#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:01:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179089 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/51/4305181.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_4305181
loop_
_publ_author_name
'Christopher W. Belock'
'Anil Çetin'
'Natalie V. Barone'
'Christopher J. Ziegler'
_publ_section_title
;
Transition Metal Coordination Chemistry
of N,N-Bis(2-{pyrid-2-ylethyl})hydroxylamine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7114
_journal_page_last               7120
_journal_paper_doi               10.1021/ic702406n
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C29 H34 Cl4 Mn2 N6 O3'
_chemical_formula_weight         766.30
_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-97
_cell_angle_alpha                82.708(4)
_cell_angle_beta                 77.339(4)
_cell_angle_gamma                81.586(4)
_cell_formula_units_Z            1
_cell_length_a                   7.9509(19)
_cell_length_b                   9.206(2)
_cell_length_c                   11.763(3)
_cell_measurement_reflns_used    1940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.25
_cell_volume                     827.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7005
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.9670
_exptl_absorpt_correction_T_min  0.8434
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0399
_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)+(0.0579P)²+0.2435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                2992
_reflns_number_total             3550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702406n-file002_2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4305181
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 0.3845(3) 0.6077(3) 0.6313(2) 0.0168(5) Uani 1 1 d . . .
C2 C 0.3111(3) 0.4807(3) 0.6320(2) 0.0204(5) Uani 1 1 d . . .
C3 C 0.1320(4) 0.4908(3) 0.6473(3) 0.0261(6) Uani 1 1 d . . .
C4 C 0.0338(3) 0.6262(3) 0.6603(2) 0.0225(6) Uani 1 1 d . . .
C5 C 0.1155(3) 0.7508(3) 0.6576(2) 0.0160(5) Uani 1 1 d . . .
C6 C 0.0159(3) 0.9013(3) 0.6646(2) 0.0174(5) Uani 1 1 d . . .
C7 C 0.0124(3) 0.9763(3) 0.7730(2) 0.0217(6) Uani 1 1 d . . .
C8 C 0.1779(3) 1.0991(3) 0.8715(2) 0.0217(6) Uani 1 1 d . . .
C9 C 0.3435(4) 1.0985(3) 0.9183(2) 0.0222(6) Uani 1 1 d . . .
C10 C 0.4844(3) 1.1684(3) 0.8319(2) 0.0178(5) Uani 1 1 d . . .
C11 C 0.5558(3) 1.2855(3) 0.8600(2) 0.0223(6) Uani 1 1 d . . .
C12 C 0.6819(4) 1.3517(3) 0.7780(2) 0.0236(6) Uani 1 1 d . . .
C13 C 0.7347(3) 1.2995(3) 0.6696(2) 0.0201(5) Uani 1 1 d . . .
C14 C 0.6605(3) 1.1822(3) 0.6475(2) 0.0162(5) Uani 1 1 d . . .
C15 C 0.0206(10) 0.6060(7) 0.0452(6) 0.0370(16) Uani 0.50 1 d P . .
Cl1 Cl 0.57801(7) 0.75836(7) 0.80721(5) 0.01821(15) Uani 1 1 d . . .
Cl2 Cl 0.32273(7) 1.12961(6) 0.51162(5) 0.01488(15) Uani 1 1 d . . .
H1 H 0.511(4) 0.601(3) 0.620(2) 0.020(7) Uiso 1 1 d . . .
H2 H 0.379(4) 0.388(3) 0.620(2) 0.021(7) Uiso 1 1 d . . .
H3 H 0.078(4) 0.399(3) 0.640(3) 0.036(9) Uiso 1 1 d . . .
H4 H -0.088(4) 0.642(3) 0.667(2) 0.025(8) Uiso 1 1 d . . .
H5 H -0.104(4) 0.896(3) 0.661(2) 0.027(8) Uiso 1 1 d . . .
H6 H 0.061(3) 0.968(3) 0.598(2) 0.010(6) Uiso 1 1 d . . .
H7 H -0.059(4) 0.940(3) 0.841(3) 0.027(8) Uiso 1 1 d . . .
H8 H -0.029(4) 1.076(3) 0.756(2) 0.022(7) Uiso 1 1 d . . .
H9 H 0.074(3) 1.101(3) 0.934(2) 0.006(6) Uiso 1 1 d . . .
H10 H 0.159(4) 1.188(3) 0.801(3) 0.024(7) Uiso 1 1 d . . .
H11 H 0.393(3) 1.003(3) 0.937(2) 0.012(6) Uiso 1 1 d . . .
H12 H 0.312(4) 1.152(3) 0.989(3) 0.028(8) Uiso 1 1 d . . .
H13 H 0.516(3) 1.319(3) 0.932(2) 0.017(7) Uiso 1 1 d . . .
H14 H 0.727(4) 1.434(4) 0.790(3) 0.037(9) Uiso 1 1 d . . .
H15 H 0.813(4) 1.346(3) 0.611(3) 0.031(8) Uiso 1 1 d . . .
H16 H 0.694(3) 1.146(3) 0.573(2) 0.013(6) Uiso 1 1 d . . .
H17 H 0.300(4) 0.792(3) 0.876(3) 0.034(9) Uiso 1 1 d . . .
Mn1 Mn 0.43620(4) 0.92929(4) 0.66318(3) 0.01337(13) Uani 1 1 d . . .
N1 N 0.2908(2) 0.7410(2) 0.64332(17) 0.0146(4) Uani 1 1 d . . .
N2 N 0.5371(3) 1.1169(2) 0.72576(17) 0.0153(4) Uani 1 1 d . . .
N3 N 0.1826(3) 0.9713(2) 0.80599(17) 0.0171(4) Uani 1 1 d . . .
O3 O 0.1857(2) 0.8411(2) 0.89217(15) 0.0217(4) Uani 1 1 d . . .
O4 O 0.0000 0.5000 0.0000 0.215(5) Uani 1 2 d S . .
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'
Cl Cl 0.1484 0.1585 '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
N1 C1 C2 123.1(2) . . ?
N1 C1 H1 118.5(16) . . ?
C2 C1 H1 118.3(16) . . ?
C1 C2 C3 118.3(2) . . ?
C1 C2 H2 122.4(17) . . ?
C3 C2 H2 119.3(17) . . ?
C4 C3 C2 119.3(2) . . ?
C4 C3 H3 121.9(18) . . ?
C2 C3 H3 118.5(18) . . ?
C3 C4 C5 119.7(2) . . ?
C3 C4 H4 123.9(17) . . ?
C5 C4 H4 116.2(17) . . ?
N1 C5 C4 121.0(2) . . ?
N1 C5 C6 117.2(2) . . ?
C4 C5 C6 121.8(2) . . ?
C5 C6 C7 116.3(2) . . ?
C5 C6 H5 109.2(17) . . ?
C7 C6 H5 107.4(17) . . ?
C5 C6 H6 110.8(15) . . ?
C7 C6 H6 106.4(15) . . ?
H5 C6 H6 106(2) . . ?
N3 C7 C6 115.4(2) . . ?
N3 C7 H7 104.0(19) . . ?
C6 C7 H7 115.2(19) . . ?
N3 C7 H8 107.4(18) . . ?
C6 C7 H8 106.2(18) . . ?
H7 C7 H8 108(2) . . ?
N3 C8 C9 113.3(2) . . ?
N3 C8 H9 108.2(14) . . ?
C9 C8 H9 111.9(15) . . ?
N3 C8 H10 98.1(15) . . ?
C9 C8 H10 114.5(15) . . ?
H9 C8 H10 110(2) . . ?
C10 C9 C8 113.6(2) . . ?
C10 C9 H11 105.0(16) . . ?
C8 C9 H11 111.3(16) . . ?
C10 C9 H12 109.2(17) . . ?
C8 C9 H12 108.0(17) . . ?
H11 C9 H12 110(2) . . ?
N2 C10 C11 121.2(2) . . ?
N2 C10 C9 118.2(2) . . ?
C11 C10 C9 120.6(2) . . ?
C12 C11 C10 120.0(2) . . ?
C12 C11 H13 121.0(17) . . ?
C10 C11 H13 119.0(17) . . ?
C13 C12 C11 118.7(2) . . ?
C13 C12 H14 118(2) . . ?
C11 C12 H14 123(2) . . ?
C12 C13 C14 118.6(2) . . ?
C12 C13 H15 121(2) . . ?
C14 C13 H15 121(2) . . ?
N2 C14 C13 123.5(2) . . ?
N2 C14 H16 116.8(16) . . ?
C13 C14 H16 119.6(16) . . ?
Mn1 Cl2 Mn1 97.16(3) 2_676 . ?
N2 Mn1 N1 166.19(7) . . ?
N2 Mn1 N3 87.88(7) . . ?
N1 Mn1 N3 79.10(7) . . ?
N2 Mn1 Cl1 87.59(5) . . ?
N1 Mn1 Cl1 88.03(5) . . ?
N3 Mn1 Cl1 90.93(5) . . ?
N2 Mn1 Cl2 100.44(5) . 2_676 ?
N1 Mn1 Cl2 92.96(5) . 2_676 ?
N3 Mn1 Cl2 170.21(5) . 2_676 ?
Cl1 Mn1 Cl2 94.54(3) . 2_676 ?
N2 Mn1 Cl2 85.54(5) . . ?
N1 Mn1 Cl2 99.55(5) . . ?
N3 Mn1 Cl2 92.77(5) . . ?
Cl1 Mn1 Cl2 172.07(2) . . ?
Cl2 Mn1 Cl2 82.84(3) 2_676 . ?
C1 N1 C5 118.5(2) . . ?
C1 N1 Mn1 116.76(15) . . ?
C5 N1 Mn1 124.23(16) . . ?
C14 N2 C10 118.0(2) . . ?
C14 N2 Mn1 115.56(16) . . ?
C10 N2 Mn1 126.47(16) . . ?
O3 N3 C8 105.74(18) . . ?
O3 N3 C7 102.80(19) . . ?
C8 N3 C7 108.8(2) . . ?
O3 N3 Mn1 105.14(13) . . ?
C8 N3 Mn1 114.04(15) . . ?
C7 N3 Mn1 118.75(15) . . ?
N3 O3 H17 105.9(19) . . ?
C15 O4 C15 180.0(5) . 2_565 ?
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 N1 1.345(3) . ?
C1 C2 1.380(3) . ?
C1 H1 0.98(3) . ?
C2 C3 1.387(4) . ?
C2 H2 0.94(3) . ?
C3 C4 1.378(4) . ?
C3 H3 1.02(3) . ?
C4 C5 1.392(3) . ?
C4 H4 0.95(3) . ?
C5 N1 1.358(3) . ?
C5 C6 1.494(3) . ?
C6 C7 1.519(4) . ?
C6 H5 0.97(3) . ?
C6 H6 0.97(3) . ?
C7 N3 1.480(3) . ?
C7 H7 0.93(3) . ?
C7 H8 0.94(3) . ?
C8 N3 1.478(3) . ?
C8 C9 1.534(4) . ?
C8 H9 0.98(2) . ?
C8 H10 1.11(3) . ?
C9 C10 1.499(4) . ?
C9 H11 0.93(3) . ?
C9 H12 0.99(3) . ?
C10 N2 1.350(3) . ?
C10 C11 1.395(3) . ?
C11 C12 1.383(4) . ?
C11 H13 0.92(3) . ?
C12 C13 1.377(4) . ?
C12 H14 0.93(3) . ?
C13 C14 1.380(3) . ?
C13 H15 0.93(3) . ?
C14 N2 1.345(3) . ?
C14 H16 0.94(3) . ?
C15 O4 1.216(5) . ?
Cl1 Mn1 2.5018(7) . ?
Cl2 Mn1 2.5390(8) 2_676 ?
Cl2 Mn1 2.6032(7) . ?
Mn1 N2 2.271(2) . ?
Mn1 N1 2.281(2) . ?
Mn1 N3 2.343(2) . ?
Mn1 Cl2 2.5390(8) 2_676 ?
N3 O3 1.469(3) . ?
O3 H17 0.94(3) . ?
O4 C15 1.216(5) 2_565 ?
