#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/81/2208186.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_2208186
loop_
_publ_author_name
'Hwang, In-Chul'
'Ha, Kwang'
_publ_section_title
;
 Tris(1,10-phenanthroline)manganese(II) bis(hexafluorophosphate)
;
_journal_coeditor_code           TK6305
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m376
_journal_page_last               m378
_journal_paper_doi               10.1107/S1600536806002753
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Mn (C12 H8 N2)3] (P F6)2'
_chemical_formula_moiety         'C36 H24 Mn N6 2+ , 2F6 P -'
_chemical_formula_sum            'C36 H24 F12 Mn N6 P2'
_chemical_formula_weight         885.49
_chemical_name_systematic
;
Tris(1,10-phenanthroline)manganese(II) bis(hexafluorophosphate)
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 94.2630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3133(7)
_cell_length_b                   15.2753(11)
_cell_length_c                   12.8037(9)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.1
_cell_volume                     1816.5(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker SMART 1000 area-detector CCD'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.063
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11432
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.131
_refine_ls_R_factor_gt           0.077
_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)+(0.0752P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.159
_refine_ls_wR_factor_ref         0.185
_reflns_number_gt                2469
_reflns_number_total             4178
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tk6305.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2208186
_cod_database_fobs_code          2208186
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_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
_atom_site_type_symbol
Mn 0.5 0.28106(5) 0.75 0.0493(3) Uani d S 1 . . Mn
N1 0.4343(4) 0.1887(2) 0.6194(3) 0.0621(9) Uani d . 1 . . N
N2 0.6928(4) 0.2693(2) 0.6553(3) 0.0565(9) Uani d . 1 . . N
N3 0.4178(3) 0.3978(2) 0.6578(2) 0.0491(8) Uani d . 1 . . N
C1 0.3053(6) 0.1523(3) 0.5998(4) 0.0783(14) Uani d . 1 . . C
H1 0.2357 0.1623 0.6468 0.094 Uiso calc R 1 . . H
C2 0.2691(7) 0.1001(4) 0.5130(5) 0.1014(19) Uani d . 1 . . C
H2 0.1778 0.0757 0.5021 0.122 Uiso calc R 1 . . H
C3 0.3715(8) 0.0860(4) 0.4447(4) 0.104(2) Uani d . 1 . . C
H3 0.3499 0.0511 0.3861 0.125 Uiso calc R 1 . . H
C4 0.5085(7) 0.1229(3) 0.4607(4) 0.0823(15) Uani d . 1 . . C
C5 0.6248(8) 0.1112(4) 0.3924(4) 0.104(2) Uani d . 1 . . C
H5 0.6105 0.0745 0.3346 0.124 Uiso calc R 1 . . H
C6 0.7511(8) 0.1512(4) 0.4096(4) 0.0977(19) Uani d . 1 . . C
H6 0.8221 0.1428 0.3632 0.117 Uiso calc R 1 . . H
C7 0.7790(6) 0.2066(3) 0.4974(4) 0.0733(14) Uani d . 1 . . C
C8 0.9080(6) 0.2547(4) 0.5175(5) 0.0855(16) Uani d . 1 . . C
H8 0.9822 0.2484 0.4733 0.103 Uiso calc R 1 . . H
C9 0.9244(5) 0.3096(4) 0.6003(4) 0.0873(17) Uani d . 1 . . C
H9 1.0067 0.3438 0.6116 0.105 Uiso calc R 1 . . H
C10 0.8147(5) 0.3134(3) 0.6681(4) 0.0726(13) Uani d . 1 . . C
H10 0.8282 0.3495 0.7266 0.087 Uiso calc R 1 . . H
C11 0.6731(5) 0.2168(3) 0.5691(3) 0.0569(10) Uani d . 1 . . C
C12 0.5359(5) 0.1748(3) 0.5502(3) 0.0609(11) Uani d . 1 . . C
C13 0.3401(4) 0.3996(3) 0.5659(3) 0.0688(12) Uani d . 1 . . C
H13 0.3136 0.3465 0.5347 0.083 Uiso calc R 1 . . H
C14 0.2969(5) 0.4754(4) 0.5147(4) 0.0834(16) Uani d . 1 . . C
H14 0.2421 0.4731 0.4510 0.100 Uiso calc R 1 . . H
C15 0.3354(6) 0.5530(4) 0.5584(5) 0.0881(17) Uani d . 1 . . C
H15 0.3066 0.6046 0.5246 0.106 Uiso calc R 1 . . H
C16 0.4181(5) 0.5567(3) 0.6540(4) 0.0664(12) Uani d . 1 . . C
C17 0.4611(6) 0.6353(3) 0.7044(5) 0.0927(19) Uani d . 1 . . C
H17 0.4345 0.6884 0.6732 0.111 Uiso calc R 1 . . H
C18 0.4578(4) 0.4761(3) 0.7015(3) 0.0497(10) Uani d . 1 . . C
P1 0 0.02571(12) 0.75 0.0774(6) Uani d S 1 . . P
F11 0.0006(4) 0.0267(3) 0.8722(3) 0.1401(14) Uani d . 1 . . F
F12 0.1697(3) 0.0246(2) 0.7557(3) 0.1216(13) Uani d . 1 . . F
F13 0 -0.0762(3) 0.75 0.187(3) Uani d S 1 . . F
F14 0 0.1280(3) 0.75 0.1140(16) Uani d S 1 . . F
P2 0 0.41737(17) 0.25 0.0933(7) Uani d S 1 . . P
F21 -0.1230(5) 0.4845(3) 0.2365(3) 0.1563(16) Uani d . 1 A . F
F22A 0.0112(16) 0.3973(13) 0.1415(13) 0.155(6) Uani d P 0.58(3) A 1 F
F23A 0.1090(14) 0.3396(8) 0.2287(17) 0.160(6) Uani d P 0.58(3) A 1 F
F22B 0.0128(16) 0.455(2) 0.1281(14) 0.167(9) Uani d P 0.42(3) A 2 F
F23B 0.1271(16) 0.3657(16) 0.299(3) 0.189(10) Uani d P 0.42(3) A 2 F
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'
F F 0.0171 0.0103 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
N1 Mn N1 2_656 . 101.85(18) yes
N1 Mn N3 2_656 2_656 92.56(12) ?
N1 Mn N3 . 2_656 163.43(12) yes
N1 Mn N3 2_656 . 163.43(12) ?
N1 Mn N3 . . 92.56(12) yes
N3 Mn N3 2_656 . 74.57(16) yes
N1 Mn N2 2_656 2_656 74.42(13) ?
N1 Mn N2 . 2_656 99.66(12) yes
N3 Mn N2 2_656 2_656 92.01(11) ?
N3 Mn N2 . 2_656 95.29(12) ?
N1 Mn N2 2_656 . 99.66(12) ?
N1 Mn N2 . . 74.42(13) yes
N3 Mn N2 2_656 . 95.29(12) ?
N3 Mn N2 . . 92.01(11) yes
N2 Mn N2 2_656 . 170.82(18) yes
C1 N1 C12 . . 118.3(4) ?
C1 N1 Mn . . 126.7(3) ?
C12 N1 Mn . . 114.8(3) ?
C10 N2 C11 . . 117.6(4) ?
C10 N2 Mn . . 127.3(3) ?
C11 N2 Mn . . 114.7(3) ?
C13 N3 C18 . . 117.3(4) ?
C13 N3 Mn . . 128.4(3) ?
C18 N3 Mn . . 114.2(2) ?
N1 C1 C2 . . 123.6(5) ?
N1 C1 H1 . . 118.2 ?
C2 C1 H1 . . 118.2 ?
C3 C2 C1 . . 117.8(5) ?
C3 C2 H2 . . 121.1 ?
C1 C2 H2 . . 121.1 ?
C2 C3 C4 . . 121.2(5) ?
C2 C3 H3 . . 119.4 ?
C4 C3 H3 . . 119.4 ?
C3 C4 C12 . . 117.2(5) ?
C3 C4 C5 . . 125.2(5) ?
C12 C4 C5 . . 117.6(5) ?
C6 C5 C4 . . 122.3(5) ?
C6 C5 H5 . . 118.9 ?
C4 C5 H5 . . 118.9 ?
C5 C6 C7 . . 121.0(5) ?
C5 C6 H6 . . 119.5 ?
C7 C6 H6 . . 119.5 ?
C11 C7 C8 . . 116.9(5) ?
C11 C7 C6 . . 119.3(5) ?
C8 C7 C6 . . 123.9(5) ?
C9 C8 C7 . . 120.6(5) ?
C9 C8 H8 . . 119.7 ?
C7 C8 H8 . . 119.7 ?
C8 C9 C10 . . 118.0(5) ?
C8 C9 H9 . . 121.0 ?
C10 C9 H9 . . 121.0 ?
N2 C10 C9 . . 124.5(5) ?
N2 C10 H10 . . 117.8 ?
C9 C10 H10 . . 117.8 ?
N2 C11 C7 . . 122.3(4) ?
N2 C11 C12 . . 117.6(4) ?
C7 C11 C12 . . 120.0(4) ?
N1 C12 C4 . . 121.8(4) ?
N1 C12 C11 . . 118.3(4) ?
C4 C12 C11 . . 119.8(4) ?
N3 C13 C14 . . 123.8(5) ?
N3 C13 H13 . . 118.1 ?
C14 C13 H13 . . 118.1 ?
C15 C14 C13 . . 118.9(5) ?
C15 C14 H14 . . 120.6 ?
C13 C14 H14 . . 120.6 ?
C14 C15 C16 . . 120.7(5) ?
C14 C15 H15 . . 119.6 ?
C16 C15 H15 . . 119.6 ?
C15 C16 C17 . . 123.8(5) ?
C15 C16 C18 . . 116.9(5) ?
C17 C16 C18 . . 119.3(4) ?
C17 C17 C16 2_656 . 121.4(3) ?
C17 C17 H17 2_656 . 119.3 ?
C16 C17 H17 . . 119.3 ?
N3 C18 C16 . . 122.3(4) ?
N3 C18 C18 . 2_656 118.5(2) ?
C16 C18 C18 . 2_656 119.2(3) ?
F13 P1 F14 . . 180.0000(10) ?
F13 P1 F11 . . 90.56(17) ?
F14 P1 F11 . . 89.44(17) ?
F13 P1 F11 . 2_556 90.56(17) ?
F14 P1 F11 . 2_556 89.44(17) ?
F11 P1 F11 . 2_556 178.9(3) ?
F13 P1 F12 . 2_556 89.37(15) ?
F14 P1 F12 . 2_556 90.63(15) ?
F11 P1 F12 . 2_556 88.61(19) ?
F11 P1 F12 2_556 2_556 91.41(19) ?
F13 P1 F12 . . 89.37(15) ?
F14 P1 F12 . . 90.63(15) ?
F11 P1 F12 . . 91.41(19) ?
F11 P1 F12 2_556 . 88.61(19) ?
F12 P1 F12 2_556 . 178.7(3) ?
F22A P2 F22A 2 . 155.3(18) ?
F22A P2 F23B 2 2 100.2(19) ?
F22A P2 F23B . 2 66.5(12) ?
F22A P2 F23B 2 . 66.5(12) ?
F22A P2 F23B . . 100.2(19) ?
F23B P2 F23B 2 . 117.3(19) ?
F22A P2 F21 2 2 98.1(9) ?
F22A P2 F21 . 2 98.3(6) ?
F23B P2 F21 2 2 160.9(14) ?
F23B P2 F21 . 2 75.5(9) ?
F22A P2 F21 2 . 98.3(6) ?
F22A P2 F21 . . 98.1(9) ?
F23B P2 F21 2 . 75.5(8) ?
F23B P2 F21 . . 160.9(14) ?
F21 P2 F21 2 . 96.4(4) ?
F22A P2 F23A 2 2 65.4(14) ?
F22A P2 F23A . 2 95.7(8) ?
F23B P2 F23A . 2 91.6(10) ?
F21 P2 F23A 2 2 162.4(8) ?
F21 P2 F23A . 2 92.2(6) ?
F22A P2 F23A 2 . 95.7(8) ?
F22A P2 F23A . . 65.4(14) ?
F23B P2 F23A 2 . 91.6(10) ?
F21 P2 F23A 2 . 92.2(6) ?
F21 P2 F23A . . 162.4(8) ?
F23A P2 F23A 2 . 84.0(10) ?
F22A P2 F22B . 2 172(2) ?
F23B P2 F22B 2 2 117.1(15) ?
F23B P2 F22B . 2 84.5(10) ?
F21 P2 F22B 2 2 76.6(9) ?
F21 P2 F22B . 2 76.7(10) ?
F23A P2 F22B 2 2 90.5(15) ?
F23A P2 F22B . 2 120.4(9) ?
F22A P2 F22B 2 . 172(2) ?
F23B P2 F22B 2 . 84.5(10) ?
F23B P2 F22B . . 117.1(15) ?
F21 P2 F22B 2 . 76.7(10) ?
F21 P2 F22B . . 76.6(9) ?
F23A P2 F22B 2 . 120.4(9) ?
F23A P2 F22B . . 90.5(15) ?
F22B P2 F22B 2 . 140(3) ?
P2 F22A F23A . . 62.2(12) ?
P2 F23A F22A . . 52.5(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
Mn N1 2_656 2.239(3) ?
Mn N1 . 2.239(3) yes
Mn N3 2_656 2.242(3) ?
Mn N3 . 2.242(3) yes
Mn N2 2_656 2.247(3) ?
Mn N2 . 2.247(3) yes
N1 C1 . 1.330(5) ?
N1 C12 . 1.360(5) ?
N2 C10 . 1.320(5) ?
N2 C11 . 1.366(5) ?
N3 C13 . 1.335(5) ?
N3 C18 . 1.361(5) ?
C1 C2 . 1.388(6) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.359(8) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.396(8) ?
C3 H3 . 0.9300 ?
C4 C12 . 1.401(6) ?
C4 C5 . 1.454(8) ?
C5 C6 . 1.328(8) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.416(7) ?
C6 H6 . 0.9300 ?
C7 C11 . 1.405(6) ?
C7 C8 . 1.415(7) ?
C8 C9 . 1.352(7) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.391(6) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.434(6) ?
C13 C14 . 1.376(7) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.347(7) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.398(7) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.408(6) ?
C16 C18 . 1.410(5) ?
C17 C17 2_656 1.327(10) ?
C17 H17 . 0.9300 ?
C18 C18 2_656 1.419(7) ?
P1 F13 . 1.556(5) ?
P1 F14 . 1.562(4) ?
P1 F11 . 1.564(3) ?
P1 F11 2_556 1.564(3) ?
P1 F12 2_556 1.577(3) ?
P1 F12 . 1.577(3) ?
P2 F22A 2 1.435(13) ?
P2 F22A . 1.435(13) ?
P2 F23B 2 1.518(16) ?
P2 F23B . 1.518(16) ?
P2 F21 2 1.537(4) ?
P2 F21 . 1.537(4) ?
P2 F23A 2 1.600(10) ?
P2 F23A . 1.600(10) ?
P2 F22B 2 1.677(13) ?
P2 F22B . 1.677(13) ?
F22A F23A . 1.64(3) ?
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_site_symmetry_1
_geom_torsion
N1 Mn N1 C1 2_656 86.2(4)
N3 Mn N1 C1 2_656 -123.9(5)
N3 Mn N1 C1 . -85.6(4)
N2 Mn N1 C1 2_656 10.2(4)
N1 Mn N1 C12 2_656 -98.9(3)
N3 Mn N1 C12 2_656 51.0(6)
N3 Mn N1 C12 . 89.4(3)
N3 Mn N2 C10 2_656 7.8(3)
N3 Mn N2 C10 . 82.4(3)
N3 Mn N2 C11 2_656 -165.1(3)
N3 Mn N2 C11 . -90.4(3)
N1 Mn N3 C13 . 8.7(4)
N2 Mn N3 C13 2_656 -91.3(3)
N2 Mn N3 C13 . 83.1(3)
N1 Mn N3 C18 2_656 40.4(6)
N1 Mn N3 C18 . -169.0(3)
N2 Mn N3 C18 2_656 91.0(3)
N2 Mn N3 C18 . -94.5(3)
