#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/06/2230628.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2230628
loop_
_publ_author_name
'Xu, Wei'
_publ_section_title
;
 catena-Poly[[[aqua(formato-κO)(1,10-phenanthroline-κ²N,N')manganese(II)]-μ-formato-κ²O:O']
 monohydrate]
;
_journal_coeditor_code           FJ2422
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m893
_journal_paper_doi               10.1107/S1600536811020575
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mn (H C O2)2 (C12 H8 N2) (H2 O)], H2 O'
_chemical_formula_moiety         'C14 H12 Mn N2 O5, H2 O'
_chemical_formula_sum            'C14 H14 Mn N2 O6'
_chemical_formula_weight         361.21
_chemical_name_systematic
;
catena-Poly[[[aqua(formato-κO)(1,10-phenanthroline-
κ²N,N')manganese(II)]-μ-formato-κ²O:O']
monohydrate]
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.260(4)
_cell_length_b                   12.161(2)
_cell_length_c                   6.5493(13)
_cell_measurement_reflns_used    8376
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      3.35
_cell_volume                     1534.0(5)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            11493
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.35
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.933
_refine_ls_abs_structure_details 'Flack (1983), 1165 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       0.0025(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2644
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0370
_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)+(0.0135P)²+2.7605P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                1921
_reflns_number_total             2644
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fj2422.cif
_cod_data_source_block           I
_cod_database_code               2230628
_cod_database_fobs_code          2230628
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'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.57992(4) 0.37155(6) 0.67916(16) 0.0454(3) Uani d . 1 1 . .
N N1 0.6768(3) 0.3026(4) 0.5202(9) 0.0525(13) Uani d . 1 1 . .
N N2 0.6704(2) 0.4167(4) 0.8785(8) 0.0470(12) Uani d . 1 1 . .
C C1 0.6796(4) 0.2444(5) 0.3480(10) 0.068(2) Uani d . 1 1 . .
H H1A 0.6385 0.2277 0.2802 0.082 Uiso calc R 1 1 . .
C C2 0.7429(5) 0.2076(6) 0.2658(13) 0.087(3) Uani d . 1 1 . .
H H2A 0.7435 0.1662 0.1464 0.105 Uiso calc R 1 1 . .
C C3 0.8034(5) 0.2333(7) 0.3629(15) 0.091(3) Uani d . 1 1 . .
H H3A 0.8455 0.2099 0.3084 0.110 Uiso calc R 1 1 . .
C C4 0.8027(4) 0.2946(6) 0.5440(13) 0.073(2) Uani d . 1 1 . .
C C5 0.8643(4) 0.3266(7) 0.6559(18) 0.093(3) Uani d . 1 1 . .
H H5A 0.9077 0.3074 0.6049 0.112 Uiso calc R 1 1 . .
C C6 0.8603(4) 0.3828(8) 0.8299(16) 0.096(3) Uani d . 1 1 . .
H H6A 0.9010 0.4006 0.8988 0.116 Uiso calc R 1 1 . .
C C7 0.7958(3) 0.4161(6) 0.9127(12) 0.067(2) Uani d . 1 1 . .
C C8 0.7882(4) 0.4722(7) 1.0989(12) 0.079(3) Uani d . 1 1 . .
H H8A 0.8274 0.4906 1.1742 0.095 Uiso calc R 1 1 . .
C C9 0.7246(4) 0.4999(5) 1.1701(14) 0.0725(19) Uani d . 1 1 . .
H H9A 0.7197 0.5372 1.2932 0.087 Uiso calc R 1 1 . .
C C10 0.6668(4) 0.4714(5) 1.0556(11) 0.0600(17) Uani d . 1 1 . .
H H10A 0.6233 0.4913 1.1043 0.072 Uiso calc R 1 1 . .
C C11 0.7335(3) 0.3880(5) 0.8082(10) 0.0513(16) Uani d . 1 1 . .
C C12 0.7379(3) 0.3280(5) 0.6200(10) 0.0553(19) Uani d . 1 1 . .
C C13 0.5493(3) 0.5910(5) 0.4494(9) 0.0508(15) Uani d . 1 1 . .
H H13 0.5562 0.6662 0.4325 0.061 Uiso calc R 1 1 . .
O O1 0.5939(2) 0.5392(3) 0.5480(7) 0.0537(11) Uani d . 1 1 . .
O O2 0.4966(2) 0.5501(3) 0.3718(7) 0.0599(12) Uani d . 1 1 . .
C C14 0.5604(4) 0.1288(6) 0.7827(12) 0.071(2) Uani d . 1 1 . .
H H14 0.5642 0.1173 0.6428 0.086 Uiso calc R 1 1 . .
O O3 0.5629(3) 0.2210(4) 0.8388(7) 0.0747(14) Uani d . 1 1 . .
O O4 0.5534(4) 0.0457(4) 0.8904(10) 0.112(2) Uani d . 1 1 . .
O O5 0.5090(2) 0.3307(3) 0.4372(7) 0.0719(14) Uani d . 1 1 . .
H H5B 0.4990 0.3890 0.3784 0.108 Uiso d R 1 1 . .
H H5C 0.5014 0.2710 0.3749 0.108 Uiso d R 1 1 . .
O O6 0.4906(3) 0.1479(4) 0.2384(9) 0.115(2) Uani d . 1 1 . .
H H6B 0.4780 0.0927 0.3042 0.173 Uiso d R 1 1 . .
H H6C 0.5237 0.1210 0.1706 0.173 Uiso d R 1 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Mn1 O5 . . 93.75(19) ?
O3 Mn1 O2 . 2_665 89.28(17) ?
O5 Mn1 O2 . 2_665 95.71(18) ?
O3 Mn1 O1 . . 172.92(19) ?
O5 Mn1 O1 . . 90.21(16) ?
O2 Mn1 O1 2_665 . 84.49(17) ?
O3 Mn1 N2 . . 92.55(19) ?
O5 Mn1 N2 . . 167.9(2) ?
O2 Mn1 N2 2_665 . 94.70(18) ?
O1 Mn1 N2 . . 84.64(16) ?
O3 Mn1 N1 . . 91.92(18) ?
O5 Mn1 N1 . . 95.6(2) ?
O2 Mn1 N1 2_665 . 168.5(2) ?
O1 Mn1 N1 . . 93.53(17) ?
N2 Mn1 N1 . . 73.86(18) ?
C1 N1 C12 . . 119.0(6) ?
C1 N1 Mn1 . . 127.6(5) ?
C12 N1 Mn1 . . 113.4(4) ?
C10 N2 C11 . . 118.2(6) ?
C10 N2 Mn1 . . 125.8(4) ?
C11 N2 Mn1 . . 116.0(4) ?
N1 C1 C2 . . 121.9(8) ?
N1 C1 H1A . . 119.1 ?
C2 C1 H1A . . 119.1 ?
C3 C2 C1 . . 119.3(8) ?
C3 C2 H2A . . 120.3 ?
C1 C2 H2A . . 120.3 ?
C2 C3 C4 . . 120.5(8) ?
C2 C3 H3A . . 119.7 ?
C4 C3 H3A . . 119.7 ?
C3 C4 C12 . . 117.6(8) ?
C3 C4 C5 . . 124.3(8) ?
C12 C4 C5 . . 118.1(8) ?
C6 C5 C4 . . 121.6(8) ?
C6 C5 H5A . . 119.2 ?
C4 C5 H5A . . 119.2 ?
C5 C6 C7 . . 121.8(9) ?
C5 C6 H6A . . 119.1 ?
C7 C6 H6A . . 119.1 ?
C8 C7 C6 . . 124.3(8) ?
C8 C7 C11 . . 116.5(7) ?
C6 C7 C11 . . 119.1(8) ?
C9 C8 C7 . . 121.0(7) ?
C9 C8 H8A . . 119.5 ?
C7 C8 H8A . . 119.5 ?
C8 C9 C10 . . 118.6(8) ?
C8 C9 H9A . . 120.7 ?
C10 C9 H9A . . 120.7 ?
N2 C10 C9 . . 123.5(7) ?
N2 C10 H10A . . 118.3 ?
C9 C10 H10A . . 118.3 ?
N2 C11 C7 . . 122.3(7) ?
N2 C11 C12 . . 118.6(6) ?
C7 C11 C12 . . 119.0(6) ?
N1 C12 C4 . . 121.7(7) ?
N1 C12 C11 . . 118.0(6) ?
C4 C12 C11 . . 120.3(7) ?
O2 C13 O1 . . 125.0(6) ?
O2 C13 H13 . . 117.5 ?
O1 C13 H13 . . 117.5 ?
C13 O1 Mn1 . . 125.5(4) ?
C13 O2 Mn1 . 2_664 128.4(4) ?
O3 C14 O4 . . 127.0(8) ?
O3 C14 H14 . . 116.5 ?
O4 C14 H14 . . 116.5 ?
C14 O3 Mn1 . . 131.9(5) ?
Mn1 O5 H5B . . 107.1 ?
Mn1 O5 H5C . . 131.6 ?
H5B O5 H5C . . 118.0 ?
H6B O6 H6C . . 100.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O3 . 2.134(5) ?
Mn1 O5 . 2.150(4) ?
Mn1 O2 2_665 2.161(4) ?
Mn1 O1 . 2.228(4) ?
Mn1 N2 . 2.246(5) ?
Mn1 N1 . 2.295(5) ?
N1 C1 . 1.333(8) ?
N1 C12 . 1.382(8) ?
N2 C10 . 1.339(9) ?
N2 C11 . 1.346(7) ?
C1 C2 . 1.406(10) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.364(11) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.401(12) ?
C3 H3A . 0.9300 ?
C4 C12 . 1.403(9) ?
C4 C5 . 1.448(12) ?
C5 C6 . 1.331(13) ?
C5 H5A . 0.9300 ?
C6 C7 . 1.414(11) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.405(11) ?
C7 C11 . 1.422(9) ?
C8 C9 . 1.353(10) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.385(9) ?
C9 H9A . 0.9300 ?
C10 H10A . 0.9300 ?
C11 C12 . 1.435(9) ?
C13 O2 . 1.240(7) ?
C13 O1 . 1.245(7) ?
C13 H13 . 0.9300 ?
O2 Mn1 2_664 2.161(4) ?
C14 O3 . 1.180(8) ?
C14 O4 . 1.240(8) ?
C14 H14 . 0.9300 ?
O5 H5B . 0.8290 ?
O5 H5C . 0.8460 ?
O6 H6B . 0.8339 ?
O6 H6C . 0.8420 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O5 H5B O2 . . 1_555 0.83 1.96 2.713(5) 150 y
O5 H5C O6 . . 1_555 0.85 1.76 2.601(6) 177 y
O6 H6B O4 . . 2_654 0.83 1.88 2.693(8) 166 y
O6 H6C O4 . . 1_554 0.83 2.13 2.864(9) 145 y
