#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:49:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179991 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/85/7028518.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_7028518
loop_
_publ_author_name
'Arroyo, Marta'
'Gómez-Iglesias, Patricia'
'Antón, Noelia'
'García-Rodríguez, Raúl'
'Alegria, Elisabete C. B. A.'
'Pombeiro, Armando J. L.'
'Miguel, Daniel'
'Villafañe, Fernando'
_publ_section_title
;
 Homo- and heteropolymetallic 3-(2-pyridyl)pyrazolate manganese and
 rhenium complexes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4009
_journal_page_last               4020
_journal_paper_doi               10.1039/c3dt53439a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C38 H24 Mn2 N12 Na2 O6'
_chemical_formula_weight         900.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 92.759(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.639(6)
_cell_length_b                   12.712(5)
_cell_length_c                   19.580(8)
_cell_measurement_reflns_used    909
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.085
_cell_measurement_theta_min      2.285
_cell_volume                     3888(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8447
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.712015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         2779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0309
_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)+(0.0478P)²+1.0867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                2252
_reflns_number_total             2779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53439a.txt
_cod_data_source_block           Compound_Na3a_ma2591am
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7028518
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Mn1 Mn 0.67919(2) 0.86077(3) 0.822739(18) 0.04298(16) Uani 1 1 d .
C1 C 0.70535(16) 0.7303(2) 0.84832(12) 0.0476(6) Uani 1 1 d .
O1 O 0.71517(14) 0.64469(16) 0.86710(11) 0.0690(6) Uani 1 1 d .
C2 C 0.69009(17) 0.8273(2) 0.73365(15) 0.0559(7) Uani 1 1 d .
O2 O 0.69673(14) 0.8051(2) 0.67769(11) 0.0882(7) Uani 1 1 d .
C3 C 0.56935(19) 0.8200(3) 0.82132(14) 0.0716(9) Uani 1 1 d .
O3 O 0.50066(15) 0.7912(3) 0.82469(13) 0.1381(14) Uani 1 1 d .
N1 N 0.64289(12) 1.01596(17) 0.80593(11) 0.0508(6) Uani 1 1 d .
N2 N 0.66615(11) 0.91196(17) 0.91879(9) 0.0427(5) Uani 1 1 d .
N3 N 0.66940(12) 0.86277(16) 0.98015(10) 0.0460(5) Uani 1 1 d .
C11 C 0.63594(17) 1.0665(2) 0.74606(15) 0.0634(8) Uani 1 1 d .
H11 H 0.6470 1.0294 0.7065 0.076 Uiso 1 1 calc R
C12 C 0.61334(18) 1.1704(3) 0.74013(17) 0.0712(9) Uani 1 1 d .
H12 H 0.6098 1.2030 0.6976 0.085 Uiso 1 1 calc R
C13 C 0.5962(2) 1.2247(3) 0.79760(19) 0.0758(9) Uani 1 1 d .
H13 H 0.5801 1.2951 0.7948 0.091 Uiso 1 1 calc R
C14 C 0.60274(19) 1.1752(2) 0.85974(17) 0.0668(8) Uani 1 1 d .
H14 H 0.5914 1.2119 0.8994 0.080 Uiso 1 1 calc R
C15 C 0.62623(14) 1.0708(2) 0.86313(14) 0.0501(7) Uani 1 1 d .
C16 C 0.63513(14) 1.0096(2) 0.92567(13) 0.0461(6) Uani 1 1 d .
C17 C 0.61695(16) 1.0263(2) 0.99294(14) 0.0562(7) Uani 1 1 d .
H17 H 0.5950 1.0867 1.0124 0.067 Uiso 1 1 calc R
C18 C 0.63881(16) 0.9334(2) 1.02436(13) 0.0556(7) Uani 1 1 d .
H18 H 0.6333 0.9203 1.0707 0.067 Uiso 1 1 calc R
Na Na 0.83640(6) 0.82486(8) 0.99454(5) 0.0535(3) Uani 1 1 d .
N4 N 0.98991(13) 0.85773(16) 0.98210(11) 0.0474(5) Uani 1 1 d .
N5 N 0.85700(11) 0.87897(14) 0.88288(10) 0.0390(5) Uani 1 1 d .
N6 N 0.80227(11) 0.91355(15) 0.83172(9) 0.0397(5) Uani 1 1 d .
C19 C 1.05625(18) 0.8393(2) 1.02658(15) 0.0605(8) Uani 1 1 d .
H19 H 1.0459 0.8038 1.0669 0.073 Uiso 1 1 calc R
C20 C 1.13862(18) 0.8703(2) 1.01570(17) 0.0691(9) Uani 1 1 d .
H20 H 1.1829 0.8555 1.0476 0.083 Uiso 1 1 calc R
C21 C 1.15381(18) 0.9232(2) 0.95696(18) 0.0695(9) Uani 1 1 d .
H21 H 1.2089 0.9453 0.9483 0.083 Uiso 1 1 calc R
C22 C 1.08672(16) 0.9436(2) 0.91046(15) 0.0574(7) Uani 1 1 d .
H22 H 1.0961 0.9799 0.8703 0.069 Uiso 1 1 calc R
C23 C 1.00478(14) 0.90920(19) 0.92432(13) 0.0435(6) Uani 1 1 d .
C24 C 0.93227(14) 0.92773(18) 0.87580(12) 0.0401(6) Uani 1 1 d .
C25 C 0.92616(17) 0.9944(2) 0.81991(14) 0.0586(8) Uani 1 1 d .
H25 H 0.9686 1.0376 0.8035 0.070 Uiso 1 1 calc R
C26 C 0.84400(17) 0.9828(2) 0.79417(13) 0.0540(7) Uani 1 1 d .
H26 H 0.8205 1.0180 0.7561 0.065 Uiso 1 1 calc R
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'
Na Na 0.0362 0.0249 '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
C1 Mn1 C3 86.66(13) . .
C1 Mn1 C2 91.22(12) . .
C3 Mn1 C2 92.96(13) . .
C1 Mn1 N2 94.06(10) . .
C3 Mn1 N2 88.16(11) . .
C2 Mn1 N2 174.65(11) . .
C1 Mn1 N6 94.55(10) . .
C3 Mn1 N6 175.25(12) . .
C2 Mn1 N6 91.61(10) . .
N2 Mn1 N6 87.17(8) . .
C1 Mn1 N1 172.32(10) . .
C3 Mn1 N1 91.03(13) . .
C2 Mn1 N1 96.21(11) . .
N2 Mn1 N1 78.53(8) . .
N6 Mn1 N1 87.18(8) . .
O1 C1 Mn1 173.9(2) . .
C1 O1 Na 97.65(17) . 7_667
O2 C2 Mn1 179.3(3) . .
O3 C3 Mn1 175.4(2) . .
C11 N1 C15 117.8(2) . .
C11 N1 Mn1 127.3(2) . .
C15 N1 Mn1 114.85(16) . .
C16 N2 N3 109.67(19) . .
C16 N2 Mn1 116.56(16) . .
N3 N2 Mn1 132.84(17) . .
C18 N3 N2 105.2(2) . .
C18 N3 Na 120.12(17) . 7_667
N2 N3 Na 129.22(16) . 7_667
C18 N3 Na 115.42(16) . .
N2 N3 Na 99.95(13) . .
Na N3 Na 81.20(7) 7_667 .
N1 C11 C12 123.2(3) . .
C13 C12 C11 118.7(3) . .
C12 C13 C14 119.6(3) . .
C13 C14 C15 119.6(3) . .
N1 C15 C14 121.2(2) . .
N1 C15 C16 114.0(2) . .
C14 C15 C16 124.9(3) . .
N2 C16 C17 109.4(2) . .
N2 C16 C15 115.6(2) . .
C17 C16 C15 135.0(3) . .
C18 C17 C16 103.8(2) . .
N3 C18 C17 112.0(2) . .
N5 Na N3 119.20(8) . 7_667
N5 Na N4 71.17(7) . .
N3 Na N4 103.43(8) 7_667 .
N5 Na N3 91.52(7) . .
N3 Na N3 98.80(7) 7_667 .
N4 Na N3 156.54(8) . .
N5 Na O1 153.89(8) . 7_667
N3 Na O1 85.74(7) 7_667 7_667
N4 Na O1 112.81(7) . 7_667
N3 Na O1 75.99(7) . 7_667
N5 Na Na 112.31(7) . 7_667
N3 Na Na 52.26(6) 7_667 7_667
N4 Na Na 154.78(8) . 7_667
N3 Na Na 46.53(5) . 7_667
O1 Na Na 75.62(5) 7_667 7_667
C23 N4 C19 118.3(2) . .
C23 N4 Na 112.16(16) . .
C19 N4 Na 129.30(18) . .
C24 N5 N6 107.37(18) . .
C24 N5 Na 113.25(15) . .
N6 N5 Na 132.59(14) . .
C26 N6 N5 108.15(19) . .
C26 N6 Mn1 130.79(17) . .
N5 N6 Mn1 121.05(14) . .
N4 C19 C20 123.4(3) . .
C21 C20 C19 118.4(3) . .
C20 C21 C22 119.4(3) . .
C21 C22 C23 119.3(3) . .
N4 C23 C22 121.2(2) . .
N4 C23 C24 117.9(2) . .
C22 C23 C24 121.0(2) . .
N5 C24 C25 109.7(2) . .
N5 C24 C23 120.9(2) . .
C25 C24 C23 129.3(2) . .
C26 C25 C24 104.7(2) . .
N6 C26 C25 110.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 C1 1.774(3) .
Mn1 C3 1.793(3) .
Mn1 C2 1.811(3) .
Mn1 N2 2.010(2) .
Mn1 N6 2.038(2) .
Mn1 N1 2.075(2) .
C1 O1 1.157(3) .
O1 Na 2.890(3) 7_667
C2 O2 1.141(3) .
C3 O3 1.140(3) .
N1 C11 1.337(3) .
N1 C15 1.355(3) .
N2 C16 1.341(3) .
N2 N3 1.353(3) .
N3 C18 1.351(3) .
N3 Na 2.439(2) 7_667
N3 Na 2.657(2) .
C11 C12 1.371(4) .
C12 C13 1.358(4) .
C13 C14 1.369(4) .
C14 C15 1.378(4) .
C15 C16 1.452(3) .
C16 C17 1.377(3) .
C17 C18 1.368(4) .
Na N5 2.329(2) .
Na N3 2.439(2) 7_667
Na N4 2.461(2) .
Na O1 2.890(3) 7_667
Na Na 3.321(2) 7_667
N4 C23 1.337(3) .
N4 C19 1.343(3) .
N5 C24 1.343(3) .
N5 N6 1.359(3) .
N6 C26 1.337(3) .
C19 C20 1.373(4) .
C20 C21 1.363(4) .
C21 C22 1.380(4) .
C22 C23 1.393(3) .
C23 C24 1.463(3) .
C24 C25 1.384(3) .
C25 C26 1.365(4) .
