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#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/26/7012699.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_7012699
loop_
_publ_author_name
'Yolanda Rodríguez-Martín'
'María Hernández-Molina'
'Joaquín Sanchiz'
'Catalina Ruiz-Pérez'
'Francesc Lloret'
'Miguel Julve'
_publ_section_title
;
 Crystal structures and magnetic properties of two- and
 three-dimensional malonato-bridged manganese(II) complexes
;
_journal_issue                   11
_journal_name_full               'Dalton Trans.'
_journal_page_first              2359
_journal_page_last               2365
_journal_paper_doi               10.1039/b300291h
_journal_year                    2003
_chemical_formula_sum            'C16 H16 Mn2 N2 O10'
_chemical_formula_weight         506.18
_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                 91.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.291(2)
_cell_length_b                   18.454(3)
_cell_length_c                   7.532(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      6
_cell_volume                     1013.0(4)
_computing_cell_refinement       'Enraf-Nonius CAD-4 Express'
_computing_data_collection       'Enraf-Nonius CAD-4 Express'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'PARST95 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'MACH-3 four-circle diffractometer'
_diffrn_measurement_method       w-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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3144
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        <10%
_exptl_absorpt_coefficient_mu    1.303
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2942
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0557
_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)+(0.0794P)²+1.7242P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                1897
_reflns_number_total             2942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300291h.txt
_cod_data_source_block           COMPOUND_2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7012699
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 0.09591(8) 0.20604(3) 0.11173(7) 0.02383(18) Uani 1 1 d . . .
O1 O -0.0678(4) 0.26897(17) -0.0770(4) 0.0343(7) Uani 1 1 d . . .
O2 O 0.2194(4) 0.15071(16) 0.3386(4) 0.0324(7) Uani 1 1 d . . .
O3 O -0.0619(4) 0.26511(16) 0.3043(4) 0.0321(6) Uani 1 1 d . . .
O4 O 0.2317(4) 0.15501(16) -0.1078(4) 0.0343(7) Uani 1 1 d . . .
C1 C -0.1624(5) 0.3255(2) -0.0524(5) 0.0248(8) Uani 1 1 d . . .
C2 C -0.1284(6) 0.3679(2) 0.1191(5) 0.0299(9) Uani 1 1 d . . .
C3 C -0.1555(5) 0.3222(2) 0.2842(5) 0.0247(7) Uani 1 1 d . . .
C11 C -0.4127(8) 0.0706(4) 0.1558(9) 0.0698(11) Uani 1 1 d . . .
H11 H -0.5085 0.0719 0.2347 0.084 Uiso 1 1 calc R . .
C12 C -0.2625(8) 0.1159(4) 0.1818(9) 0.0698(11) Uani 1 1 d . . .
H12 H -0.2612 0.1466 0.2799 0.084 Uiso 1 1 calc R . .
C13 C -0.1301(8) 0.0734(4) -0.0578(9) 0.0698(11) Uani 1 1 d . . .
H13 H -0.0328 0.0732 -0.1349 0.084 Uiso 1 1 calc R . .
C14 C -0.2730(2) 0.02632(10) -0.0931(3) 0.0698(11) Uani 1 1 d . . .
H14 H -0.2698 -0.0043 -0.1910 0.084 Uiso 1 1 calc R . .
C15 C -0.4201(2) 0.02462(10) 0.0162(3) 0.0316(9) Uani 1 1 d R . .
N1 N -0.1215(2) 0.11834(10) 0.0764(3) 0.0342(8) Uani 1 1 d R . .
O1W O 0.3142(2) 0.29113(10) 0.1124(3) 0.0329(6) Uani 1 1 d RD . .
H2 H -0.2156 0.4129 0.1077 0.038(13) Uiso 1 1 d R . .
H11W H 0.3819 0.2764 0.0059 0.047(15) Uiso 1 1 d RD . .
H12W H 0.3895 0.2780 0.2186 0.07(2) Uiso 1 1 d RD . .
H1 H -0.0166 0.3795 0.1226 0.063(19) Uiso 1 1 d 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'
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
O2 Mn1 O1 168.35(12) . . ?
O2 Mn1 O4 102.04(12) . . ?
O1 Mn1 O4 89.29(12) . . ?
O2 Mn1 O3 85.75(11) . . ?
O1 Mn1 O3 82.90(11) . . ?
O4 Mn1 O3 172.19(11) . . ?
O2 Mn1 O1W 92.87(10) . . ?
O1 Mn1 O1W 90.20(11) . . ?
O4 Mn1 O1W 88.04(10) . . ?
O3 Mn1 O1W 92.13(10) . . ?
O2 Mn1 N1 91.67(9) . . ?
O1 Mn1 N1 86.33(10) . . ?
O4 Mn1 N1 86.21(9) . . ?
O3 Mn1 N1 93.11(10) . . ?
O1W Mn1 N1 173.31(10) . . ?
C1 O1 Mn1 129.6(2) . . ?
C1 O2 Mn1 127.9(3) 4_666 . ?
C3 O3 Mn1 129.4(2) . . ?
C3 O4 Mn1 132.5(3) 4_665 . ?
O2 C1 O1 124.0(4) 4_565 . ?
O2 C1 C2 117.9(4) 4_565 . ?
O1 C1 C2 118.1(3) . . ?
C3 C2 C1 112.7(3) . . ?
C3 C2 H2 114.4 . . ?
C1 C2 H2 104.7 . . ?
C3 C2 H1 105.3 . . ?
C1 C2 H1 106.9 . . ?
H2 C2 H1 112.7 . . ?
O4 C3 O3 124.6(4) 4_566 . ?
O4 C3 C2 116.7(4) 4_566 . ?
O3 C3 C2 118.6(3) . . ?
C15 C11 C12 120.1(5) . . ?
C15 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
N1 C12 C11 124.2(5) . . ?
N1 C12 H12 117.9 . . ?
C11 C12 H12 117.9 . . ?
N1 C13 C14 124.6(4) . . ?
N1 C13 H13 117.7 . . ?
C14 C13 H13 117.7 . . ?
C15 C14 C13 119.9(2) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C11 C15 C14 116.0(2) . . ?
C11 C15 C15 121.5(3) . 3_455 ?
C14 C15 C15 122.45(15) . 3_455 ?
C13 N1 C12 115.1(4) . . ?
C13 N1 Mn1 124.0(3) . . ?
C12 N1 Mn1 120.4(3) . . ?
Mn1 O1W H11W 100.2 . . ?
Mn1 O1W H12W 102.1 . . ?
H11W O1W H12W 108.1 . . ?
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 O2 2.164(3) . ?
Mn1 O1 2.167(3) . ?
Mn1 O4 2.168(3) . ?
Mn1 O3 2.171(3) . ?
Mn1 O1W 2.2354(18) . ?
Mn1 N1 2.2755(18) . ?
O1 C1 1.267(5) . ?
O2 C1 1.252(5) 4_666 ?
O3 C3 1.262(5) . ?
O4 C3 1.247(5) 4_665 ?
C1 O2 1.252(5) 4_565 ?
C1 C2 1.525(5) . ?
C2 C3 1.521(5) . ?
C2 H2 1.0478 . ?
C2 H1 0.8423 . ?
C3 O4 1.247(5) 4_566 ?
C11 C15 1.351(6) . ?
C11 C12 1.387(7) . ?
C11 H11 0.9300 . ?
C12 N1 1.318(6) . ?
C12 H12 0.9300 . ?
C13 N1 1.308(6) . ?
C13 C14 1.376(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.3715 . ?
C14 H14 0.9300 . ?
C15 C15 1.492(3) 3_455 ?
O1W H11W 0.9919 . ?
O1W H12W 0.9877 . ?
