#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/77/1517784.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_1517784
loop_
_publ_author_name
'Hui-Fen Qian'
'Yuan Liu'
'Tao Tao'
'Ke-Hua Gu'
'Gui Yin'
'Wei Huang'
_publ_section_title
;
 Four sodium tetrafluoroborate directed supramolecular networks having 3-
 and 3,8-disubstituted 1,10-phenanthroline ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              1
_journal_page_last               8
_journal_volume                  405
_journal_year                    2013
_chemical_formula_moiety         'C16 H10 N2 Na S, B F4'
_chemical_formula_sum            'C16 H10 B F4 N2 Na S'
_chemical_formula_weight         372.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7705(16)
_cell_length_b                   11.815(2)
_cell_length_c                   17.437(4)
_cell_measurement_reflns_used    3903
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1829
_cell_volume                     1562.4(6)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2001)'
_computing_data_collection
'CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation & Rigaku Corporation, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (BRUKER 2000)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku Mercury CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1114
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13096
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.9701
_exptl_absorpt_correction_T_min  0.9563
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(REQAB, Jacobson, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         2716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0980
_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)+(0.0275P)²+10.6952P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2095
_refine_ls_wR_factor_ref         0.2188
_reflns_number_gt                2393
_reflns_number_total             2716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-405-1-8-4.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1517784
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
Na1 Na 0.8027(7) 0.0872(5) 0.0673(3) 0.1094(16) Uani 1 1 d .
B1 B 0.7392(11) -0.1249(6) -0.0973(4) 0.0361(17) Uani 1 1 d .
C1 C 0.8943(8) 0.4308(5) 0.0964(4) 0.0325(14) Uani 1 1 d .
H1 H 0.9691 0.4032 0.1431 0.039 Uiso 1 1 calc R
C2 C 0.8940(8) 0.5491(5) 0.0823(3) 0.0297(14) Uani 1 1 d .
C3 C 0.7917(8) 0.5870(5) 0.0131(3) 0.0300(14) Uani 1 1 d .
H3 H 0.7900 0.6654 0.0007 0.036 Uiso 1 1 calc R
C4 C 0.6900(7) 0.5115(5) -0.0394(3) 0.0269(13) Uani 1 1 d .
C5 C 0.5795(9) 0.5469(6) -0.1136(4) 0.0393(16) Uani 1 1 d .
H5 H 0.5760 0.6246 -0.1279 0.047 Uiso 1 1 calc R
C6 C 0.4829(9) 0.4726(6) -0.1619(4) 0.0433(18) Uani 1 1 d .
H6 H 0.4133 0.4976 -0.2107 0.052 Uiso 1 1 calc R
C7 C 0.4826(8) 0.3547(6) -0.1412(4) 0.0349(15) Uani 1 1 d .
C8 C 0.3788(9) 0.2725(6) -0.1892(4) 0.0406(17) Uani 1 1 d .
H8 H 0.3055 0.2944 -0.2379 0.049 Uiso 1 1 calc R
C9 C 0.3833(9) 0.1628(6) -0.1662(4) 0.0444(18) Uani 1 1 d .
H9 H 0.3132 0.1079 -0.1986 0.053 Uiso 1 1 calc R
C10 C 0.4894(9) 0.1312(6) -0.0960(4) 0.0460(18) Uani 1 1 d .
H10 H 0.4921 0.0543 -0.0799 0.055 Uiso 1 1 calc R
C11 C 0.5887(8) 0.3192(5) -0.0702(4) 0.0313(14) Uani 1 1 d .
C12 C 0.6958(7) 0.3969(5) -0.0182(4) 0.0284(13) Uani 1 1 d .
C13 C 0.9994(8) 0.6264(5) 0.1397(4) 0.0282(14) Uani 1 1 d .
C14 C 1.0339(7) 0.7455(5) 0.1266(4) 0.0293(14) Uani 1 1 d .
H14 H 0.9955 0.7865 0.0790 0.035 Uiso 1 1 calc R
C15 C 1.1364(9) 0.7889(6) 0.1988(4) 0.0419(17) Uani 1 1 d .
H15 H 1.1753 0.8654 0.2039 0.050 Uiso 1 1 calc R
C16 C 1.1750(9) 0.7147(6) 0.2596(4) 0.0403(16) Uani 1 1 d .
H16 H 1.2416 0.7335 0.3105 0.048 Uiso 1 1 calc R
N1 N 0.7981(6) 0.3562(4) 0.0491(3) 0.0308(12) Uani 1 1 d .
N2 N 0.5895(7) 0.2077(5) -0.0497(3) 0.0369(13) Uani 1 1 d .
S1 S 1.0901(3) 0.58457(16) 0.23398(11) 0.0468(6) Uani 1 1 d .
F2 F 0.8460(6) -0.2079(4) -0.1197(2) 0.0537(12) Uani 1 1 d .
F1 F 0.777(2) -0.1131(7) -0.0195(4) 0.097(5) Uani 0.84(3) 1 d P
F4 F 0.7529(12) -0.0306(5) -0.1369(5) 0.136(4) Uani 1 1 d .
F3 F 0.586(4) -0.1573(18) -0.089(3) 0.116(11) Uani 0.50(6) 1 d P
F1' F 0.851(4) -0.065(8) -0.048(4) 0.10(4) Uani 0.16(3) 1 d P
F3' F 0.5779(19) -0.154(3) -0.127(2) 0.121(10) Uani 0.50(6) 1 d P
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N2 Na1 F1' 87(2) . .
N2 Na1 F1 94.4(3) . .
F1' Na1 F1 20.8(19) . .
N2 Na1 F1' 114(2) . 3_755
F1' Na1 F1' 64.4(13) . 3_755
F1 Na1 F1' 79.3(14) . 3_755
N2 Na1 S1 138.0(2) . 2_745
F1' Na1 S1 134(2) . 2_745
F1 Na1 S1 121.3(2) . 2_745
F1' Na1 S1 95.5(15) 3_755 2_745
F3 B1 F1' 126(4) . .
F1' B1 F3' 150(2) . .
F3 B1 F4 119.3(14) . .
F1' B1 F4 77(5) . .
F3' B1 F4 101(2) . .
F3 B1 F1 85(2) . .
F1' B1 F1 45(4) . .
F3' B1 F1 115(2) . .
F4 B1 F1 114.7(8) . .
F3 B1 F2 116.4(13) . .
F1' B1 F2 102(2) . .
F3' B1 F2 106.5(10) . .
F4 B1 F2 108.9(6) . .
F1 B1 F2 110.4(8) . .
N1 C1 C2 124.7(6) . .
N1 C1 H1 117.6 . .
C2 C1 H1 117.6 . .
C3 C2 C1 117.0(6) . .
C3 C2 C13 121.9(6) . .
C1 C2 C13 121.1(6) . .
C2 C3 C4 120.5(6) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C3 C4 C12 117.6(5) . .
C3 C4 C5 122.8(6) . .
C12 C4 C5 119.6(6) . .
C6 C5 C4 121.1(6) . .
C6 C5 H5 119.4 . .
C4 C5 H5 119.4 . .
C5 C6 C7 120.7(6) . .
C5 C6 H6 119.6 . .
C7 C6 H6 119.6 . .
C11 C7 C8 118.0(6) . .
C11 C7 C6 118.8(6) . .
C8 C7 C6 123.2(6) . .
C9 C8 C7 120.5(7) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C9 C10 119.8(7) . .
C8 C9 H9 120.1 . .
C10 C9 H9 120.1 . .
N2 C10 C9 120.7(7) . .
N2 C10 H10 119.6 . .
C9 C10 H10 119.6 . .
N2 C11 C7 119.4(6) . .
N2 C11 C12 119.1(6) . .
C7 C11 C12 121.5(6) . .
N1 C12 C4 123.4(6) . .
N1 C12 C11 118.4(5) . .
C4 C12 C11 118.2(6) . .
C14 C13 C2 126.0(6) . .
C14 C13 S1 112.1(4) . .
C2 C13 S1 121.8(4) . .
C15 C14 C13 107.1(6) . .
C15 C14 H14 126.5 . .
C13 C14 H14 126.5 . .
C16 C15 C14 116.2(6) . .
C16 C15 H15 121.9 . .
C14 C15 H15 121.9 . .
C15 C16 S1 111.9(5) . .
C15 C16 H16 124.1 . .
S1 C16 H16 124.1 . .
C1 N1 C12 116.7(5) . .
C10 N2 C11 121.6(6) . .
C10 N2 Na1 106.0(5) . .
C11 N2 Na1 131.8(4) . .
C16 S1 C13 92.7(3) . .
C16 S1 Na1 74.1(3) . 2_755
C13 S1 Na1 159.7(2) . 2_755
B1 F1 F3 46.4(11) . .
B1 F1 Na1 127.9(5) . .
F3 F1 Na1 124.8(10) . .
B1 F4 F1' 51(3) . .
B1 F3 F1 48.4(14) . .
B1 F1' F4 52(2) . .
B1 F1' Na1 131(2) . .
F4 F1' Na1 115(4) . .
B1 F1' Na1 113(2) . 3_755
F4 F1' Na1 100(3) . 3_755
Na1 F1' Na1 115.6(13) . 3_755
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na1 N2 2.732(8) .
Na1 F1' 2.781(9) .
Na1 F1 2.792(9) .
Na1 F1' 2.80(4) 3_755
Na1 S1 3.383(5) 2_745
B1 F3 1.29(2) .
B1 F1' 1.29(3) .
B1 F3' 1.295(14) .
B1 F4 1.328(9) .
B1 F1 1.331(8) .
B1 F2 1.394(8) .
C1 N1 1.321(8) .
C1 C2 1.418(9) .
C1 H1 0.9500 .
C2 C3 1.368(8) .
C2 C13 1.466(9) .
C3 C4 1.395(9) .
C3 H3 0.9500 .
C4 C12 1.402(9) .
C4 C5 1.449(9) .
C5 C6 1.331(10) .
C5 H5 0.9500 .
C6 C7 1.439(10) .
C6 H6 0.9500 .
C7 C11 1.393(9) .
C7 C8 1.414(9) .
C8 C9 1.356(10) .
C8 H8 0.9500 .
C9 C10 1.371(10) .
C9 H9 0.9500 .
C10 N2 1.341(9) .
C10 H10 0.9500 .
C11 N2 1.365(8) .
C11 C12 1.425(9) .
C12 N1 1.354(8) .
C13 C14 1.460(9) .
C13 S1 1.714(6) .
C14 C15 1.431(9) .
C14 H14 0.9500 .
C15 C16 1.359(10) .
C15 H15 0.9500 .
C16 S1 1.694(7) .
C16 H16 0.9500 .
S1 Na1 3.383(5) 2_755
F1 F3 1.77(4) .
F4 F1' 1.63(9) .
F1' Na1 2.80(4) 3_755
