#------------------------------------------------------------------------------
#$Date: 2016-02-14 05:40:26 +0100 (Sun 14 de Feb de 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/74/2227424.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_2227424
loop_
_publ_author_name
'Watton, Stephen P.'
_publ_section_title
;
 Acetonitrilebis(2-methyl-1,10-phenanthroline)copper(II)
 tetrafluoridoborate
;
_journal_coeditor_code           FJ2341
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1359
_journal_paper_doi               10.1107/S1600536810038845
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cu (C2 H3 N) (C13 H10 N2)2] (B F4)2'
_chemical_formula_moiety         'C28 H23 Cu N5 2+, 2(B F4 -)'
_chemical_formula_sum            'C28 H23 B2 Cu F8 N5'
_chemical_formula_weight         666.67
_chemical_melting_point          573
_chemical_name_systematic
;
Acetonitrilebis(2-methyl-1,10-phenanthroline)copper(II) tetrafluoridoborate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 131.824(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.0665(11)
_cell_length_b                   8.81200(10)
_cell_length_c                   16.8419(14)
_cell_measurement_reflns_used    18534
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.572
_cell_measurement_theta_min      3.770
_cell_volume                     2772.2(4)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Oxford Diffraction Sapphire 3 CCD'
_diffrn_measurement_method       '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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30296
_diffrn_reflns_theta_full        34.67
_diffrn_reflns_theta_max         34.67
_diffrn_reflns_theta_min         4.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Crysalis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.811
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         5578
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0396
_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)+(0.0639P)²+2.7650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                4442
_reflns_number_total             5578
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fj2341.cif
_cod_data_source_block           I
_cod_original_cell_volume        2772.2(3)
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2227424
_cod_database_fobs_code          2227424
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'
'-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_disorder_assembly
_atom_site_disorder_group
C C1 0.13529(8) 1.05662(18) 0.79172(12) 0.0273(3) Uani d . 1 . .
C C2 0.17740(9) 1.0448(2) 0.76412(15) 0.0338(3) Uani d . 1 . .
H H2 0.2207 1.0967 0.8041 0.041 Uiso calc R 1 . .
C C3 0.15571(9) 0.9591(2) 0.68020(15) 0.0338(3) Uani d . 1 . .
H H3 0.1844 0.9503 0.6638 0.041 Uiso calc R 1 . .
C C4 0.08932(8) 0.88348(17) 0.61807(13) 0.0268(3) Uani d . 1 . .
C C5 0.06222(10) 0.7871(2) 0.52973(15) 0.0335(3) Uani d . 1 . .
H H5 0.0894 0.7721 0.5111 0.040 Uiso calc R 1 . .
C C6 -0.00201(10) 0.7173(2) 0.47264(14) 0.0325(3) Uani d . 1 . .
H H6 -0.0181 0.6543 0.4162 0.039 Uiso calc R 1 . .
C C7 -0.04559(8) 0.73991(17) 0.49864(12) 0.0257(3) Uani d . 1 . .
C C8 -0.11375(9) 0.6737(2) 0.44131(13) 0.0332(3) Uani d . 1 . .
H H8 -0.1322 0.6085 0.3847 0.040 Uiso calc R 1 . .
C C9 -0.15234(9) 0.7061(2) 0.46972(14) 0.0340(3) Uani d . 1 . .
H H9 -0.1975 0.6637 0.4322 0.041 Uiso calc R 1 . .
C C10 -0.12360(8) 0.80361(17) 0.55573(12) 0.0267(3) Uani d . 1 . .
H H10 -0.1506 0.8253 0.5740 0.032 Uiso calc R 1 . .
C C11 -0.02038(7) 0.83494(15) 0.58437(10) 0.0198(2) Uani d . 1 . .
C C12 0.04852(7) 0.90451(15) 0.64633(11) 0.0205(2) Uani d . 1 . .
C C13 0.16252(10) 1.1435(2) 0.88823(14) 0.0377(4) Uani d . 1 . .
H H13A 0.1605 1.2502 0.8748 0.057 Uiso calc R 1 . .
H H13B 0.2112 1.1148 0.9471 0.057 Uiso calc R 1 . .
H H13C 0.1335 1.1217 0.9050 0.057 Uiso calc R 1 . .
C C14 0.0000 1.3587(2) 0.7500 0.0282(4) Uani d S 1 . .
C C15 0.0000 1.5232(3) 0.7500 0.0525(9) Uani d S 1 . .
H H15A -0.0443 1.5595 0.7279 0.079 Uiso calc PR 0.50 . .
H H15B 0.0051 1.5595 0.7016 0.079 Uiso calc PR 0.50 . .
H H15C 0.0392 1.5595 0.8205 0.079 Uiso calc PR 0.50 . .
Cu Cu1 0.0000 0.99458(2) 0.7500 0.01924(7) Uani d S 1 . .
N N1 0.07141(6) 0.98891(12) 0.73210(10) 0.0208(2) Uani d . 1 . .
N N2 -0.05911(6) 0.86627(13) 0.61224(9) 0.0207(2) Uani d . 1 . .
N N3 0.0000 1.2302(2) 0.7500 0.0303(4) Uani d S 1 . .
B B1 0.18636(13) 0.4493(3) 0.30558(19) 0.0314(4) Uani d PD 0.810(3) A 1
F F1 0.19869(8) 0.38867(18) 0.24324(13) 0.0455(4) Uani d PD 0.810(3) A 1
F F2 0.1938(6) 0.3381(6) 0.3661(9) 0.1162(15) Uani d PD 0.810(3) A 1
F F3 0.2324(2) 0.5670(4) 0.3570(3) 0.0722(10) Uani d PD 0.810(3) A 1
F F4 0.1172(3) 0.5089(5) 0.2417(3) 0.0696(13) Uani d P 0.810(3) A 1
B B1B 0.1736(6) 0.4482(13) 0.3248(8) 0.0314(4) Uani d PD 0.190(3) A 2
F F1B 0.1694(4) 0.4945(7) 0.4000(6) 0.0455(4) Uani d PD 0.190(3) A 2
F F2B 0.193(3) 0.306(3) 0.363(4) 0.1162(15) Uani d PD 0.190(3) A 2
F F3B 0.2359(10) 0.532(2) 0.3811(16) 0.0722(10) Uani d PD 0.190(3) A 2
F F4B 0.1126(13) 0.463(3) 0.2259(18) 0.0696(13) Uani d P 0.190(3) A 2
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'
Cu Cu 0.3201 1.2651 '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 C1 C2 . . 120.27(15) ?
N1 C1 C13 . . 119.85(14) ?
C2 C1 C13 . . 119.87(14) ?
C3 C2 C1 . . 121.05(15) ?
C3 C2 H2 . . 119.5 ?
C1 C2 H2 . . 119.5 ?
C2 C3 C4 . . 119.43(15) ?
C2 C3 H3 . . 120.3 ?
C4 C3 H3 . . 120.3 ?
C12 C4 C3 . . 117.02(15) ?
C12 C4 C5 . . 118.98(14) ?
C3 C4 C5 . . 124.00(14) ?
C6 C5 C4 . . 121.56(14) ?
C6 C5 H5 . . 119.2 ?
C4 C5 H5 . . 119.2 ?
C5 C6 C7 . . 120.47(15) ?
C5 C6 H6 . . 119.8 ?
C7 C6 H6 . . 119.8 ?
C11 C7 C8 . . 117.39(13) ?
C11 C7 C6 . . 118.96(14) ?
C8 C7 C6 . . 123.65(14) ?
C9 C8 C7 . . 119.42(14) ?
C9 C8 H8 . . 120.3 ?
C7 C8 H8 . . 120.3 ?
C8 C9 C10 . . 119.64(15) ?
C8 C9 H9 . . 120.2 ?
C10 C9 H9 . . 120.2 ?
N2 C10 C9 . . 122.38(14) ?
N2 C10 H10 . . 118.8 ?
C9 C10 H10 . . 118.8 ?
N2 C11 C7 . . 122.78(13) ?
N2 C11 C12 . . 117.02(12) ?
C7 C11 C12 . . 120.20(12) ?
N1 C12 C4 . . 123.06(13) ?
N1 C12 C11 . . 117.17(11) ?
C4 C12 C11 . . 119.77(13) ?
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 ?
N3 C14 C15 . . 180.000(3) ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C14 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
N1 Cu1 N1 2_556 . 177.15(6) ?
N1 Cu1 N2 2_556 . 96.41(5) ?
N1 Cu1 N2 . . 82.02(5) ?
N1 Cu1 N2 2_556 2_556 82.02(5) ?
N1 Cu1 N2 . 2_556 96.41(5) ?
N2 Cu1 N2 . 2_556 113.67(7) ?
N1 Cu1 N3 2_556 . 91.43(3) ?
N1 Cu1 N3 . . 91.43(3) ?
N2 Cu1 N3 . . 123.16(3) ?
N2 Cu1 N3 2_556 . 123.16(3) ?
C1 N1 C12 . . 119.08(13) ?
C1 N1 Cu1 . . 128.24(11) ?
C12 N1 Cu1 . . 112.67(9) ?
C10 N2 C11 . . 118.39(12) ?
C10 N2 Cu1 . . 130.48(10) ?
C11 N2 Cu1 . . 110.88(9) ?
C14 N3 Cu1 . . 180.0000(10) ?
F2 B1 F3 . . 116.7(6) ?
F2 B1 F1 . . 107.9(5) ?
F3 B1 F1 . . 104.8(2) ?
F2 B1 F4 . . 109.5(5) ?
F3 B1 F4 . . 107.2(3) ?
F1 B1 F4 . . 110.5(2) ?
F4B B1B F2B . . 116(3) ?
F4B B1B F3B . . 130.2(18) ?
F2B B1B F3B . . 107(2) ?
F4B B1B F1B . . 113.1(12) ?
F2B B1B F1B . . 94(2) ?
F3B B1B F1B . . 87.4(9) ?
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
C1 N1 . 1.3356(18) ?
C1 C2 . 1.413(2) ?
C1 C13 . 1.488(2) ?
C2 C3 . 1.356(3) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.409(2) ?
C3 H3 . 0.9300 ?
C4 C12 . 1.3985(19) ?
C4 C5 . 1.431(2) ?
C5 C6 . 1.353(3) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.436(2) ?
C6 H6 . 0.9300 ?
C7 C11 . 1.4030(19) ?
C7 C8 . 1.411(2) ?
C8 C9 . 1.365(3) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.401(2) ?
C9 H9 . 0.9300 ?
C10 N2 . 1.3312(18) ?
C10 H10 . 0.9300 ?
C11 N2 . 1.3589(17) ?
C11 C12 . 1.4297(18) ?
C12 N1 . 1.3652(18) ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
C14 N3 . 1.133(3) ?
C14 C15 . 1.449(3) ?
C15 H15A . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15C . 0.9600 ?
Cu1 N1 2_556 2.0042(12) ?
Cu1 N1 . 2.0043(12) ?
Cu1 N2 . 2.0669(12) ?
Cu1 N2 2_556 2.0669(12) ?
Cu1 N3 . 2.0759(19) ?
B1 F2 . 1.334(6) ?
B1 F3 . 1.351(4) ?
B1 F1 . 1.384(3) ?
B1 F4 . 1.397(5) ?
B1B F4B . 1.32(3) ?
B1B F2B . 1.344(16) ?
B1B F3B . 1.381(15) ?
B1B F1B . 1.399(11) ?
