#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/05/7050554.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_7050554
loop_
_publ_author_name
'Ma, Chengbing'
'Chen, Changneng'
'Liu, Qiutian'
'Liao, Daizheng'
'Li, Licun'
'Sun, Licheng'
_publ_section_title
;
 Structural transformation mediated by o-, m-, and p-phthalates from
 two to three dimensions for manganese/phthalate/4,4'-bpy complexes
 (4,4'-bpy = 4,4'-bipyridine)
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              890
_journal_paper_doi               10.1039/b301076g
_journal_volume                  27
_journal_year                    2003
_chemical_formula_moiety         'C18.50 H15 Mn N2 O5'
_chemical_formula_sum            'C18.5 H15 Mn N2 O5'
_chemical_formula_weight         400.26
_chemical_melting_point          ?
_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                 102.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.116(2)
_cell_length_b                   11.562(2)
_cell_length_c                   16.084(3)
_cell_measurement_reflns_used    4121
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.80
_cell_volume                     1833.1(6)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8646
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  .6883
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             820
_exptl_crystal_size_max          .27
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .10
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_gt           0.0631
_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)+(0.1155P)²+1.1859P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.1960
_reflns_number_gt                2799
_reflns_number_total             3990
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301076g.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        1833.0(6)
_cod_original_sg_symbol_H-M      P2/c
_cod_original_formula_sum        'C18.50 H15 Mn N2 O5'
_cod_database_code               7050554
#BEGIN Tags that were not found in dictionaries:
_refine_ls_r_factor_ref          0.0887
#END Tags that were not found in dictionaries
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
Mn Mn 0.38064(5) 0.72302(5) 0.83376(3) 0.0353(2) Uani 1 1 d . . .
O1 O 0.5794(3) 0.7181(2) 0.91545(18) 0.0448(6) Uani 1 1 d . . .
O2 O 0.6580(3) 0.7274(3) 0.80010(18) 0.0513(7) Uani 1 1 d . . .
O3 O 1.2931(3) 0.7094(3) 0.9537(2) 0.0653(10) Uani 1 1 d . . .
O4 O 1.1587(3) 0.7189(3) 0.82807(18) 0.0528(8) Uani 1 1 d . . .
O5 O 0.0000 0.5154(12) 0.7500 0.134(4) Uani 0.63 2 d SP . .
O6 O 0.0000 -0.0789(18) 0.7500 0.196(7) Uani 0.63 2 d SP . .
O7 O 0.0000 0.177(3) 0.7500 0.155(15) Uani 0.25 2 d SP . .
O8 O 1.133(4) 0.992(3) 1.023(3) 0.229(17) Uiso 0.25 1 d P . .
N1 N 0.3875(3) 0.5275(3) 0.8260(2) 0.0433(7) Uani 1 1 d . . .
N2 N 0.3849(3) -0.0840(3) 0.8334(2) 0.0477(8) Uani 1 1 d . . .
C1 C 0.4766(4) 0.4655(4) 0.8831(3) 0.0510(10) Uani 1 1 d . . .
H1A H 0.5418 0.5053 0.9228 0.061 Uiso 1 1 calc R . .
C2 C 0.4775(4) 0.3490(4) 0.8866(3) 0.0506(10) Uani 1 1 d . . .
H2A H 0.5414 0.3108 0.9281 0.061 Uiso 1 1 calc R . .
C3 C 0.3836(4) 0.2866(3) 0.8283(2) 0.0409(8) Uani 1 1 d . . .
C4 C 0.2910(5) 0.3492(4) 0.7689(3) 0.0632(13) Uani 1 1 d . . .
H4A H 0.2254 0.3114 0.7283 0.076 Uiso 1 1 calc R . .
C5 C 0.2969(5) 0.4666(4) 0.7707(3) 0.0660(14) Uani 1 1 d . . .
H5A H 0.2333 0.5070 0.7304 0.079 Uiso 1 1 calc R . .
C6 C 0.3834(4) 0.1595(3) 0.8307(2) 0.0427(8) Uani 1 1 d . . .
C7 C 0.4757(8) 0.1005(5) 0.8841(5) 0.140(4) Uani 1 1 d . . .
H7A H 0.5433 0.1395 0.9226 0.168 Uiso 1 1 calc R . .
C8 C 0.4738(8) -0.0192(5) 0.8840(5) 0.123(4) Uani 1 1 d . . .
H8A H 0.5418 -0.0566 0.9233 0.148 Uiso 1 1 calc R . .
C9 C 0.2986(8) -0.0235(5) 0.7815(6) 0.143(4) Uani 1 1 d . . .
H9A H 0.2336 -0.0636 0.7419 0.171 Uiso 1 1 calc R . .
C10 C 0.2921(8) 0.0948(5) 0.7782(6) 0.144(4) Uani 1 1 d . . .
H10A H 0.2228 0.1305 0.7388 0.173 Uiso 1 1 calc R . .
C11 C 0.8157(3) 0.6933(3) 0.9302(2) 0.0362(8) Uani 1 1 d . . .
C12 C 0.8346(4) 0.6592(5) 1.0145(3) 0.0556(11) Uani 1 1 d . . .
H12A H 0.7598 0.6501 1.0385 0.067 Uiso 1 1 calc R . .
C13 C 0.9622(4) 0.6389(5) 1.0630(3) 0.0679(15) Uani 1 1 d . . .
H13A H 0.9739 0.6139 1.1191 0.081 Uiso 1 1 calc R . .
C14 C 1.0739(4) 0.6558(5) 1.0277(3) 0.0616(13) Uani 1 1 d . . .
H14A H 1.1609 0.6443 1.0608 0.074 Uiso 1 1 calc R . .
C15 C 1.0565(4) 0.6892(4) 0.9446(2) 0.0433(9) Uani 1 1 d . . .
C16 C 0.9264(3) 0.7053(3) 0.8952(2) 0.0375(8) Uani 1 1 d . . .
H16A H 0.9144 0.7244 0.8378 0.045 Uiso 1 1 calc R . .
C17 C 0.6743(3) 0.7141(3) 0.8778(2) 0.0346(7) Uani 1 1 d . . .
C18 C 1.1773(4) 0.7067(3) 0.9066(3) 0.0440(9) Uani 1 1 d . . .
C19 C 1.030(3) 0.954(3) 1.119(3) 0.139(16) Uani 0.25 1 d P . .
C20 C 1.0000 1.0000 1.0000 0.101(8) Uani 0.50 2 d SP . .
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 Mn O1 124.22(11) 2_656 . ?
O2 Mn O4 90.26(12) 2_656 1_455 ?
O1 Mn O4 145.46(11) . 1_455 ?
O2 Mn N2 88.43(12) 2_656 1_565 ?
O1 Mn N2 90.68(11) . 1_565 ?
O4 Mn N2 92.35(12) 1_455 1_565 ?
O2 Mn N1 88.20(12) 2_656 . ?
O1 Mn N1 88.36(11) . . ?
O4 Mn N1 91.12(12) 1_455 . ?
N2 Mn N1 175.17(12) 1_565 . ?
O2 Mn O3 147.43(11) 2_656 1_455 ?
O1 Mn O3 88.22(10) . 1_455 ?
O4 Mn O3 57.25(10) 1_455 1_455 ?
N2 Mn O3 94.68(13) 1_565 1_455 ?
N1 Mn O3 90.02(13) . 1_455 ?
O2 Mn C18 118.75(12) 2_656 1_455 ?
O1 Mn C18 116.86(12) . 1_455 ?
O4 Mn C18 28.61(11) 1_455 1_455 ?
N2 Mn C18 95.25(12) 1_565 1_455 ?
N1 Mn C18 89.40(12) . 1_455 ?
O3 Mn C18 28.69(11) 1_455 1_455 ?
C17 O1 Mn 115.0(2) . . ?
C17 O2 Mn 171.0(3) . 2_656 ?
C18 O3 Mn 88.7(3) . 1_655 ?
C18 O4 Mn 92.3(2) . 1_655 ?
C5 N1 C1 115.6(4) . . ?
C5 N1 Mn 122.8(3) . . ?
C1 N1 Mn 121.3(3) . . ?
C9 N2 C8 111.6(5) . . ?
C9 N2 Mn 122.7(3) . 1_545 ?
C8 N2 Mn 125.7(3) . 1_545 ?
N1 C1 C2 124.0(4) . . ?
C1 C2 C3 119.9(4) . . ?
C2 C3 C4 116.8(3) . . ?
C2 C3 C6 120.7(3) . . ?
C4 C3 C6 122.5(3) . . ?
C5 C4 C3 119.3(4) . . ?
N1 C5 C4 124.4(4) . . ?
C7 C6 C10 114.4(5) . . ?
C7 C6 C3 122.2(4) . . ?
C10 C6 C3 123.4(4) . . ?
C6 C7 C8 120.9(5) . . ?
N2 C8 C7 125.6(5) . . ?
N2 C9 C10 126.4(5) . . ?
C6 C10 C9 121.1(5) . . ?
C16 C11 C12 119.1(3) . . ?
C16 C11 C17 121.0(3) . . ?
C12 C11 C17 119.9(3) . . ?
C13 C12 C11 120.8(4) . . ?
C12 C13 C14 119.5(4) . . ?
C15 C14 C13 120.2(4) . . ?
C14 C15 C16 119.7(4) . . ?
C14 C15 C18 120.1(3) . . ?
C16 C15 C18 120.2(4) . . ?
C11 C16 C15 120.5(3) . . ?
O2 C17 O1 123.1(3) . . ?
O2 C17 C11 118.7(3) . . ?
O1 C17 C11 118.2(3) . . ?
O4 C18 O3 121.6(4) . . ?
O4 C18 C15 118.6(3) . . ?
O3 C18 C15 119.8(4) . . ?
O4 C18 Mn 59.1(2) . 1_655 ?
O3 C18 Mn 62.6(2) . 1_655 ?
C15 C18 Mn 175.6(3) . 1_655 ?
O8 C20 C19 77(2) . . ?
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
Mn O2 2.101(3) 2_656 ?
Mn O1 2.142(3) . ?
Mn O4 2.227(3) 1_455 ?
Mn N2 2.232(4) 1_565 ?
Mn N1 2.266(3) . ?
Mn O3 2.302(3) 1_455 ?
Mn C18 2.592(4) 1_455 ?
O1 C17 1.245(4) . ?
O2 C17 1.234(5) . ?
O2 Mn 2.101(3) 2_656 ?
O3 C18 1.245(5) . ?
O3 Mn 2.302(3) 1_655 ?
O4 C18 1.242(5) . ?
O4 Mn 2.227(3) 1_655 ?
O8 C20 1.325(4) . ?
N1 C5 1.326(5) . ?
N1 C1 1.342(5) . ?
N2 C9 1.273(6) . ?
N2 C8 1.304(6) . ?
N2 Mn 2.232(4) 1_545 ?
C1 C2 1.348(6) . ?
C2 C3 1.379(5) . ?
C3 C4 1.383(5) . ?
C3 C6 1.469(6) . ?
C4 C5 1.359(6) . ?
C6 C7 1.309(6) . ?
C6 C10 1.332(6) . ?
C7 C8 1.384(8) . ?
C9 C10 1.370(8) . ?
C11 C16 1.369(5) . ?
C11 C12 1.382(6) . ?
C11 C17 1.507(4) . ?
C12 C13 1.371(6) . ?
C13 C14 1.387(6) . ?
C14 C15 1.364(6) . ?
C15 C16 1.389(5) . ?
C15 C18 1.498(5) . ?
C18 Mn 2.592(4) 1_655 ?
C19 C20 1.497(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Mn O1 C17 -2.3(3) 2_656 . . . ?
O4 Mn O1 C17 174.0(2) 1_455 . . . ?
N2 Mn O1 C17 -90.8(3) 1_565 . . . ?
N1 Mn O1 C17 84.4(3) . . . . ?
O3 Mn O1 C17 174.5(3) 1_455 . . . ?
C18 Mn O1 C17 172.9(2) 1_455 . . . ?
O2 Mn N1 C5 -44.5(4) 2_656 . . . ?
O1 Mn N1 C5 -168.8(4) . . . . ?
O4 Mn N1 C5 45.7(4) 1_455 . . . ?
N2 Mn N1 C5 -90.3(13) 1_565 . . . ?
O3 Mn N1 C5 102.9(4) 1_455 . . . ?
C18 Mn N1 C5 74.3(4) 1_455 . . . ?
O2 Mn N1 C1 142.0(3) 2_656 . . . ?
O1 Mn N1 C1 17.7(3) . . . . ?
O4 Mn N1 C1 -127.8(3) 1_455 . . . ?
N2 Mn N1 C1 96.3(13) 1_565 . . . ?
O3 Mn N1 C1 -70.5(3) 1_455 . . . ?
C18 Mn N1 C1 -99.2(3) 1_455 . . . ?
C5 N1 C1 C2 -0.2(7) . . . . ?
Mn N1 C1 C2 173.7(4) . . . . ?
N1 C1 C2 C3 0.7(7) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
C1 C2 C3 C6 179.6(4) . . . . ?
C2 C3 C4 C5 0.1(8) . . . . ?
C6 C3 C4 C5 179.8(5) . . . . ?
C1 N1 C5 C4 -0.4(8) . . . . ?
Mn N1 C5 C4 -174.2(5) . . . . ?
C3 C4 C5 N1 0.5(9) . . . . ?
C2 C3 C6 C7 -4.0(8) . . . . ?
C4 C3 C6 C7 176.3(7) . . . . ?
C2 C3 C6 C10 177.4(7) . . . . ?
C4 C3 C6 C10 -2.4(8) . . . . ?
C10 C6 C7 C8 -0.4(13) . . . . ?
C3 C6 C7 C8 -179.1(8) . . . . ?
C9 N2 C8 C7 1.2(14) . . . . ?
Mn N2 C8 C7 -179.5(8) 1_545 . . . ?
C6 C7 C8 N2 0.0(17) . . . . ?
C8 N2 C9 C10 -2.2(15) . . . . ?
Mn N2 C9 C10 178.4(9) 1_545 . . . ?
C7 C6 C10 C9 -0.6(14) . . . . ?
C3 C6 C10 C9 178.2(9) . . . . ?
N2 C9 C10 C6 2.1(19) . . . . ?
C16 C11 C12 C13 0.7(7) . . . . ?
C17 C11 C12 C13 179.5(5) . . . . ?
C11 C12 C13 C14 1.8(9) . . . . ?
C12 C13 C14 C15 -1.9(9) . . . . ?
C13 C14 C15 C16 -0.6(8) . . . . ?
C13 C14 C15 C18 -179.7(5) . . . . ?
C12 C11 C16 C15 -3.2(6) . . . . ?
C17 C11 C16 C15 178.1(3) . . . . ?
C14 C15 C16 C11 3.1(6) . . . . ?
C18 C15 C16 C11 -177.8(4) . . . . ?
Mn O2 C17 O1 -78.4(17) 2_656 . . . ?
Mn O2 C17 C11 102.2(16) 2_656 . . . ?
Mn O1 C17 O2 9.3(5) . . . . ?
Mn O1 C17 C11 -171.4(2) . . . . ?
C16 C11 C17 O2 9.4(5) . . . . ?
C12 C11 C17 O2 -169.3(4) . . . . ?
C16 C11 C17 O1 -170.0(3) . . . . ?
C12 C11 C17 O1 11.3(5) . . . . ?
Mn O4 C18 O3 4.8(4) 1_655 . . . ?
Mn O4 C18 C15 -175.6(3) 1_655 . . . ?
Mn O3 C18 O4 -4.6(4) 1_655 . . . ?
Mn O3 C18 C15 175.8(3) 1_655 . . . ?
C14 C15 C18 O4 168.6(4) . . . . ?
C16 C15 C18 O4 -10.4(6) . . . . ?
C14 C15 C18 O3 -11.7(7) . . . . ?
C16 C15 C18 O3 169.2(4) . . . . ?
C14 C15 C18 Mn 110(4) . . . 1_655 ?
C16 C15 C18 Mn -69(4) . . . 1_655 ?
