C15 128.77(16) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N21 C22 C23 109.93(16) . . ?
N21 C22 C21 123.32(17) . . ?
C23 C22 C21 126.75(17) . . ?
C24 C23 C22 107.32(16) . . ?
C24 C23 H23 126.3 . . ?
C22 C23 H23 126.3 . . ?
C23 C24 N22 106.35(16) . . ?
C23 C24 C25 125.60(17) . . ?
N22 C24 C25 128.04(17) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O31 C31 Mn1 177.43(17) . . ?
O41 C41 Mn1 178.34(17) . . ?
O51 C51 Mn1 176.42(16) . . ?
C41 Mn1 C51 88.24(8) . . ?
C41 Mn1 C31 90.46(8) . . ?
C51 Mn1 C31 87.29(8) . . ?
C41 Mn1 O1 177.92(7) . . ?
C51 Mn1 O1 92.25(7) . . ?
C31 Mn1 O1 91.58(7) . . ?
C41 Mn1 N11 94.65(7) . . ?
C51 Mn1 N11 177.10(8) . . ?
C31 Mn1 N11 92.57(7) . . ?
O1 Mn1 N11 84.86(6) . . ?
C41 Mn1 N21 93.21(7) . . ?
C51 Mn1 N21 94.31(7) . . ?
C31 Mn1 N21 176.04(7) . . ?
O1 Mn1 N21 84.74(6) . . ?
N11 Mn1 N21 85.65(6) . . ?
C12 N11 N12 106.34(14) . . ?
C12 N11 Mn1 133.08(12) . . ?
N12 N11 Mn1 120.57(11) . . ?
C14 N12 N11 110.05(14) . . ?
C14 N12 C2 132.90(15) . . ?
N11 N12 C2 117.00(14) . . ?
C22 N21 N22 106.10(14) . . ?
C22 N21 Mn1 133.20(12) . . ?
N22 N21 Mn1 119.64(11) . . ?
C24 N22 N21 110.27(14) . . ?
C24 N22 C2 132.91(15) . . ?
N21 N22 C2 116.77(13) . . ?
C1 O1 Mn1 122.51(11) . . ?
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
C1 O2 1.228(2) . ?
C1 O1 1.272(2) . ?
C1 C2 1.591(2) . ?
C2 N12 1.475(2) . ?
C2 N22 1.480(2) . ?
C2 C3 1.513(2) . ?
C3 H3A 0.96 . ?
C3 H3B 0.96 . ?
C3 H3C 0.96 . ?
C11 C12 1.498(2) . ?
C11 H11A 0.96 . ?
C11 H11B 0.96 . ?
C11 H11C 0.96 . ?
C12 N11 1.338(2) . ?
C12 C13 1.398(3) . ?
C13 C14 1.364(3) . ?
C13 H13 0.93 . ?
C14 N12 1.375(2) . ?
C14 C15 1.500(3) . ?
C15 H15A 0.96 . ?
C15 H15B 0.96 . ?
C15 H15C 0.96 . ?
C21 C22 1.494(3) . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 N21 1.340(2) . ?
C22 C23 1.396(3) . ?
C23 C24 1.372(3) . ?
C23 H23 0.93 . ?
C24 N22 1.375(2) . ?
C24 C25 1.500(3) . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C31 O31 1.147(2) . ?
C31 Mn1 1.818(2) . ?
C41 O41 1.155(2) . ?
C41 Mn1 1.7918(19) . ?
C51 O51 1.146(2) . ?
C51 Mn1 1.811(2) . ?
Mn1 O1 2.0051(13) . ?
Mn1 N11 2.0537(15) . ?
Mn1 N21 2.0658(15) . ?
N11 N12 1.380(2) . ?
N21 N22 1.3812(19) . ?
