#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/10/2221035.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2221035
loop_
_publ_author_name
'Li, Ming-Jie'
'Yan, Peng-Fei'
'Li, Guang-Ming'
'Li, Hong-Feng'
_publ_section_title
Chlorido{2,2'-[propane-1,3-diylbis(nitrilomethylidyne)]diphenolato-κ⁴O,N,N',O'}manganese(III)
_journal_coeditor_code           CV2500
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m306
_journal_paper_doi               10.1107/S1600536809005352
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Mn (C17 H16 N2 O2) Cl]'
_chemical_formula_moiety         'C17 H16 Mn N2 O2 +, Cl -'
_chemical_formula_sum            'C17 H16 Cl Mn N2 O2'
_chemical_formula_weight         370.71
_chemical_name_systematic
;
Chlorido{2,2'-[propane-1,3-diylbis(nitrilomethylidyne)]diphenolato-
κ⁴O,N,N',O'}manganese(III)
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 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                   10.428(3)
_cell_length_b                   12.067(4)
_cell_length_c                   12.530(5)
_cell_measurement_reflns_used    12324
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.05
_cell_volume                     1576.7(9)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11321
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  0.8894
_exptl_absorpt_correction_T_min  0.8303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.305
_refine_ls_abs_structure_details 'Flack (1983), 1227 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2689
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0350
_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)+(0.0666P)²+0.1785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                2526
_reflns_number_total             2689
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2500.cif
_cod_data_source_block           I
_cod_original_cell_volume        1576.6(10)
_cod_database_code               2221035
_cod_database_fobs_code          2221035
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.8363(3) 0.4885(3) 0.7136(3) 0.0330(8) Uani d . 1 . .
C C2 0.9063(3) 0.4297(3) 0.6323(3) 0.0383(8) Uani d . 1 . .
H H1 0.9918 0.4508 0.6257 0.046 Uiso calc R 1 . .
C C3 0.8679(3) 0.3466(3) 0.5617(3) 0.0434(9) Uani d . 1 . .
H H2 0.9238 0.3167 0.5115 0.052 Uiso calc R 1 . .
C C4 0.7560(5) 0.3148(3) 0.5694(5) 0.0550(12) Uani d . 1 . .
H H3 0.7204 0.2607 0.5256 0.066 Uiso calc R 1 . .
C C5 0.6881(3) 0.3678(3) 0.6502(4) 0.0506(11) Uani d . 1 . .
H H4 0.6045 0.3426 0.6589 0.061 Uiso calc R 1 . .
C C6 0.7247(3) 0.4555(3) 0.7232(3) 0.0365(9) Uani d . 1 . .
C C7 0.6476(3) 0.5107(3) 0.8041(3) 0.0365(8) Uani d . 1 . .
H H5 0.5738 0.4717 0.8224 0.044 Uiso calc R 1 . .
C C8 0.5664(3) 0.6436(3) 0.9321(3) 0.0378(8) Uani d . 1 . .
H H7 0.6039 0.6538 1.0022 0.045 Uiso calc R 1 . .
H H6 0.4934 0.5941 0.9376 0.045 Uiso calc R 1 . .
C C9 0.5303(3) 0.7500(3) 0.8835(3) 0.0393(8) Uani d . 1 . .
H H8 0.5342 0.7425 0.8065 0.047 Uiso calc R 1 . .
H H9 0.4421 0.7665 0.9024 0.047 Uiso calc R 1 . .
C C10 0.6086(3) 0.8410(3) 0.9145(3) 0.0397(9) Uani d . 1 . .
H H10 0.5632 0.9106 0.9056 0.048 Uiso calc R 1 . .
H H11 0.6352 0.8340 0.9884 0.048 Uiso calc R 1 . .
C C11 0.7546(3) 0.9233(3) 0.8068(3) 0.0341(8) Uani d . 1 . .
H H12 0.7055 0.9853 0.8231 0.041 Uiso calc R 1 . .
C C12 0.8596(3) 0.9429(3) 0.7439(3) 0.0342(8) Uani d . 1 . .
C C13 0.8794(3) 1.0423(3) 0.6866(4) 0.0468(10) Uani d . 1 . .
H H13 0.8180 1.0976 0.6947 0.056 Uiso calc R 1 . .
C C14 0.9749(4) 1.0638(3) 0.6237(4) 0.0499(10) Uani d . 1 . .
H H14 0.9815 1.1286 0.5839 0.060 Uiso calc R 1 . .
C C15 1.0592(3) 0.9870(3) 0.6221(3) 0.0455(10) Uani d . 1 . .
H H15 1.1323 0.9960 0.5805 0.055 Uiso calc R 1 . .
C C16 1.0440(3) 0.8901(3) 0.6812(3) 0.0422(9) Uani d . 1 . .
H H16 1.1107 0.8390 0.6787 0.051 Uiso calc R 1 . .
C C17 0.9428(3) 0.8637(3) 0.7408(3) 0.0320(8) Uani d . 1 . .
Cl Cl1 0.82072(8) 0.70229(8) 1.06882(7) 0.0435(2) Uani d . 1 . .
Mn Mn1 0.79832(4) 0.69247(3) 0.83324(5) 0.03055(16) Uani d . 1 . .
N N1 0.6603(2) 0.6027(2) 0.8558(2) 0.0319(7) Uani d . 1 . .
N N2 0.7160(2) 0.8353(2) 0.8449(3) 0.0303(6) Uani d . 1 . .
O O1 0.87583(19) 0.56992(19) 0.7799(2) 0.0435(6) Uani d . 1 . .
O O2 0.92804(19) 0.76783(19) 0.7896(2) 0.0457(7) Uani d . 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 C1 O1 . . 117.5(3) ?
C6 C1 C2 . . 112.9(3) ?
O1 C1 C2 . . 129.6(3) ?
C3 C2 C1 . . 131.0(3) ?
C3 C2 H1 . . 114.5 ?
C1 C2 H1 . . 114.5 ?
C4 C3 C2 . . 116.5(4) ?
C4 C3 H2 . . 121.8 ?
C2 C3 H2 . . 121.8 ?
C3 C4 C5 . . 113.3(4) ?
C3 C4 H3 . . 123.3 ?
C5 C4 H3 . . 123.3 ?
C4 C5 C6 . . 131.4(3) ?
C4 C5 H4 . . 114.3 ?
C6 C5 H4 . . 114.3 ?
C1 C6 C5 . . 114.9(4) ?
C1 C6 C7 . . 116.1(3) ?
C5 C6 C7 . . 128.9(3) ?
N1 C7 C6 . . 133.3(3) ?
N1 C7 H5 . . 113.4 ?
C6 C7 H5 . . 113.4 ?
N1 C8 C9 . . 101.3(3) ?
N1 C8 H7 . . 111.5 ?
C9 C8 H7 . . 111.5 ?
N1 C8 H6 . . 111.5 ?
C9 C8 H6 . . 111.5 ?
H7 C8 H6 . . 109.3 ?
C10 C9 C8 . . 114.5(3) ?
C10 C9 H8 . . 108.6 ?
C8 C9 H8 . . 108.6 ?
C10 C9 H9 . . 108.6 ?
C8 C9 H9 . . 108.6 ?
H8 C9 H9 . . 107.6 ?
N2 C10 C9 . . 104.3(3) ?
N2 C10 H10 . . 110.9 ?
C9 C10 H10 . . 110.9 ?
N2 C10 H11 . . 110.9 ?
C9 C10 H11 . . 110.9 ?
H10 C10 H11 . . 108.9 ?
N2 C11 C12 . . 129.3(3) ?
N2 C11 H12 . . 115.4 ?
C12 C11 H12 . . 115.4 ?
C17 C12 C11 . . 115.2(3) ?
C17 C12 C13 . . 121.0(3) ?
C11 C12 C13 . . 123.8(3) ?
C14 C13 C12 . . 126.3(4) ?
C14 C13 H13 . . 116.9 ?
C12 C13 H13 . . 116.9 ?
C15 C14 C13 . . 113.1(4) ?
C15 C14 H14 . . 123.4 ?
C13 C14 H14 . . 123.4 ?
C14 C15 C16 . . 121.5(4) ?
C14 C15 H15 . . 119.3 ?
C16 C15 H15 . . 119.3 ?
C17 C16 C15 . . 126.1(3) ?
C17 C16 H16 . . 116.9 ?
C15 C16 H16 . . 116.9 ?
C12 C17 O2 . . 123.9(3) ?
C12 C17 C16 . . 111.8(3) ?
O2 C17 C16 . . 124.3(3) ?
O2 Mn1 O1 . . 87.90(11) ?
O2 Mn1 N1 . . 169.92(14) ?
O1 Mn1 N1 . . 85.65(11) ?
O2 Mn1 N2 . . 84.35(11) ?
O1 Mn1 N2 . . 162.58(14) ?
N1 Mn1 N2 . . 99.68(11) ?
O2 Mn1 Cl1 . . 103.51(11) ?
O1 Mn1 Cl1 . . 111.39(10) ?
N1 Mn1 Cl1 . . 86.08(9) ?
N2 Mn1 Cl1 . . 85.64(10) ?
C7 N1 C8 . . 123.5(3) ?
C7 N1 Mn1 . . 120.9(2) ?
C8 N1 Mn1 . . 115.6(2) ?
C11 N2 C10 . . 117.0(3) ?
C11 N2 Mn1 . . 126.5(2) ?
C10 N2 Mn1 . . 116.1(2) ?
C1 O1 Mn1 . . 133.14(19) ?
C17 O2 Mn1 . . 134.8(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C6 . 1.236(5) ?
C1 O1 . 1.351(4) ?
C1 C2 . 1.439(5) ?
C2 C3 . 1.397(5) ?
C2 H1 . 0.9300 ?
C3 C4 . 1.232(6) ?
C3 H2 . 0.9300 ?
C4 C5 . 1.391(7) ?
C4 H3 . 0.9300 ?
C5 C6 . 1.449(6) ?
C5 H4 . 0.9300 ?
C6 C7 . 1.456(5) ?
C7 N1 . 1.291(4) ?
C7 H5 . 0.9300 ?
C8 N1 . 1.455(4) ?
C8 C9 . 1.470(5) ?
C8 H7 . 0.9700 ?
C8 H6 . 0.9700 ?
C9 C10 . 1.423(5) ?
C9 H8 . 0.9700 ?
C9 H9 . 0.9700 ?
C10 N2 . 1.421(4) ?
C10 H10 . 0.9700 ?
C10 H11 . 0.9700 ?
C11 N2 . 1.232(4) ?
C11 C12 . 1.370(5) ?
C11 H12 . 0.9300 ?
C12 C17 . 1.292(5) ?
C12 C13 . 1.413(5) ?
C13 C14 . 1.296(6) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.277(5) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.394(5) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.331(5) ?
C16 H16 . 0.9300 ?
C17 O2 . 1.317(4) ?
Cl1 Mn1 . 2.9634(16) ?
Mn1 O2 . 1.719(2) ?
Mn1 O1 . 1.813(2) ?
Mn1 N1 . 1.824(2) ?
Mn1 N2 . 1.931(2) ?
