#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179758 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/54/7005462.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_7005462
loop_
_publ_author_name
'Alvarez, Celedonio M.'
'García-Rodríguez, Raúl'
'Miguel, Daniel'
_publ_section_title
;
 Pyridine-2-carboxaldehyde as ligand: synthesis and derivatization of
 carbonyl complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3546
_journal_page_last               3554
_journal_paper_doi               10.1039/b702418e
_journal_year                    2007
_chemical_formula_sum            'C9 H5 Cl Mn N O8'
_chemical_formula_weight         345.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_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                 98.857(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.206(5)
_cell_length_b                   7.084(3)
_cell_length_c                   16.026(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1257.0(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0139
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5364
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.747138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'DARK RED'
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0025(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0283
_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)+(0.0371P)²+0.9701P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                1678
_reflns_number_total             1809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702418e.txt
_cod_data_source_block           Compound_3a_rg263am
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_cell_volume        1257.1(9)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7005462
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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_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 0.33980(3) 0.31963(6) 0.57825(2) 0.04579(19) Uani 1 1 d . . .
N1 N 0.23950(17) 0.1271(3) 0.50322(12) 0.0384(5) Uani 1 1 d . . .
C1 C 0.4794(3) 0.2123(5) 0.56578(19) 0.0581(8) Uani 1 1 d . . .
O1 O 0.5692(2) 0.1432(4) 0.56113(17) 0.0826(8) Uani 1 1 d . . .
C2 C 0.4237(3) 0.5172(6) 0.6285(2) 0.0732(10) Uani 1 1 d . . .
O2 O 0.4806(3) 0.6400(5) 0.6565(2) 0.1201(13) Uani 1 1 d . . .
C3 C 0.3488(3) 0.1947(6) 0.6761(2) 0.0650(9) Uani 1 1 d . . .
O3 O 0.3581(2) 0.1104(5) 0.73695(16) 0.1042(10) Uani 1 1 d . . .
O4 O 0.32010(17) 0.4505(3) 0.46394(12) 0.0508(5) Uani 1 1 d . . .
C11 C 0.1958(2) -0.0365(4) 0.52315(18) 0.0505(7) Uani 1 1 d . . .
H11 H 0.2107 -0.0761 0.5791 0.061 Uiso 1 1 calc R . .
C12 C 0.1295(3) -0.1505(4) 0.4647(2) 0.0605(8) Uani 1 1 d . . .
H12 H 0.0997 -0.2648 0.4813 0.073 Uiso 1 1 calc R . .
C13 C 0.1070(3) -0.0971(4) 0.3826(2) 0.0600(8) Uani 1 1 d . . .
H13 H 0.0629 -0.1744 0.3422 0.072 Uiso 1 1 calc R . .
C14 C 0.1503(2) 0.0721(4) 0.36059(17) 0.0507(7) Uani 1 1 d . . .
H14 H 0.1363 0.1130 0.3048 0.061 Uiso 1 1 calc R . .
C15 C 0.2146(2) 0.1804(4) 0.42182(15) 0.0385(6) Uani 1 1 d . . .
C16 C 0.2622(2) 0.3633(4) 0.40661(18) 0.0473(7) Uani 1 1 d . . .
H16 H 0.2484 0.4148 0.3526 0.057 Uiso 1 1 calc R . .
Cl1 Cl 0.12558(6) 0.50816(9) 0.65456(4) 0.0452(2) Uani 1 1 d . . .
O11 O 0.17301(16) 0.4378(3) 0.58061(11) 0.0508(5) Uani 1 1 d . . .
O12 O 0.1350(2) 0.3683(3) 0.71679(15) 0.0766(7) Uani 1 1 d . . .
O13 O 0.1946(3) 0.6646(3) 0.68614(16) 0.0840(8) Uani 1 1 d . . .
O14 O 0.0048(2) 0.5568(4) 0.62692(16) 0.0799(7) 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
C1 Mn1 C3 87.43(14) . . ?
C1 Mn1 C2 88.58(15) . . ?
C3 Mn1 C2 92.11(17) . . ?
C1 Mn1 O4 93.96(12) . . ?
C3 Mn1 O4 176.20(12) . . ?
C2 Mn1 O4 91.46(14) . . ?
C1 Mn1 N1 93.57(12) . . ?
C3 Mn1 N1 97.93(13) . . ?
C2 Mn1 N1 169.81(14) . . ?
O4 Mn1 N1 78.47(8) . . ?
C1 Mn1 O11 174.47(11) . . ?
C3 Mn1 O11 96.55(11) . . ?
C2 Mn1 O11 95.09(12) . . ?
O4 Mn1 O11 81.83(8) . . ?
N1 Mn1 O11 82.11(8) . . ?
C11 N1 C15 116.9(2) . . ?
C11 N1 Mn1 129.63(19) . . ?
C15 N1 Mn1 113.43(17) . . ?
O1 C1 Mn1 177.3(3) . . ?
O2 C2 Mn1 175.9(3) . . ?
O3 C3 Mn1 177.0(3) . . ?
C16 O4 Mn1 114.97(18) . . ?
N1 C11 C12 122.5(3) . . ?
C13 C12 C11 120.1(3) . . ?
C12 C13 C14 118.5(3) . . ?
C13 C14 C15 118.7(3) . . ?
N1 C15 C14 123.3(2) . . ?
N1 C15 C16 113.0(2) . . ?
C14 C15 C16 123.7(2) . . ?
O4 C16 C15 120.1(3) . . ?
O12 Cl1 O13 109.03(17) . . ?
O12 Cl1 O14 111.30(16) . . ?
O13 Cl1 O14 111.88(17) . . ?
O12 Cl1 O11 109.89(14) . . ?
O13 Cl1 O11 108.28(14) . . ?
O14 Cl1 O11 106.39(13) . . ?
Cl1 O11 Mn1 126.90(11) . . ?
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 C1 1.778(3) . ?
Mn1 C3 1.790(4) . ?
Mn1 C2 1.805(4) . ?
Mn1 O4 2.035(2) . ?
Mn1 N1 2.038(2) . ?
Mn1 O11 2.0536(19) . ?
N1 C11 1.317(4) . ?
N1 C15 1.345(3) . ?
C1 O1 1.131(4) . ?
C2 O2 1.130(4) . ?
C3 O3 1.134(4) . ?
O4 C16 1.210(3) . ?
C11 C12 1.367(4) . ?
C12 C13 1.355(4) . ?
C13 C14 1.360(4) . ?
C14 C15 1.361(4) . ?
C15 C16 1.436(4) . ?
Cl1 O12 1.398(2) . ?
Cl1 O13 1.401(2) . ?
Cl1 O14 1.401(2) . ?
Cl1 O11 1.4593(19) . ?
