#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/75/2207537.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_2207537
loop_
_publ_author_name
'Butcher, Ray J.'
'Towns, William'
_publ_section_title
;Aqua[N,N'-ethylenebis(5-nitrosalicylideneiminato)]methanolmanganese(III)
 perchlorate
;
_journal_coeditor_code           HB2001
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2618
_journal_page_last               m2620
_journal_paper_doi               10.1107/S1600536805036913
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Mn (C16 H12 N4 O6) (C H4 O) (H2 O)] Cl O4'
_chemical_formula_moiety         'C17 H18 Mn N4 O8 +, Cl O4 -'
_chemical_formula_sum            'C17 H18 Cl Mn N4 O12'
_chemical_formula_weight         560.74
_chemical_name_systematic
;
Aqua[N,N'-ethylenebis(5-nitrosalicylideneiminato)]methanolmanganese(III)
perchlorate
;
_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                84.549(13)
_cell_angle_beta                 79.701(15)
_cell_angle_gamma                72.128(12)
_cell_formula_units_Z            2
_cell_length_a                   8.3102(15)
_cell_length_b                   10.3320(16)
_cell_length_c                   13.995(2)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.42
_cell_measurement_theta_min      2.48
_cell_volume                     1124.2(3)
_computing_cell_refinement       'XSCANS '
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4S'
_diffrn_measurement_method       2θ/ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0145
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5181
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0.01
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al.,  1968)'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5169
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0653P)²+0.3336P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                3452
_reflns_number_total             5169
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2001.cif
_cod_data_source_block           I
_cod_database_code               2207537
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_type_symbol
Mn 0.12669(7) 0.24444(5) 0.26710(4) 0.03583(16) Uani d . 1 Mn
Cl -0.29676(13) 0.25177(11) 0.04343(7) 0.0549(3) Uani d . 1 Cl
O11A -0.2816(7) 0.1147(4) 0.0725(3) 0.1263(17) Uani d . 1 O
O12A -0.3641(5) 0.3297(5) 0.1266(3) 0.1171(16) Uani d . 1 O
O13A -0.4084(5) 0.2944(5) -0.0245(3) 0.1071(15) Uani d . 1 O
O14A -0.1339(4) 0.2635(5) 0.0023(3) 0.1000(13) Uani d . 1 O
O1A 0.1237(3) 0.3581(2) 0.36624(17) 0.0437(6) Uani d . 1 O
O1B 0.0515(3) 0.1093(2) 0.35038(17) 0.0426(6) Uani d . 1 O
O1M 0.3991(4) 0.1309(3) 0.2782(2) 0.0608(8) Uani d D 1 O
H1M 0.4080 0.0496 0.2785 0.091 Uiso calc RD 1 H
O1W -0.1522(3) 0.3528(3) 0.2586(2) 0.0576(7) Uani d D 1 O
H1W1 -0.169(5) 0.4327(14) 0.269(4) 0.086 Uiso d D 1 H
H1W2 -0.237(3) 0.343(4) 0.242(4) 0.086 Uiso d D 1 H
O51A 0.3951(5) 0.8342(3) 0.4380(3) 0.0805(10) Uani d . 1 O
O52A 0.4334(4) 0.8450(3) 0.2809(2) 0.0629(8) Uani d . 1 O
O51B -0.1670(5) -0.3357(3) 0.1785(2) 0.0741(10) Uani d . 1 O
O52B -0.2365(4) -0.3765(3) 0.3314(2) 0.0591(8) Uani d . 1 O
N1A 0.1967(4) 0.3741(3) 0.1655(2) 0.0378(6) Uani d . 1 N
N1B 0.1518(4) 0.1390(3) 0.1513(2) 0.0399(7) Uani d . 1 N
N5A 0.3891(4) 0.7926(3) 0.3607(3) 0.0548(9) Uani d . 1 N
N5B -0.1797(4) -0.3093(3) 0.2628(3) 0.0472(8) Uani d . 1 N
C1A 0.2560(4) 0.5162(3) 0.2725(3) 0.0377(8) Uani d . 1 C
C2A 0.1936(4) 0.4578(3) 0.3617(3) 0.0392(8) Uani d . 1 C
C3A 0.2029(5) 0.5099(4) 0.4484(3) 0.0513(10) Uani d . 1 C
H3AA 0.1646 0.4709 0.5073 0.062 Uiso calc R 1 H
C4A 0.2673(5) 0.6175(4) 0.4490(3) 0.0523(10) Uani d . 1 C
H4AA 0.2711 0.6515 0.5074 0.063 Uiso calc R 1 H
C5A 0.3268(5) 0.6750(4) 0.3607(3) 0.0464(9) Uani d . 1 C
C6A 0.3240(5) 0.6254(3) 0.2740(3) 0.0416(8) Uani d . 1 C
H6AA 0.3670 0.6636 0.2159 0.050 Uiso calc R 1 H
C7A 0.2505(4) 0.4735(3) 0.1793(3) 0.0394(8) Uani d . 1 C
H7AA 0.2887 0.5212 0.1247 0.047 Uiso calc R 1 H
C8A 0.1869(5) 0.3430(4) 0.0659(3) 0.0479(9) Uani d . 1 C
H8AA 0.2619 0.3813 0.0184 0.058 Uiso calc R 1 H
H8AB 0.0708 0.3810 0.0524 0.058 Uiso calc R 1 H
C1B 0.0112(4) -0.0237(3) 0.2302(2) 0.0368(7) Uani d . 1 C
C2B -0.0058(4) 0.0134(3) 0.3268(2) 0.0369(7) Uani d . 1 C
C3B -0.0846(5) -0.0596(4) 0.4023(3) 0.0442(8) Uani d . 1 C
H3BA -0.0972 -0.0367 0.4665 0.053 Uiso calc R 1 H
C4B -0.1423(5) -0.1631(4) 0.3823(3) 0.0440(8) Uani d . 1 C
H4BA -0.1925 -0.2108 0.4324 0.053 Uiso calc R 1 H
C5B -0.1250(4) -0.1963(3) 0.2860(3) 0.0401(8) Uani d . 1 C
C6B -0.0506(5) -0.1294(3) 0.2116(3) 0.0415(8) Uani d . 1 C
H6BA -0.0405 -0.1537 0.1479 0.050 Uiso calc R 1 H
C7B 0.0950(5) 0.0379(4) 0.1482(3) 0.0414(8) Uani d . 1 C
H7BA 0.1091 0.0014 0.0880 0.050 Uiso calc R 1 H
C8B 0.2421(5) 0.1904(4) 0.0615(3) 0.0487(9) Uani d . 1 C
H8BA 0.2111 0.1637 0.0044 0.058 Uiso calc R 1 H
H8BB 0.3652 0.1540 0.0588 0.058 Uiso calc R 1 H
C1M 0.5077(8) 0.1502(6) 0.3363(5) 0.102(2) Uani d . 1 C
H1MA 0.6238 0.1201 0.3036 0.152 Uiso calc R 1 H
H1MB 0.4966 0.0988 0.3967 0.152 Uiso calc R 1 H
H1MC 0.4779 0.2451 0.3489 0.152 Uiso calc R 1 H
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_publ_flag
O1A Mn O1B 96.90(10) n
O1A Mn N1B 171.73(11) n
O1B Mn N1B 90.91(11) n
O1A Mn N1A 90.69(11) n
O1B Mn N1A 172.11(11) n
N1B Mn N1A 81.61(11) n
O1A Mn O1M 89.58(11) n
O1B Mn O1M 90.50(11) n
N1B Mn O1M 87.64(12) n
N1A Mn O1M 91.72(12) n
O1A Mn O1W 91.05(11) n
O1B Mn O1W 87.43(11) n
N1B Mn O1W 92.00(12) n
N1A Mn O1W 90.28(12) n
O1M Mn O1W 177.89(11) n
O13A Cl O12A 109.6(3) ?
O13A Cl O14A 110.1(2) ?
O12A Cl O14A 110.9(3) ?
O13A Cl O11A 109.3(3) ?
O12A Cl O11A 107.7(3) ?
O14A Cl O11A 109.1(3) ?
C2A O1A Mn 129.3(2) ?
C2B O1B Mn 128.4(2) ?
C1M O1M Mn 130.6(3) ?
C1M O1M H1M 109.5 ?
Mn O1M H1M 106.9 ?
Mn O1W H1W1 107(3) ?
Mn O1W H1W2 142(3) ?
H1W1 O1W H1W2 110.2(9) ?
C7A N1A C8A 120.4(3) ?
C7A N1A Mn 126.6(2) ?
C8A N1A Mn 113.0(2) ?
C7B N1B C8B 120.0(3) ?
C7B N1B Mn 126.3(2) ?
C8B N1B Mn 113.7(2) ?
O51A N5A O52A 123.4(3) ?
O51A N5A C5A 119.0(4) ?
O52A N5A C5A 117.6(3) ?
O51B N5B O52B 122.3(3) ?
O51B N5B C5B 119.9(3) ?
O52B N5B C5B 117.8(3) ?
C6A C1A C2A 119.2(3) ?
C6A C1A C7A 117.0(3) ?
C2A C1A C7A 123.8(3) ?
O1A C2A C3A 118.7(3) ?
O1A C2A C1A 122.7(3) ?
C3A C2A C1A 118.6(3) ?
C4A C3A C2A 121.7(4) ?
C4A C3A H3AA 119.1 ?
C2A C3A H3AA 119.1 ?
C3A C4A C5A 119.1(4) ?
C3A C4A H4AA 120.4 ?
C5A C4A H4AA 120.4 ?
C6A C5A C4A 121.3(3) ?
C6A C5A N5A 119.3(4) ?
C4A C5A N5A 119.4(3) ?
C5A C6A C1A 120.0(3) ?
C5A C6A H6AA 120.0 ?
C1A C6A H6AA 120.0 ?
N1A C7A C1A 124.6(3) ?
N1A C7A H7AA 117.7 ?
C1A C7A H7AA 117.7 ?
N1A C8A C8B 106.9(3) ?
N1A C8A H8AA 110.3 ?
C8B C8A H8AA 110.3 ?
N1A C8A H8AB 110.3 ?
C8B C8A H8AB 110.3 ?
H8AA C8A H8AB 108.6 ?
C6B C1B C2B 119.7(3) ?
C6B C1B C7B 116.9(3) ?
C2B C1B C7B 123.4(3) ?
O1B C2B C1B 123.3(3) ?
O1B C2B C3B 118.6(3) ?
C1B C2B C3B 118.1(3) ?
C4B C3B C2B 121.1(3) ?
C4B C3B H3BA 119.4 ?
C2B C3B H3BA 119.4 ?
C3B C4B C5B 119.3(3) ?
C3B C4B H4BA 120.3 ?
C5B C4B H4BA 120.3 ?
C6B C5B C4B 121.6(3) ?
C6B C5B N5B 117.8(3) ?
C4B C5B N5B 120.5(3) ?
C5B C6B C1B 120.2(3) ?
C5B C6B H6BA 119.9 ?
C1B C6B H6BA 119.9 ?
N1B C7B C1B 125.2(3) ?
N1B C7B H7BA 117.4 ?
C1B C7B H7BA 117.4 ?
N1B C8B C8A 106.3(3) ?
N1B C8B H8BA 110.5 ?
C8A C8B H8BA 110.5 ?
N1B C8B H8BB 110.5 ?
C8A C8B H8BB 110.5 ?
H8BA C8B H8BB 108.7 ?
O1M C1M H1MA 109.5 ?
O1M C1M H1MB 109.5 ?
H1MA C1M H1MB 109.5 ?
O1M C1M H1MC 109.5 ?
H1MA C1M H1MC 109.5 ?
H1MB C1M H1MC 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Mn O1A 1.893(2) y
Mn O1B 1.914(2) y
Mn N1B 1.982(3) y
Mn N1A 1.994(3) y
Mn O1M 2.233(3) y
Mn O1W 2.263(3) y
Cl O13A 1.395(3) ?
Cl O12A 1.409(4) ?
Cl O14A 1.409(3) ?
Cl O11A 1.410(4) ?
O1A C2A 1.320(4) ?
O1B C2B 1.313(4) ?
O1M C1M 1.385(6) ?
O1M H1M 0.8200 ?
O1W H1W1 0.818(5) ?
O1W H1W2 0.820(5) ?
O51A N5A 1.216(4) ?
O52A N5A 1.239(4) ?
O51B N5B 1.215(4) ?
O52B N5B 1.240(4) ?
N1A C7A 1.281(4) ?
N1A C8A 1.482(4) ?
N1B C7B 1.279(4) ?
N1B C8B 1.485(4) ?
N5A C5A 1.459(4) ?
N5B C5B 1.458(4) ?
C1A C6A 1.411(5) ?
C1A C2A 1.418(5) ?
C1A C7A 1.430(5) ?
C2A C3A 1.397(5) ?
C3A C4A 1.375(5) ?
C3A H3AA 0.9300 ?
C4A C5A 1.395(6) ?
C4A H4AA 0.9300 ?
C5A C6A 1.369(5) ?
C6A H6AA 0.9300 ?
C7A H7AA 0.9300 ?
C8A C8B 1.505(5) ?
C8A H8AA 0.9700 ?
C8A H8AB 0.9700 ?
C1B C6B 1.405(4) ?
C1B C2B 1.411(5) ?
C1B C7B 1.433(5) ?
C2B C3B 1.421(5) ?
C3B C4B 1.368(5) ?
C3B H3BA 0.9300 ?
C4B C5B 1.394(5) ?
C4B H4BA 0.9300 ?
C5B C6B 1.357(5) ?
C6B H6BA 0.9300 ?
C7B H7BA 0.9300 ?
C8B H8BA 0.9700 ?
C8B H8BB 0.9700 ?
C1M H1MA 0.9600 ?
C1M H1MB 0.9600 ?
C1M H1MC 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1M H1M O52A 1_545 0.82 2.06 2.877(4) 179
O1W H1W1 O52B 1_565 0.818(5) 2.105(14) 2.905(4) 166(5)
O1W H1W2 O12A . 0.820(5) 2.12(3) 2.842(5) 148(5)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
O1B Mn O1A C2A 165.2(3) ?
N1A Mn O1A C2A -17.0(3) ?
O1M Mn O1A C2A 74.7(3) ?
O1W Mn O1A C2A -107.3(3) ?
O1A Mn O1B C2B 165.4(3) ?
N1B Mn O1B C2B -17.3(3) ?
O1M Mn O1B C2B -105.0(3) ?
O1W Mn O1B C2B 74.6(3) ?
O1A Mn O1M C1M -1.4(5) ?
O1B Mn O1M C1M -98.3(5) ?
N1B Mn O1M C1M 170.8(5) ?
N1A Mn O1M C1M 89.2(5) ?
O1W Mn O1M C1M -109(3) ?
O1A Mn N1A C7A 12.8(3) ?
O1B Mn N1A C7A 177.0(7) ?
N1B Mn N1A C7A -164.1(3) ?
O1M Mn N1A C7A -76.8(3) ?
O1W Mn N1A C7A 103.9(3) ?
O1A Mn N1A C8A -169.1(2) ?
N1B Mn N1A C8A 13.9(2) ?
O1M Mn N1A C8A 101.3(2) ?
O1W Mn N1A C8A -78.1(2) ?
O1A Mn N1B C7B 173.5(7) ?
O1B Mn N1B C7B 12.6(3) ?
N1A Mn N1B C7B -164.9(3) ?
O1M Mn N1B C7B 103.0(3) ?
O1W Mn N1B C7B -74.9(3) ?
O1B Mn N1B C8B -169.3(3) ?
N1A Mn N1B C8B 13.2(3) ?
O1M Mn N1B C8B -78.9(3) ?
O1W Mn N1B C8B 103.2(3) ?
Mn O1A C2A C3A -167.7(3) ?
Mn O1A C2A C1A 13.8(5) ?
C6A C1A C2A O1A 178.0(3) ?
C7A C1A C2A O1A -0.2(6) ?
C6A C1A C2A C3A -0.5(5) ?
C7A C1A C2A C3A -178.8(3) ?
O1A C2A C3A C4A -177.2(4) ?
C1A C2A C3A C4A 1.4(6) ?
C2A C3A C4A C5A -0.8(6) ?
C3A C4A C5A C6A -0.8(6) ?
C3A C4A C5A N5A 177.6(4) ?
O51A N5A C5A C6A -178.2(4) ?
O52A N5A C5A C6A 1.8(5) ?
O51A N5A C5A C4A 3.3(6) ?
O52A N5A C5A C4A -176.7(4) ?
C4A C5A C6A C1A 1.7(6) ?
N5A C5A C6A C1A -176.7(3) ?
C2A C1A C6A C5A -1.0(5) ?
C7A C1A C6A C5A 177.4(3) ?
C8A N1A C7A C1A 176.5(3) ?
Mn N1A C7A C1A -5.6(5) ?
C6A C1A C7A N1A 178.2(3) ?
C2A C1A C7A N1A -3.5(6) ?
C7A N1A C8A C8B 141.1(3) ?
Mn N1A C8A C8B -37.1(4) ?
Mn O1B C2B C1B 13.6(5) ?
Mn O1B C2B C3B -168.3(2) ?
C6B C1B C2B O1B 178.6(3) ?
C7B C1B C2B O1B 1.0(5) ?
C6B C1B C2B C3B 0.5(5) ?
C7B C1B C2B C3B -177.1(3) ?
O1B C2B C3B C4B -178.1(3) ?
C1B C2B C3B C4B 0.1(5) ?
C2B C3B C4B C5B -0.7(6) ?
C3B C4B C5B C6B 0.7(6) ?
C3B C4B C5B N5B 177.8(3) ?
O51B N5B C5B C6B -4.2(5) ?
O52B N5B C5B C6B 175.0(3) ?
O51B N5B C5B C4B 178.6(4) ?
O52B N5B C5B C4B -2.2(5) ?
C4B C5B C6B C1B -0.1(6) ?
N5B C5B C6B C1B -177.2(3) ?
C2B C1B C6B C5B -0.5(5) ?
C7B C1B C6B C5B 177.3(3) ?
C8B N1B C7B C1B 177.8(3) ?
Mn N1B C7B C1B -4.2(5) ?
C6B C1B C7B N1B 176.7(4) ?
C2B C1B C7B N1B -5.6(6) ?
C7B N1B C8B C8A 141.9(3) ?
Mn N1B C8B C8A -36.4(4) ?
N1A C8A C8B N1B 45.6(4) y
