#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/77/1517782.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_1517782
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         'C12 H7 Br N2 Na, B F4'
_chemical_formula_sum            'C12 H7 B Br F4 N2 Na'
_chemical_formula_weight         368.91
_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                 108.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.1267(14)
_cell_length_b                   22.640(5)
_cell_length_c                   17.917(4)
_cell_measurement_reflns_used    9432
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0088
_cell_volume                     2743.2(11)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1185
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23246
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.065
_exptl_absorpt_correction_T_max  0.7392
_exptl_absorpt_correction_T_min  0.6836
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(REQAB, Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.004
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0794
_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)+(0.0366P)²+21.0546P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                4413
_reflns_number_total             4799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-405-1-8-2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2743.3(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1517782
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
B1 B 0.2023(14) 0.4279(4) -0.0949(5) 0.0375(19) Uani 1 1 d .
B2 B 0.3191(14) 0.1649(4) 0.0838(5) 0.041(2) Uani 1 1 d .
Br1 Br 0.80950(10) 0.19775(3) 0.39820(4) 0.0361(2) Uani 1 1 d .
Br2 Br 1.26963(11) 0.53346(3) 0.39517(5) 0.0399(2) Uani 1 1 d .
C1 C 0.6052(9) 0.2750(3) 0.2750(4) 0.0251(13) Uani 1 1 d .
H1 H 0.5634 0.2390 0.2476 0.030 Uiso 1 1 calc R
C2 C 0.7340(8) 0.2725(3) 0.3529(4) 0.0245(13) Uani 1 1 d .
C3 C 0.7981(8) 0.3234(3) 0.3947(4) 0.0260(14) Uani 1 1 d .
H3 H 0.8847 0.3220 0.4472 0.031 Uiso 1 1 calc R
C4 C 0.7326(8) 0.3774(3) 0.3577(4) 0.0235(13) Uani 1 1 d .
C5 C 0.7875(9) 0.4335(3) 0.3966(4) 0.0283(14) Uani 1 1 d .
H5 H 0.8730 0.4345 0.4494 0.034 Uiso 1 1 calc R
C6 C 0.7191(9) 0.4849(3) 0.3590(4) 0.0307(15) Uani 1 1 d .
H6 H 0.7596 0.5214 0.3853 0.037 Uiso 1 1 calc R
C7 C 0.5856(9) 0.4848(3) 0.2796(4) 0.0261(14) Uani 1 1 d .
C8 C 0.5059(10) 0.5367(3) 0.2386(5) 0.0380(17) Uani 1 1 d .
H8 H 0.5435 0.5742 0.2625 0.046 Uiso 1 1 calc R
C9 C 0.3728(11) 0.5329(3) 0.1636(5) 0.0371(17) Uani 1 1 d .
H9 H 0.3156 0.5678 0.1363 0.044 Uiso 1 1 calc R
C10 C 0.3233(10) 0.4788(3) 0.1283(4) 0.0339(16) Uani 1 1 d .
H10 H 0.2335 0.4764 0.0764 0.041 Uiso 1 1 calc R
C11 C 0.5313(8) 0.4306(3) 0.2415(4) 0.0238(13) Uani 1 1 d .
C12 C 0.6026(8) 0.3762(3) 0.2792(3) 0.0204(12) Uani 1 1 d .
C13 C 1.0661(10) 0.4595(3) 0.2666(4) 0.0289(14) Uani 1 1 d .
H13 H 1.0170 0.4960 0.2420 0.035 Uiso 1 1 calc R
C14 C 1.1980(9) 0.4602(3) 0.3437(4) 0.0303(15) Uani 1 1 d .
C15 C 1.2708(9) 0.4081(3) 0.3821(4) 0.0297(15) Uani 1 1 d .
H15 H 1.3582 0.4081 0.4346 0.036 Uiso 1 1 calc R
C16 C 1.2114(8) 0.3552(3) 0.3409(4) 0.0262(14) Uani 1 1 d .
C17 C 1.2780(10) 0.2982(3) 0.3764(5) 0.0389(17) Uani 1 1 d .
H17 H 1.3650 0.2962 0.4289 0.047 Uiso 1 1 calc R
C18 C 1.2163(11) 0.2476(4) 0.3350(5) 0.0409(18) Uani 1 1 d .
H18 H 1.2636 0.2105 0.3581 0.049 Uiso 1 1 calc R
C19 C 1.0814(9) 0.2498(3) 0.2571(4) 0.0291(15) Uani 1 1 d .
C20 C 1.0102(11) 0.1985(3) 0.2149(5) 0.0416(19) Uani 1 1 d .
H20 H 1.0561 0.1610 0.2367 0.050 Uiso 1 1 calc R
C21 C 0.8728(13) 0.2027(4) 0.1413(5) 0.048(2) Uani 1 1 d .
H21 H 0.8204 0.1678 0.1128 0.058 Uiso 1 1 calc R
C22 C 0.8108(10) 0.2572(3) 0.1086(4) 0.0373(17) Uani 1 1 d .
H22 H 0.7176 0.2597 0.0574 0.045 Uiso 1 1 calc R
C23 C 1.0158(9) 0.3046(3) 0.2230(4) 0.0257(14) Uani 1 1 d .
C24 C 1.0806(9) 0.3585(3) 0.2645(4) 0.0247(13) Uani 1 1 d .
F1 F 0.2518(12) 0.2207(2) 0.0614(4) 0.091(2) Uani 1 1 d .
F2 F 0.3886(8) 0.1607(2) 0.1641(3) 0.0557(13) Uani 1 1 d .
F3 F 0.1651(7) 0.1252(3) 0.0538(3) 0.0631(14) Uani 1 1 d .
F4 F 0.4690(7) 0.1499(2) 0.0524(3) 0.0610(14) Uani 1 1 d .
F5 F 0.0636(6) 0.4215(2) -0.0534(3) 0.0477(11) Uani 1 1 d .
F6 F 0.3464(7) 0.3851(2) -0.0675(3) 0.0621(14) Uani 1 1 d .
F7 F 0.2784(9) 0.4828(2) -0.0836(4) 0.0807(19) Uani 1 1 d .
F8 F 0.1048(8) 0.4180(2) -0.1732(3) 0.0596(14) Uani 1 1 d .
N1 N 0.5403(7) 0.3249(2) 0.2387(3) 0.0212(11) Uani 1 1 d .
N2 N 0.4007(7) 0.4293(2) 0.1667(3) 0.0269(12) Uani 1 1 d .
N3 N 1.0079(8) 0.4101(2) 0.2272(3) 0.0273(12) Uani 1 1 d .
N4 N 0.8805(8) 0.3064(2) 0.1483(3) 0.0294(12) Uani 1 1 d .
Na1 Na 0.2131(9) 0.3410(2) 0.0750(3) 0.1075(18) Uani 1 1 d .
Na2 Na 0.7068(9) 0.3955(3) 0.0520(4) 0.124(2) Uani 1 1 d .
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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'
H H 0.0000 0.0000 '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
F7 B1 F8 110.7(7) . .
F7 B1 F6 112.0(8) . .
F8 B1 F6 109.2(6) . .
F7 B1 F5 109.2(7) . .
F8 B1 F5 107.9(7) . .
F6 B1 F5 107.7(6) . .
F1 B2 F2 110.4(7) . .
F1 B2 F3 108.9(7) . .
F2 B2 F3 110.0(7) . .
F1 B2 F4 110.5(8) . .
F2 B2 F4 109.7(7) . .
F3 B2 F4 107.3(7) . .
N1 C1 C2 122.9(6) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C3 C2 C1 120.5(6) . .
C3 C2 Br1 121.4(5) . .
C1 C2 Br1 118.2(5) . .
C2 C3 C4 118.2(6) . .
C2 C3 H3 120.9 . .
C4 C3 H3 120.9 . .
C3 C4 C12 117.9(6) . .
C3 C4 C5 122.8(6) . .
C12 C4 C5 119.2(6) . .
C6 C5 C4 121.1(6) . .
C6 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
C5 C6 C7 120.7(6) . .
C5 C6 H6 119.6 . .
C7 C6 H6 119.6 . .
C11 C7 C8 118.3(6) . .
C11 C7 C6 118.6(6) . .
C8 C7 C6 123.1(6) . .
C9 C8 C7 119.7(7) . .
C9 C8 H8 120.1 . .
C7 C8 H8 120.1 . .
C10 C9 C8 120.1(7) . .
C10 C9 H9 120.0 . .
C8 C9 H9 120.0 . .
N2 C10 C9 120.4(7) . .
N2 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
N2 C11 C7 119.6(6) . .
N2 C11 C12 118.6(6) . .
C7 C11 C12 121.7(6) . .
N1 C12 C11 118.4(5) . .
N1 C12 C4 122.9(5) . .
C11 C12 C4 118.6(5) . .
N3 C13 C14 122.4(6) . .
N3 C13 H13 118.8 . .
C14 C13 H13 118.8 . .
C15 C14 C13 120.6(6) . .
C15 C14 Br2 120.4(5) . .
C13 C14 Br2 119.0(5) . .
C14 C15 C16 117.6(6) . .
C14 C15 H15 121.2 . .
C16 C15 H15 121.2 . .
C24 C16 C15 118.0(6) . .
C24 C16 C17 120.2(6) . .
C15 C16 C17 121.7(6) . .
C18 C17 C16 120.3(7) . .
C18 C17 H17 119.8 . .
C16 C17 H17 119.8 . .
C17 C18 C19 120.4(7) . .
C17 C18 H18 119.8 . .
C19 C18 H18 119.8 . .
C20 C19 C23 119.2(7) . .
C20 C19 C18 121.4(7) . .
C23 C19 C18 119.4(7) . .
C21 C20 C19 119.4(7) . .
C21 C20 H20 120.3 . .
C19 C20 H20 120.3 . .
C20 C21 C22 120.3(7) . .
C20 C21 H21 119.9 . .
C22 C21 H21 119.9 . .
N4 C22 C21 120.5(7) . .
N4 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
N4 C23 C19 119.1(6) . .
N4 C23 C24 119.4(6) . .
C19 C23 C24 121.4(6) . .
N3 C24 C16 124.0(6) . .
N3 C24 C23 117.8(6) . .
C16 C24 C23 118.2(6) . .
B2 F1 Na1 157.5(6) . .
B1 F5 Na1 110.0(4) . .
B1 F6 Na2 127.9(5) . .
B1 F7 Na2 157.6(6) . 3_665
C1 N1 C12 117.6(5) . .
C10 N2 C11 121.9(6) . .
C10 N2 Na1 105.5(4) . .
C11 N2 Na1 132.3(4) . .
C13 N3 C24 117.3(6) . .
C22 N4 C23 121.5(6) . .
C22 N4 Na2 105.4(5) . .
C23 N4 Na2 133.1(4) . .
N2 Na1 F1 138.7(3) . .
N2 Na1 F5 90.3(2) . .
F1 Na1 F5 125.4(3) . .
N2 Na1 Na2 95.7(2) . 1_455
F1 Na1 Na2 116.1(3) . 1_455
F5 Na1 Na2 66.22(18) . 1_455
N2 Na1 Na2 61.98(19) . .
F1 Na1 Na2 100.7(3) . .
F5 Na1 Na2 80.32(19) . .
Na2 Na1 Na2 140.0(2) 1_455 .
N4 Na2 F6 123.7(3) . .
N4 Na2 F7 128.8(3) . 3_665
F6 Na2 F7 101.8(3) . 3_665
N4 Na2 Na1 56.27(18) . 1_655
F6 Na2 Na1 133.2(3) . 1_655
F7 Na2 Na1 109.3(2) 3_665 1_655
N4 Na2 Na1 86.7(2) . .
F6 Na2 Na1 53.58(19) . .
F7 Na2 Na1 105.6(2) 3_665 .
Na1 Na2 Na1 140.0(2) 1_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
B1 F7 1.347(10) .
B1 F8 1.374(9) .
B1 F6 1.385(10) .
B1 F5 1.419(10) .
B2 F1 1.367(10) .
B2 F2 1.369(10) .
B2 F3 1.389(10) .
B2 F4 1.397(11) .
Br1 C2 1.881(6) .
Br2 C14 1.887(7) .
C1 N1 1.313(8) .
C1 C2 1.409(9) .
C1 H1 0.9500 .
C2 C3 1.372(9) .
C3 C4 1.398(9) .
C3 H3 0.9500 .
C4 C12 1.420(9) .
C4 C5 1.443(9) .
C5 C6 1.355(10) .
C5 H5 0.9500 .
C6 C7 1.441(10) .
C6 H6 0.9500 .
C7 C11 1.399(9) .
C7 C8 1.408(9) .
C8 C9 1.382(11) .
C8 H8 0.9500 .
C9 C10 1.373(10) .
C9 H9 0.9500 .
C10 N2 1.338(8) .
C10 H10 0.9500 .
C11 N2 1.370(8) .
C11 C12 1.419(9) .
C12 N1 1.366(8) .
C13 N3 1.319(9) .
C13 C14 1.404(10) .
C13 H13 0.9500 .
C14 C15 1.383(10) .
C15 C16 1.400(10) .
C15 H15 0.9500 .
C16 C24 1.394(9) .
C16 C17 1.452(10) .
C17 C18 1.361(11) .
C17 H17 0.9500 .
C18 C19 1.424(10) .
C18 H18 0.9500 .
C19 C20 1.392(10) .
C19 C23 1.395(9) .
C20 C21 1.376(12) .
C20 H20 0.9500 .
C21 C22 1.378(11) .
C21 H21 0.9500 .
C22 N4 1.330(9) .
C22 H22 0.9500 .
C23 N4 1.380(9) .
C23 C24 1.428(9) .
C24 N3 1.364(8) .
F1 Na1 2.755(8) .
F5 Na1 2.865(7) .
F6 Na2 2.787(8) .
F7 Na2 2.807(8) 3_665
N2 Na1 2.664(8) .
N4 Na2 2.690(8) .
Na1 Na2 3.712(9) 1_455
Na1 Na2 3.871(9) .
Na2 F7 2.807(8) 3_665
Na2 Na1 3.712(9) 1_655
