#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:29:31 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179898 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/94/7019472.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_7019472
loop_
_publ_author_name
'Alvarez, Celedonio M.'
'Alvarez-Miguel, Lucía'
'García-Rodríguez, Raúl'
'Miguel, Daniel'
_publ_section_title
;
 Complexes with 3-(pyridin-2-yl)imidazo[1,5-a]pyridine ligands by
 spontaneous dimerization of pyridine-2-carboxaldehyde within the
 coordination sphere of manganese(ii) in a one-pot reaction.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7041
_journal_page_last               7046
_journal_paper_doi               10.1039/c2dt30453h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C20 H29 Mn N3 O4 P2 S4'
_chemical_formula_weight         620.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.219(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5548(4)
_cell_length_b                   17.5085(4)
_cell_length_c                   16.3988(4)
_cell_measurement_reflns_used    5246
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4588
_cell_measurement_theta_min      2.0392
_cell_volume                     2878.55(15)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω 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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14704
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.3143
_exptl_crystal_size_mid          0.1678
_exptl_crystal_size_min          0.0673
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0670P)²+2.9134P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                4019
_reflns_number_total             6697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30453h.txt
_cod_data_source_block           Compound_2a_lam19c
_cod_original_cell_volume        2878.56(15)
_cod_database_code               7019472
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_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 0.56682(7) 0.77753(4) 0.91990(4) 0.0636(2) Uani 1 1 d . . .
S1 S 0.75031(13) 0.77419(8) 0.84245(8) 0.0848(4) Uani 1 1 d . . .
S2 S 0.45825(13) 0.68970(8) 0.78829(8) 0.0827(4) Uani 1 1 d . . .
S3 S 0.67276(15) 0.67294(8) 1.03324(9) 0.0905(4) Uani 1 1 d . . .
S4 S 0.38963(15) 0.76448(8) 0.99924(9) 0.0878(4) Uani 1 1 d . . .
N1 N 0.4677(4) 0.8884(2) 0.8553(2) 0.0676(9) Uani 1 1 d . . .
N2 N 0.6823(3) 0.87366(17) 0.99445(19) 0.0604(8) Uani 1 1 d . . .
N3 N 0.7496(4) 0.99299(18) 0.9971(2) 0.0638(9) Uani 1 1 d . . .
P1 P 0.62625(13) 0.70447(7) 0.76081(7) 0.0724(4) Uani 1 1 d . . .
P2 P 0.51045(17) 0.68396(8) 1.06567(8) 0.0879(4) Uani 1 1 d . A .
O34 O 0.5552(6) 0.6961(3) 1.1646(2) 0.148(2) Uani 1 1 d G . .
C37A C 0.4783(5) 0.7252(6) 1.2154(4) 0.124(3) Uani 0.70 1 d PG A 1
H37A H 0.4309 0.6839 1.2326 0.149 Uiso 0.70 1 d PG A 1
H37B H 0.4134 0.7618 1.1824 0.149 Uiso 0.70 1 d PG A 1
C37B C 0.5507(12) 0.7711(3) 1.1992(4) 0.126(9) Uani 0.30 1 d PG A 2
H37C H 0.4651 0.7948 1.1711 0.151 Uiso 0.30 1 d PG A 2
H37D H 0.6201 0.8030 1.1899 0.151 Uiso 0.30 1 d PG A 2
C38 C 0.5712(7) 0.7632(4) 1.2933(3) 0.156(3) Uani 1 1 d G A .
H38A H 0.6561 0.7378 1.3093 0.234 Uiso 1 1 d G A .
H38B H 0.5344 0.7603 1.3398 0.234 Uiso 1 1 d G A .
H38C H 0.5827 0.8158 1.2806 0.234 Uiso 1 1 d G A .
C1 C 0.3500(5) 0.8928(3) 0.7925(3) 0.0795(13) Uani 1 1 d . . .
H1 H 0.3112 0.8478 0.7660 0.095 Uiso 1 1 calc R . .
C2 C 0.2848(6) 0.9601(3) 0.7660(3) 0.0910(15) Uani 1 1 d . . .
H2 H 0.2042 0.9605 0.7216 0.109 Uiso 1 1 calc R . .
C3 C 0.3389(5) 1.0274(3) 0.8053(3) 0.0884(16) Uani 1 1 d . . .
H3 H 0.2940 1.0734 0.7890 0.106 Uiso 1 1 calc R . .
C4 C 0.4604(5) 1.0257(3) 0.8689(3) 0.0728(12) Uani 1 1 d . . .
H4 H 0.4999 1.0703 0.8959 0.087 Uiso 1 1 calc R . .
C5 C 0.5231(4) 0.9539(2) 0.8917(2) 0.0590(10) Uani 1 1 d . . .
C6 C 0.6492(4) 0.9425(2) 0.9591(2) 0.0554(9) Uani 1 1 d . . .
C7 C 0.8015(4) 0.8788(2) 1.0560(2) 0.0648(11) Uani 1 1 d . . .
H7 H 0.8447 0.8384 1.0903 0.078 Uiso 1 1 calc R . .
C8 C 0.8502(4) 0.9518(2) 1.0612(3) 0.0664(11) Uani 1 1 d . . .
C9 C 0.9642(5) 0.9901(3) 1.1094(3) 0.0894(15) Uani 1 1 d . . .
H9 H 1.0289 0.9645 1.1526 0.107 Uiso 1 1 calc R . .
C10 C 0.9810(6) 1.0642(3) 1.0937(4) 0.1029(18) Uani 1 1 d . . .
H10 H 1.0574 1.0898 1.1260 0.123 Uiso 1 1 calc R . .
C11 C 0.8837(6) 1.1030(3) 1.0286(5) 0.1040(19) Uani 1 1 d . . .
H11 H 0.8974 1.1541 1.0182 0.125 Uiso 1 1 calc R . .
C12 C 0.7721(6) 1.0687(3) 0.9811(4) 0.0878(15) Uani 1 1 d . . .
H12 H 0.7098 1.0954 0.9376 0.105 Uiso 1 1 calc R . .
O31 O 0.6936(4) 0.62635(18) 0.7509(2) 0.0959(11) Uani 1 1 d G . .
C31 C 0.7473(7) 0.5781(3) 0.8239(2) 0.147(3) Uani 1 1 d G . .
H31A H 0.6757 0.5557 0.8412 0.176 Uiso 1 1 d G . .
H31B H 0.8035 0.6076 0.8716 0.176 Uiso 1 1 d G . .
C32 C 0.8274(9) 0.5166(4) 0.7999(5) 0.195(4) Uani 1 1 d G . .
H32A H 0.7699 0.4748 0.7741 0.292 Uiso 1 1 d G . .
H32B H 0.8951 0.4990 0.8504 0.292 Uiso 1 1 d G . .
H32C H 0.8685 0.5364 0.7597 0.292 Uiso 1 1 d G . .
O32 O 0.6005(4) 0.72980(19) 0.66439(19) 0.0872(10) Uani 1 1 d . . .
C33 C 0.5509(7) 0.8048(3) 0.6370(4) 0.114(2) Uani 1 1 d . . .
H33A H 0.6135 0.8427 0.6697 0.137 Uiso 1 1 calc R . .
H33B H 0.4666 0.8124 0.6479 0.137 Uiso 1 1 calc R . .
C34 C 0.5322(7) 0.8152(4) 0.5464(4) 0.121(2) Uani 1 1 d . . .
H34A H 0.6172 0.8140 0.5366 0.181 Uiso 1 1 calc R . .
H34B H 0.4900 0.8635 0.5280 0.181 Uiso 1 1 calc R . .
H34C H 0.4769 0.7749 0.5144 0.181 Uiso 1 1 calc R . .
O33 O 0.4277(5) 0.6052(3) 1.0593(3) 0.1307(16) Uani 1 1 d G . .
C35 C 0.3678(7) 0.5735(5) 0.9750(4) 0.186(4) Uani 1 1 d G A .
H35A H 0.4257 0.5347 0.9638 0.224 Uiso 1 1 d G A .
H35B H 0.3559 0.6133 0.9321 0.224 Uiso 1 1 d G A .
C36 C 0.2372(7) 0.5395(5) 0.9695(5) 0.207(5) Uani 1 1 d G A .
H36A H 0.2433 0.5141 1.0225 0.310 Uiso 1 1 d G A .
H36B H 0.2123 0.5034 0.9232 0.310 Uiso 1 1 d G A .
H36C H 0.1710 0.5791 0.9592 0.310 Uiso 1 1 d G A .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N2 Mn1 N1 72.83(12)
N2 Mn1 S3 95.82(9)
N1 Mn1 S3 162.86(9)
N2 Mn1 S4 98.56(10)
N1 Mn1 S4 90.56(10)
S3 Mn1 S4 78.24(5)
N2 Mn1 S2 158.68(10)
N1 Mn1 S2 95.61(10)
S3 Mn1 S2 98.97(5)
S4 Mn1 S2 99.42(5)
N2 Mn1 S1 85.52(10)
N1 Mn1 S1 95.40(10)
S3 Mn1 S1 96.47(5)
S4 Mn1 S1 173.58(5)
S2 Mn1 S1 77.66(4)
P1 S1 Mn1 84.76(6)
P1 S2 Mn1 85.30(5)
P2 S3 Mn1 84.69(6)
P2 S4 Mn1 84.13(6)
C5 N1 C1 117.5(4)
C5 N1 Mn1 116.5(3)
C1 N1 Mn1 125.4(3)
C6 N2 C7 108.7(3)
C6 N2 Mn1 115.0(2)
C7 N2 Mn1 133.7(3)
C6 N3 C12 133.2(4)
C6 N3 C8 107.4(3)
C12 N3 C8 119.3(4)
O31 P1 O32 94.71(18)
O31 P1 S1 112.46(15)
O32 P1 S1 111.99(15)
O31 P1 S2 112.09(17)
O32 P1 S2 112.25(16)
S1 P1 S2 112.20(7)
O34 P2 O33 99.6(3)
O34 P2 S3 106.9(2)
O33 P2 S3 113.52(19)
O34 P2 S4 114.15(18)
O33 P2 S4 109.2(2)
S3 P2 S4 112.85(9)
C37A O34 P2 127.9(4)
C37B O34 P2 120.0(4)
O34 C37A C38 108.4
O34 C37B C38 108.1
N1 C1 C2 123.1(5)
C1 C2 C3 119.7(5)
C4 C3 C2 119.1(5)
C3 C4 C5 117.9(5)
N1 C5 C4 122.7(4)
N1 C5 C6 112.8(3)
C4 C5 C6 124.4(4)
N2 C6 N3 109.0(3)
N2 C6 C5 120.5(4)
N3 C6 C5 130.5(3)
N2 C7 C8 110.7(3)
C7 C8 C9 136.7(4)
C7 C8 N3 104.2(4)
C9 C8 N3 119.1(4)
C10 C9 C8 119.9(5)
C9 C10 C11 120.2(5)
C12 C11 C10 121.9(5)
C11 C12 N3 119.5(5)
C31 O31 P1 120.1(3)
O31 C31 C32 108.3
C33 O32 P1 120.1(3)
O32 C33 C34 110.8(5)
C35 O33 P2 117.2(4)
O33 C35 C36 109.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn1 N2 2.209(3)
Mn1 N1 2.300(4)
Mn1 S3 2.5998(13)
Mn1 S4 2.6008(15)
Mn1 S2 2.6056(13)
Mn1 S1 2.6278(15)
S1 P1 1.9750(16)
S2 P1 1.9784(19)
S3 P2 1.956(2)
S4 P2 1.9828(18)
N1 C5 1.341(5)
N1 C1 1.345(5)
N2 C6 1.335(5)
N2 C7 1.347(5)
N3 C6 1.371(5)
N3 C12 1.386(6)
N3 C8 1.433(5)
P1 O31 1.573(3)
P1 O32 1.582(3)
P2 O34 1.556(4)
P2 O33 1.619(5)
O34 C37A 1.4270
O34 C37B 1.4375
C37A C38 1.5006
C37B C38 1.4954
C1 C2 1.365(7)
C2 C3 1.379(7)
C3 C4 1.377(6)
C4 C5 1.415(6)
C5 C6 1.454(5)
C7 C8 1.371(6)
C8 C9 1.388(6)
C9 C10 1.346(7)
C10 C11 1.404(8)
C11 C12 1.335(7)
O31 C31 1.4293
C31 C32 1.4961
O32 C33 1.434(7)
C33 C34 1.448(7)
O33 C35 1.4382
C35 C36 1.4779
