#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:33:27 +0100 (jue 24 de mar de 2016) $
#$Revision: 179585 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/50/4505052.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_4505052
loop_
_publ_author_name
'Ang, Siau Gek'
'Sun, Bai Wang'
_publ_section_title
;
 Crystal Structure and Characterization of Organic−Inorganic
 Hybridized Molecules with Molecular Zipper Structures and Two-Dimensional
 Grid Networks
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              383
_journal_paper_doi               10.1021/cg049847n
_journal_volume                  5
_journal_year                    2005
_chemical_formula_sum            'C14 H16 Mn N2 O8'
_chemical_formula_weight         395.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.549(2)
_cell_angle_beta                 84.745(2)
_cell_angle_gamma                73.427(2)
_cell_formula_units_Z            1
_cell_length_a                   5.4059(3)
_cell_length_b                   7.2938(3)
_cell_length_c                   9.9853(4)
_cell_measurement_reflns_used    3112
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.05
_cell_volume                     375.53(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       ω
_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  0.0125
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3112
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             203
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0474P)²+0.1259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                2071
_reflns_number_total             2139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg049847nsi20040509_123106.cif
_cod_data_source_block           Mn(dpdo)(H2O)2(C4H4O4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505052
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.0000 0.0000 0.0000 0.01650(10) Uani 1 2 d S
O1 O -0.17723(19) -0.23948(15) 0.05029(9) 0.0221(2) Uani 1 1 d .
O2 O 0.09680(19) 0.00014(15) 0.19983(9) 0.0222(2) Uani 1 1 d .
O3 O -0.2696(2) 0.16160(17) 0.31330(10) 0.0282(2) Uani 1 1 d .
O4 O 0.3642(2) -0.21933(16) -0.05160(11) 0.0244(2) Uani 1 1 d .
N1 N -0.1361(2) -0.32188(16) 0.17199(11) 0.0181(2) Uani 1 1 d .
C1 C 0.0971(3) -0.44519(19) 0.19320(13) 0.0214(2) Uani 1 1 d .
H1A H 0.2221 -0.4810 0.1205 0.026 Uiso 1 1 calc R
C2 C 0.1530(3) -0.51886(19) 0.32071(13) 0.0207(2) Uani 1 1 d .
H2A H 0.3159 -0.6048 0.3343 0.025 Uiso 1 1 calc R
C3 C -0.0304(2) -0.46707(17) 0.43042(12) 0.0163(2) Uani 1 1 d .
C4 C -0.2741(2) -0.3470(2) 0.40224(13) 0.0204(2) Uani 1 1 d .
H4A H -0.4058 -0.3147 0.4722 0.024 Uiso 1 1 calc R
C5 C -0.3235(2) -0.2755(2) 0.27322(13) 0.0208(2) Uani 1 1 d .
H5A H -0.4877 -0.1944 0.2559 0.025 Uiso 1 1 calc R
C6 C -0.0426(2) 0.05609(18) 0.30749(12) 0.0171(2) Uani 1 1 d .
C7 C 0.0886(2) -0.01849(18) 0.43614(12) 0.0175(2) Uani 1 1 d .
H4B H 0.375(4) -0.214(3) -0.131(2) 0.035(6) Uiso 1 1 d .
H4C H 0.492(5) -0.219(4) -0.027(3) 0.050(7) Uiso 1 1 d .
H7B H 0.226(4) 0.046(3) 0.437(2) 0.027(5) Uiso 1 1 d .
H7A H 0.163(4) -0.155(3) 0.426(2) 0.025(5) Uiso 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'
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
O2 Mn1 O2 180.00(6) 2 .
O2 Mn1 O4 91.17(4) 2 2
O2 Mn1 O4 88.83(4) . 2
O2 Mn1 O4 88.83(4) 2 .
O2 Mn1 O4 91.17(4) . .
O4 Mn1 O4 180.00(7) 2 .
O2 Mn1 O1 91.50(4) 2 2
O2 Mn1 O1 88.50(4) . 2
O4 Mn1 O1 87.11(4) 2 2
O4 Mn1 O1 92.89(4) . 2
O2 Mn1 O1 88.50(4) 2 .
O2 Mn1 O1 91.50(4) . .
O4 Mn1 O1 92.89(4) 2 .
O4 Mn1 O1 87.11(4) . .
O1 Mn1 O1 180.0 2 .
N1 O1 Mn1 115.05(7) . .
C6 O2 Mn1 131.41(8) . .
Mn1 O4 H4B 102.7(17) . .
Mn1 O4 H4C 123(2) . .
H4B O4 H4C 109(2) . .
O1 N1 C5 119.73(11) . .
O1 N1 C1 119.17(11) . .
C5 N1 C1 121.05(11) . .
N1 C1 C2 120.37(12) . .
N1 C1 H1A 119.8 . .
C2 C1 H1A 119.8 . .
C1 C2 C3 120.70(12) . .
C1 C2 H2A 119.7 . .
C3 C2 H2A 119.7 . .
C2 C3 C4 116.76(11) . .
C2 C3 C3 121.85(13) . 2_546
C4 C3 C3 121.37(14) . 2_546
C5 C4 C3 120.96(12) . .
C5 C4 H4A 119.5 . .
C3 C4 H4A 119.5 . .
N1 C5 C4 119.98(12) . .
N1 C5 H5A 120.0 . .
C4 C5 H5A 120.0 . .
O3 C6 O2 125.40(11) . .
O3 C6 C7 120.11(11) . .
O2 C6 C7 114.48(11) . .
C7 C7 C6 114.80(13) 2_556 .
C7 C7 H7B 110.8(12) 2_556 .
C6 C7 H7B 104.7(12) . .
C7 C7 H7A 109.7(12) 2_556 .
C6 C7 H7A 105.9(12) . .
H7B C7 H7A 110.8(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 2.1088(9) 2
Mn1 O2 2.1088(9) .
Mn1 O4 2.1950(10) 2
Mn1 O4 2.1950(10) .
Mn1 O1 2.2321(10) 2
Mn1 O1 2.2321(10) .
O1 N1 1.3314(13) .
O2 C6 1.2724(15) .
O3 C6 1.2473(16) .
O4 H4B 0.79(2) .
O4 H4C 0.75(3) .
N1 C5 1.3493(17) .
N1 C1 1.3501(16) .
C1 C2 1.3771(17) .
C1 H1A 0.9400 .
C2 C3 1.4012(17) .
C2 H2A 0.9400 .
C3 C4 1.4003(17) .
C3 C3 1.477(2) 2_546
C4 C5 1.3807(17) .
C4 H4A 0.9400 .
C5 H5A 0.9400 .
C6 C7 1.5205(16) .
C7 C7 1.512(2) 2_556
C7 H7B 0.98(2) .
C7 H7A 0.97(2) .
