#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/43/2224359.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_2224359
loop_
_publ_author_name
'Wang, Xinfang'
_publ_section_title
;
 Dichlorido(2,9-dimethyl-1,10-phenanthroline)manganese(II) hemihydrate
;
_journal_coeditor_code           LH2953
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1659
_journal_paper_doi               10.1107/S1600536809049149
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Mn Cl2 (C14 H12 N2)], 0.5H2 O'
_chemical_formula_moiety         'C14 H12 Cl2 Mn N2, 0.5(H2 O)'
_chemical_formula_sum            'C14 H13 Cl2 Mn N2 O0.5'
_chemical_formula_weight         343.10
_chemical_name_systematic
;
Dichlorido(2,9-dimethyl-1,10-phenanthroline)manganese(II) hemihydrate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 101.532(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.763(4)
_cell_length_b                   7.7343(15)
_cell_length_c                   11.362(2)
_cell_measurement_reflns_used    1089
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.761
_cell_measurement_theta_min      2.876
_cell_volume                     1615.6(5)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008b)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008b)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω 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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4794
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.8127
_exptl_absorpt_correction_T_min  0.7191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008a)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0443
_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)+(0.1015P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                1199
_reflns_number_total             1511
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh2953.cif
_cod_data_source_block           I
_cod_original_cell_volume        1615.5(5)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C14 H13 Cl2 Mn N2 O0.50'
_cod_database_code               2224359
_cod_database_fobs_code          2224359
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.35177(3) 0.0000 0.27709(5) 0.0558(3) Uani d S 1 . .
Cl Cl1 0.40493(4) 0.25282(10) 0.24304(8) 0.0815(3) Uani d . 1 . .
O O1 0.5351(5) 1.0000 0.0528(9) 0.155(4) Uani d SP 0.50 . .
H H2A 0.5257 0.9426 0.1128 0.186 Uiso d PR 0.25 . .
H H1A 0.5745 0.9558 0.0399 0.186 Uiso d PR 0.25 . .
N N1 0.30817(15) 0.0000 0.4374(3) 0.0555(8) Uani d S 1 . .
N N2 0.24030(17) 0.0000 0.2034(3) 0.0601(8) Uani d S 1 . .
C C1 0.3433(2) 0.0000 0.5521(4) 0.0625(10) Uani d S 1 . .
C C2 0.3066(2) 0.0000 0.6486(4) 0.0715(12) Uani d S 1 . .
H H2 0.3329 0.0000 0.7272 0.086 Uiso calc SR 1 . .
C C3 0.2337(2) 0.0000 0.6273(4) 0.0715(12) Uani d S 1 . .
H H3 0.2089 0.0000 0.6905 0.086 Uiso calc SR 1 . .
C C4 0.1951(2) 0.0000 0.5056(3) 0.0604(10) Uani d S 1 . .
C C5 0.1191(2) 0.0000 0.4745(4) 0.0781(13) Uani d S 1 . .
H H5 0.0919 0.0000 0.5346 0.094 Uiso calc SR 1 . .
C C6 0.0848(2) 0.0000 0.3584(4) 0.0768(13) Uani d S 1 . .
H H6 0.0342 0.0000 0.3399 0.092 Uiso calc SR 1 . .
C C7 0.1240(2) 0.0000 0.2635(4) 0.0655(11) Uani d S 1 . .
C C8 0.0910(3) 0.0000 0.1374(4) 0.0840(15) Uani d S 1 . .
H H8 0.0406 0.0000 0.1136 0.101 Uiso calc SR 1 . .
C C9 0.1330(3) 0.0000 0.0535(4) 0.0875(15) Uani d S 1 . .
H H9 0.1113 0.0000 -0.0276 0.105 Uiso calc SR 1 . .
C C10 0.2073(3) 0.0000 0.0872(4) 0.0703(11) Uani d S 1 . .
C C11 0.1985(2) 0.0000 0.2896(3) 0.0562(9) Uani d S 1 . .
C C12 0.2350(2) 0.0000 0.4153(3) 0.0532(9) Uani d S 1 . .
C C13 0.4239(2) 0.0000 0.5734(4) 0.0819(14) Uani d S 1 . .
H H13A 0.4397 -0.0724 0.5150 0.123 Uiso calc PR 0.50 . .
H H13B 0.4431 -0.0434 0.6525 0.123 Uiso calc PR 0.50 . .
H H13C 0.4410 0.1158 0.5666 0.123 Uiso calc PR 0.50 . .
C C14 0.2542(3) 0.0000 -0.0069(4) 0.0933(17) Uani d S 1 . .
H H14A 0.2713 0.1152 -0.0163 0.140 Uiso calc PR 0.50 . .
H H14B 0.2260 -0.0395 -0.0820 0.140 Uiso calc PR 0.50 . .
H H14C 0.2950 -0.0756 0.0181 0.140 Uiso calc PR 0.50 . .
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'
Cl Cl 0.1484 0.1585 '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
N2 Mn1 N1 . . 79.57(12) ?
N2 Mn1 Cl1 . . 111.79(4) ?
N1 Mn1 Cl1 . . 113.70(4) ?
N2 Mn1 Cl1 . 6 111.79(4) ?
N1 Mn1 Cl1 . 6 113.70(4) ?
Cl1 Mn1 Cl1 . 6 119.53(5) ?
O1 O1 H2A 5_675 . 109.0 ?
O1 O1 H1A 5_675 . 119.0 ?
H2A O1 H1A . . 104.5 ?
C1 N1 C12 . . 117.9(3) ?
C1 N1 Mn1 . . 129.1(3) ?
C12 N1 Mn1 . . 113.0(2) ?
C10 N2 C11 . . 119.1(3) ?
C10 N2 Mn1 . . 128.4(3) ?
C11 N2 Mn1 . . 112.5(2) ?
N1 C1 C2 . . 122.5(3) ?
N1 C1 C13 . . 116.6(4) ?
C2 C1 C13 . . 121.0(4) ?
C3 C2 C1 . . 120.0(4) ?
C3 C2 H2 . . 120.0 ?
C1 C2 H2 . . 120.0 ?
C2 C3 C4 . . 118.5(4) ?
C2 C3 H3 . . 120.8 ?
C4 C3 H3 . . 120.8 ?
C12 C4 C5 . . 119.2(4) ?
C12 C4 C3 . . 118.2(4) ?
C5 C4 C3 . . 122.6(4) ?
C6 C5 C4 . . 120.7(4) ?
C6 C5 H5 . . 119.7 ?
C4 C5 H5 . . 119.7 ?
C5 C6 C7 . . 121.7(4) ?
C5 C6 H6 . . 119.2 ?
C7 C6 H6 . . 119.2 ?
C11 C7 C6 . . 119.7(4) ?
C11 C7 C8 . . 115.5(4) ?
C6 C7 C8 . . 124.8(4) ?
C9 C8 C7 . . 120.4(4) ?
C9 C8 H8 . . 119.8 ?
C7 C8 H8 . . 119.8 ?
C8 C9 C10 . . 120.4(4) ?
C8 C9 H9 . . 119.8 ?
C10 C9 H9 . . 119.8 ?
N2 C10 C9 . . 121.2(4) ?
N2 C10 C14 . . 118.4(4) ?
C9 C10 C14 . . 120.3(4) ?
C7 C11 N2 . . 123.3(3) ?
C7 C11 C12 . . 118.2(3) ?
N2 C11 C12 . . 118.5(3) ?
N1 C12 C4 . . 123.0(3) ?
N1 C12 C11 . . 116.5(3) ?
C4 C12 C11 . . 120.5(3) ?
C1 C13 H13A . . 109.5 ?
C1 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C1 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C10 C14 H14A . . 109.5 ?
C10 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C10 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
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 N2 . 2.092(3) ?
Mn1 N1 . 2.140(3) ?
Mn1 Cl1 . 2.2633(9) ?
Mn1 Cl1 6 2.2633(9) ?
O1 O1 5_675 1.59(2) ?
O1 H2A . 0.8610 ?
O1 H1A . 0.8530 ?
N1 C1 . 1.338(5) ?
N1 C12 . 1.345(5) ?
N2 C10 . 1.342(5) ?
N2 C11 . 1.371(5) ?
C1 C2 . 1.407(6) ?
C1 C13 . 1.482(6) ?
C2 C3 . 1.341(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.428(6) ?
C3 H3 . 0.9300 ?
C4 C12 . 1.387(5) ?
C4 C5 . 1.399(6) ?
C5 C6 . 1.347(6) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.421(6) ?
C6 H6 . 0.9300 ?
C7 C11 . 1.371(5) ?
C7 C8 . 1.443(6) ?
C8 C9 . 1.353(7) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.370(7) ?
C9 H9 . 0.9300 ?
C10 C14 . 1.514(7) ?
C11 C12 . 1.454(5) ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
