#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:57:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179137 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/99/4309923.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_4309923
loop_
_publ_author_name
'Kaushik Ghosh'
'Aura A. Eroy-Reveles'
'Marilyn M. Olmstead'
'Pradip K. Mascharak'
_publ_section_title
;
Reductive Nitrosylation and Proton-Assisted Bridge Splitting of a
(μ-Oxo)dimanganese(III) Complex Derived from a Polypyridine Ligand with
One Carboxamide Group
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8469
_journal_page_last               8475
_journal_paper_doi               10.1021/ic0503535
_journal_volume                  44
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H23 Mn N5 O2, Cl O4'
_chemical_formula_sum            'C21 H23 Cl Mn N5 O6'
_chemical_formula_weight         531.83
_chemical_name_common            '[Mn(PaPy3)(OCH3)](ClO4)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4315(6)
_cell_length_b                   11.0777(8)
_cell_length_c                   24.0524(18)
_cell_measurement_reflns_used    956
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.6
_cell_volume                     2246.5(3)
_computing_cell_refinement       'SMART 5.054 (Bruker, 2002)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36A (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16861
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.05 (Sheldrick, 2002)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0314
_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)+(0.0386P)²+0.1222P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                4424
_reflns_number_total             5095
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic0503535si20050307_025802.cif
_cod_data_source_block           mn1482
_cod_database_code               4309923
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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 0.29348(4) 0.52435(3) 0.881555(14) 0.01249(8) Uani 1 1 d . . .
O1 O 0.0924(2) 0.78928(15) 0.78713(8) 0.0215(4) Uani 1 1 d . . .
O2 O 0.3908(2) 0.45207(15) 0.94063(7) 0.0197(4) Uani 1 1 d . . .
N1 N 0.2163(2) 0.68617(16) 0.91998(8) 0.0154(4) Uani 1 1 d . . .
N2 N 0.2155(2) 0.61593(17) 0.81800(8) 0.0153(4) Uani 1 1 d . . .
N3 N 0.3048(2) 0.38015(17) 0.81609(8) 0.0168(4) Uani 1 1 d . . .
N4 N 0.5221(2) 0.55108(17) 0.84615(8) 0.0142(4) Uani 1 1 d . . .
N5 N 0.0731(2) 0.42358(17) 0.89276(8) 0.0159(4) Uani 1 1 d . . .
C1 C 0.2206(3) 0.7147(2) 0.97422(10) 0.0198(5) Uani 1 1 d . . .
H1 H 0.2662 0.6596 0.9999 0.024 Uiso 1 1 calc R . .
C2 C 0.1596(3) 0.8235(2) 0.99342(12) 0.0282(6) Uani 1 1 d . . .
H2 H 0.1652 0.8429 1.0318 0.034 Uiso 1 1 calc R . .
C3 C 0.0913(3) 0.9027(2) 0.95663(13) 0.0308(7) Uani 1 1 d . . .
H3 H 0.0480 0.9768 0.9694 0.037 Uiso 1 1 calc R . .
C4 C 0.0859(3) 0.8734(2) 0.90064(12) 0.0252(6) Uani 1 1 d . . .
H4 H 0.0397 0.9272 0.8745 0.030 Uiso 1 1 calc R . .
C5 C 0.1492(3) 0.7644(2) 0.88362(11) 0.0171(5) Uani 1 1 d . . .
C6 C 0.1499(3) 0.7246(2) 0.82403(10) 0.0162(5) Uani 1 1 d . . .
C7 C 0.2424(3) 0.5657(2) 0.76257(10) 0.0187(5) Uani 1 1 d . . .
H7A H 0.3508 0.5857 0.7496 0.022 Uiso 1 1 calc R . .
H7B H 0.1653 0.6000 0.7358 0.022 Uiso 1 1 calc R . .
C8 C 0.2220(3) 0.4299(2) 0.76631(10) 0.0195(5) Uani 1 1 d . . .
H8A H 0.1077 0.4101 0.7685 0.023 Uiso 1 1 calc R . .
H8B H 0.2654 0.3918 0.7323 0.023 Uiso 1 1 calc R . .
C9 C 0.4736(3) 0.3533(2) 0.80556(11) 0.0197(5) Uani 1 1 d . . .
H9A H 0.4857 0.3206 0.7675 0.024 Uiso 1 1 calc R . .
H9B H 0.5104 0.2910 0.8321 0.024 Uiso 1 1 calc R . .
C10 C 0.5750(3) 0.4654(2) 0.81168(9) 0.0160(5) Uani 1 1 d . . .
C11 C 0.7199(3) 0.4781(2) 0.78384(9) 0.0194(5) Uani 1 1 d . . .
H11 H 0.7565 0.4173 0.7591 0.023 Uiso 1 1 calc R . .
C12 C 0.8081(3) 0.5806(2) 0.79319(10) 0.0211(5) Uani 1 1 d . . .
H12 H 0.9075 0.5906 0.7752 0.025 Uiso 1 1 calc R . .
C13 C 0.7523(3) 0.6689(2) 0.82864(10) 0.0189(5) Uani 1 1 d . . .
H13 H 0.8126 0.7397 0.8355 0.023 Uiso 1 1 calc R . .
C14 C 0.6066(3) 0.6520(2) 0.85398(10) 0.0167(5) Uani 1 1 d . . .
H14 H 0.5657 0.7134 0.8775 0.020 Uiso 1 1 calc R . .
C15 C 0.2173(3) 0.2747(2) 0.83818(11) 0.0202(5) Uani 1 1 d . . .
H15A H 0.2861 0.2295 0.8643 0.024 Uiso 1 1 calc R . .
H15B H 0.1888 0.2199 0.8072 0.024 Uiso 1 1 calc R . .
C16 C 0.0684(3) 0.3149(2) 0.86795(10) 0.0180(5) Uani 1 1 d . . .
C17 C -0.0647(3) 0.2414(2) 0.87186(10) 0.0211(5) Uani 1 1 d . . .
H17 H -0.0658 0.1646 0.8543 0.025 Uiso 1 1 calc R . .
C18 C -0.1951(3) 0.2807(2) 0.90136(11) 0.0235(6) Uani 1 1 d . . .
H18 H -0.2870 0.2314 0.9043 0.028 Uiso 1 1 calc R . .
C19 C -0.1902(3) 0.3929(2) 0.92661(11) 0.0236(6) Uani 1 1 d . . .
H19 H -0.2786 0.4224 0.9470 0.028 Uiso 1 1 calc R . .
C20 C -0.0531(3) 0.4611(2) 0.92143(10) 0.0210(5) Uani 1 1 d . . .
H20 H -0.0489 0.5378 0.9390 0.025 Uiso 1 1 calc R . .
C21 C 0.3305(3) 0.3690(2) 0.97927(12) 0.0283(6) Uani 1 1 d . . .
H21A H 0.4141 0.3466 1.0056 0.043 Uiso 1 1 calc R . .
H21B H 0.2932 0.2968 0.9597 0.043 Uiso 1 1 calc R . .
H21C H 0.2419 0.4058 0.9995 0.043 Uiso 1 1 calc R . .
Cl1 Cl 0.54348(6) -0.01717(5) 0.88579(3) 0.01942(12) Uani 1 1 d . . .
O3 O 0.7126(2) -0.01220(17) 0.87643(8) 0.0344(4) Uani 1 1 d . . .
O4 O 0.4667(3) -0.0554(2) 0.83544(8) 0.0409(6) Uani 1 1 d . . .
O5 O 0.4881(2) 0.10028(17) 0.90209(10) 0.0362(5) Uani 1 1 d . . .
O6 O 0.5096(3) -0.10238(17) 0.92930(8) 0.0318(5) 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 0.0000 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'
Cl Cl 0.1484 0.1585 '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
O2 Mn1 N2 172.03(8) . . ?
O2 Mn1 N1 99.77(8) . . ?
N2 Mn1 N1 78.35(8) . . ?
O2 Mn1 N4 88.02(7) . . ?
N2 Mn1 N4 85.36(8) . . ?
N1 Mn1 N4 109.58(8) . . ?
O2 Mn1 N5 93.56(7) . . ?
N2 Mn1 N5 94.35(8) . . ?
N1 Mn1 N5 96.73(8) . . ?
N4 Mn1 N5 153.00(7) . . ?
O2 Mn1 N3 102.39(8) . . ?
N2 Mn1 N3 80.49(7) . . ?
N1 Mn1 N3 157.04(8) . . ?
N4 Mn1 N3 77.28(7) . . ?
N5 Mn1 N3 76.06(7) . . ?
C21 O2 Mn1 129.81(16) . . ?
C1 N1 C5 119.2(2) . . ?
C1 N1 Mn1 127.90(17) . . ?
C5 N1 Mn1 112.83(16) . . ?
C6 N2 C7 120.47(19) . . ?
C6 N2 Mn1 121.66(16) . . ?
C7 N2 Mn1 117.71(15) . . ?
C9 N3 C15 112.53(19) . . ?
C9 N3 C8 112.8(2) . . ?
C15 N3 C8 110.27(19) . . ?
C9 N3 Mn1 107.74(14) . . ?
C15 N3 Mn1 106.79(14) . . ?
C8 N3 Mn1 106.28(13) . . ?
C10 N4 C14 120.1(2) . . ?
C10 N4 Mn1 116.87(15) . . ?
C14 N4 Mn1 122.83(16) . . ?
C20 N5 C16 119.0(2) . . ?
C20 N5 Mn1 125.64(16) . . ?
C16 N5 Mn1 115.34(16) . . ?
N1 C1 C2 121.1(2) . . ?
N1 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 119.4(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 118.7(3) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N1 C5 C4 121.9(2) . . ?
N1 C5 C6 115.3(2) . . ?
C4 C5 C6 122.8(2) . . ?
O1 C6 N2 127.4(2) . . ?
O1 C6 C5 120.8(2) . . ?
N2 C6 C5 111.8(2) . . ?
N2 C7 C8 107.79(19) . . ?
N2 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
N2 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.5 . . ?
N3 C8 C7 111.15(19) . . ?
N3 C8 H8A 109.4 . . ?
C7 C8 H8A 109.4 . . ?
N3 C8 H8B 109.4 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
N3 C9 C10 111.28(19) . . ?
N3 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
N3 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N4 C10 C11 121.1(2) . . ?
N4 C10 C9 117.0(2) . . ?
C11 C10 C9 121.9(2) . . ?
C12 C11 C10 118.4(2) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
C13 C12 C11 120.1(2) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 118.6(2) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
N4 C14 C13 121.6(2) . . ?
N4 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
N3 C15 C16 110.54(19) . . ?
N3 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
N5 C16 C17 121.2(2) . . ?
N5 C16 C15 116.7(2) . . ?
C17 C16 C15 122.0(2) . . ?
C18 C17 C16 119.6(2) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 119.0(2) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C18 C19 C20 118.3(2) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
N5 C20 C19 122.8(2) . . ?
N5 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
O2 C21 H21A 109.5 . . ?
O2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 Cl1 O5 110.53(14) . . ?
O4 Cl1 O6 109.28(12) . . ?
O5 Cl1 O6 109.34(13) . . ?
O4 Cl1 O3 108.92(13) . . ?
O5 Cl1 O3 109.21(12) . . ?
O6 Cl1 O3 109.55(12) . . ?
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 O2 1.8256(16) . ?
Mn1 N2 1.9488(19) . ?
Mn1 N1 2.1192(19) . ?
Mn1 N4 2.128(2) . ?
Mn1 N5 2.1844(19) . ?
Mn1 N3 2.245(2) . ?
O1 C6 1.240(3) . ?
O2 C21 1.403(3) . ?
N1 C1 1.343(3) . ?
N1 C5 1.355(3) . ?
N2 C6 1.332(3) . ?
N2 C7 1.462(3) . ?
N3 C9 1.476(3) . ?
N3 C15 1.480(3) . ?
N3 C8 1.492(3) . ?
N4 C10 1.337(3) . ?
N4 C14 1.339(3) . ?
N5 C20 1.335(3) . ?
N5 C16 1.344(3) . ?
C1 C2 1.389(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.373(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.500(4) . ?
C7 C8 1.518(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.515(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.400(3) . ?
C11 C12 1.376(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.380(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.513(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.389(4) . ?
C17 C18 1.379(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.387(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
Cl1 O4 1.437(2) . ?
Cl1 O5 1.437(2) . ?
Cl1 O6 1.4381(19) . ?
Cl1 O3 1.4447(19) . ?
