#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:26:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322551.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_4322551
loop_
_publ_author_name
'Sanjib Ganguly'
'Soma Karmakar'
'Chandan Kumar Pal'
'Animesh Chakravorty'
_publ_section_title
;
 Regiospecific Oximato Coordination at the Oxygen Site: Ligand Design and
 Low-Spin MnII and FeII/III Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5984
_journal_page_last               5987
_journal_paper_doi               10.1021/ic9907011
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C25 H19 Cl2 Mn N8 O2'
_chemical_formula_weight         589.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.01(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.142(7)
_cell_length_b                   10.721(7)
_cell_length_c                   16.973(10)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     2570(3)
_computing_cell_refinement       'Siemens Shelxtl-Plus,(Sheldrick, 1990)'
_computing_data_collection       'Siemens Shelxtl-Plus,(Sheldrick, 1990)'
_computing_data_reduction        'Siemens Shelxtl-Plus,(Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXTL V-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL V-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       'ω scan'
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2453
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        Nil
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.7199
_exptl_absorpt_correction_T_min  0.6635
_exptl_absorpt_correction_type   'Semi empirical'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_obs          0.0547
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0579P)²+5.5581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1442
_refine_ls_wR_factor_obs         0.1251
_reflns_number_observed          1673
_reflns_number_total             2280
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9907011_1.cif
_cod_data_source_block           '[Mn(HL)2].CH2Cl2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (9 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (23
times).

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+5.5581P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+5.5581P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2569.8(26)
_cod_database_code               4322551
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn Mn 0.7500 -0.02139(7) 0.0000 0.0487(3) Uani 1 d S .
N1 N 0.6662(2) -0.1530(3) -0.0481(2) 0.0524(8) Uani 1 d . .
N2 N 0.7363(2) 0.1226(3) 0.1345(2) 0.0595(9) Uani 1 d . .
N3 N 0.6488(2) -0.0221(3) 0.0668(2) 0.0472(7) Uani 1 d . .
N4 N 0.5741(2) -0.0956(3) 0.0567(2) 0.0567(8) Uani 1 d . .
O1 O 0.7937(2) 0.0994(2) 0.0745(2) 0.0623(7) Uani 1 d . .
C3 C 0.5324(4) -0.3267(4) -0.0982(3) 0.084(2) Uani 1 d . .
H3 H 0.4873(4) -0.3850(4) -0.1156(3) 0.100 Uiso 1 calc R .
C2 C 0.6146(4) -0.3137(4) -0.1370(3) 0.0785(14) Uani 1 d . .
H2 H 0.6258(4) -0.3636(4) -0.1804(3) 0.094 Uiso 1 calc R .
C4 C 0.5169(4) -0.2542(4) -0.0342(3) 0.0744(13) Uani 1 d . .
H4 H 0.4615(4) -0.2625(4) -0.0075(3) 0.089 Uiso 1 calc R .
C1 C 0.6804(3) -0.2262(4) -0.1111(2) 0.0675(12) Uani 1 d . .
H1 H 0.7359(3) -0.2172(4) -0.1377(2) 0.081 Uiso 1 calc R .
C5 C 0.5854(3) -0.1675(3) -0.0092(2) 0.0556(10) Uani 1 d . .
C6 C 0.6575(3) 0.0593(3) 0.1318(2) 0.0491(9) Uani 1 d . .
C7 C 0.5902(3) 0.0796(3) 0.1937(2) 0.0501(9) Uani 1 d . .
C9 C 0.5547(4) 0.1876(4) 0.3131(3) 0.0763(13) Uani 1 d . .
H9 H 0.5732(4) 0.2431(4) 0.3531(3) 0.092 Uiso 1 calc R .
C8 C 0.6159(3) 0.1598(4) 0.2552(3) 0.0693(12) Uani 1 d . .
H8 H 0.6759(3) 0.1956(4) 0.2574(3) 0.083 Uiso 1 calc R .
C10 C 0.4670(4) 0.1340(4) 0.3121(3) 0.0709(12) Uani 1 d . .
H10 H 0.4257(4) 0.1525(4) 0.3513(3) 0.085 Uiso 1 calc R .
C11 C 0.4404(3) 0.0524(4) 0.2525(3) 0.0698(12) Uani 1 d . .
H11 H 0.3811(3) 0.0148(4) 0.2519(3) 0.084 Uiso 1 calc R .
C12 C 0.5008(3) 0.0256(4) 0.1937(2) 0.0591(10) Uani 1 d . .
H12 H 0.4815(3) -0.0292(4) 0.1535(2) 0.071 Uiso 1 calc R .
C1S C 0.7500 0.3967(9) 0.0000 0.240(9) Uani 1 d S .
H1S H 0.7500 0.3100(9) 0.0000 0.288 Uiso 1 calc SR .
Cl1S Cl 0.8103(2) 0.4699(2) -0.0631(2) 0.1982(13) Uani 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'
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
N3 Mn N3 179.5(2) . 2_655 y
N3 Mn O1 80.26(12) . . y
N3 Mn O1 100.05(12) 2_655 . y
N3 Mn O1 100.05(13) . 2_655 y
N3 Mn O1 80.26(12) 2_655 2_655 y
O1 Mn O1 93.6(2) . 2_655 y
N3 Mn N1 77.74(13) . . y
N3 Mn N1 101.93(14) 2_655 . y
O1 Mn N1 157.87(13) . . y
O1 Mn N1 92.57(13) 2_655 . y
N3 Mn N1 101.93(14) . 2_655 y
N3 Mn N1 77.74(13) 2_655 2_655 y
O1 Mn N1 92.57(13) . 2_655 y
O1 Mn N1 157.87(13) 2_655 2_655 y
N1 Mn N1 89.7(2) . 2_655 y
C1 N1 C5 118.8(4) . . ?
C1 N1 Mn 128.8(3) . . ?
C5 N1 Mn 112.3(2) . . y
C6 N2 O1 114.9(3) . . y
N4 N3 C6 120.6(3) . . ?
N4 N3 Mn 123.7(2) . . y
C6 N3 Mn 115.7(2) . . y
N3 N4 C5 108.3(3) . . y
N2 O1 Mn 116.1(2) . . y
C4 C3 C2 120.0(4) . . ?
C3 C2 C1 119.4(4) . . ?
C3 C4 C5 119.0(5) . . ?
N1 C1 C2 121.5(5) . . ?
N1 C5 N4 117.9(3) . . y
N1 C5 C4 121.2(4) . . ?
N4 C5 C4 120.9(4) . . ?
N2 C6 N3 113.0(3) . . y
N2 C6 C7 118.8(3) . . ?
N3 C6 C7 128.2(3) . . ?
C8 C7 C12 117.5(4) . . ?
C8 C7 C6 118.4(4) . . ?
C12 C7 C6 124.1(3) . . ?
C10 C9 C8 120.3(4) . . ?
C9 C8 C7 121.5(4) . . ?
C9 C10 C11 119.3(4) . . ?
C10 C11 C12 120.7(4) . . ?
C11 C12 C7 120.7(4) . . ?
Cl1S C1S Cl1S 121.6(6) . 2_655 ?
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
Mn N3 1.873(3) . y
Mn N3 1.873(3) 2_655 ?
Mn O1 1.891(3) . y
Mn O1 1.891(3) 2_655 ?
Mn N1 1.990(3) . y
Mn N1 1.990(3) 2_655 ?
N1 C1 1.350(5) . ?
N1 C5 1.358(5) . y
N2 C6 1.304(5) . y
N2 O1 1.357(4) . y
N3 N4 1.322(4) . y
N3 C6 1.406(5) . y
N4 C5 1.375(5) . y
C3 C4 1.363(6) . ?
C3 C2 1.373(7) . ?
C2 C1 1.377(6) . ?
C4 C5 1.392(5) . ?
C6 C7 1.471(5) . ?
C7 C8 1.386(5) . ?
C7 C12 1.390(5) . ?
C9 C10 1.367(6) . ?
C9 C8 1.376(6) . ?
C10 C11 1.375(6) . ?
C11 C12 1.377(6) . ?
C1S Cl1S 1.607(5) . ?
C1S Cl1S 1.607(5) 2_655 ?
