#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:18:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179747 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/43/7004358.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_7004358
loop_
_publ_author_name
'Dixon, Isabelle M.'
'Lebon, Emilie'
'Loustau, Gilles'
'Sutra, Pierre'
'Vendier, Laure'
'Igau, Alain'
'Juris, Alberto'
_publ_section_title
;
 Broad HOMO--LUMO gap tuning through the coordination of a single
 phosphine, aminophosphine or phosphite onto a Ru(tpy)(bpy)2+ core
;
_journal_issue                   41
_journal_name_full               'Dalton Transactions'
_journal_page_first              5627
_journal_page_last               5635
_journal_paper_doi               10.1039/b806325g
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H17 B1 N1 P'
_chemical_formula_sum            'C16 H17 B N P'
_chemical_formula_weight         265.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.182(15)
_cell_angle_beta                 99.474(16)
_cell_angle_gamma                103.301(18)
_cell_formula_units_Z            4
_cell_length_a                   9.503(2)
_cell_length_b                   10.494(2)
_cell_length_c                   15.347(3)
_cell_measurement_reflns_used    1329
_cell_measurement_temperature    150
_cell_measurement_theta_max      32.1287
_cell_measurement_theta_min      2.8078
_cell_measurement_wavelength     0.71073
_cell_volume                     1467.8(5)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       ω-φ
_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  0.075
_diffrn_reflns_av_unetI/netI     0.1415
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10776
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.2
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5575
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.1416
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0743P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                2608
_reflns_number_total             5575
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b806325g.txt
_cod_data_source_block           (1.BH3)
_cod_original_cell_volume        1467.7(5)
_cod_database_code               7004358
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1392(4) 0.0361(5) 0.3061(3) 0.0407(12) Uani 1 1 d . . .
H1 H 0.0616 0.0487 0.3324 0.049 Uiso 1 1 calc R . .
C2 C 0.1328(6) -0.0673(5) 0.2425(4) 0.085(2) Uani 1 1 d D . .
H2 H 0.0518 -0.1339 0.2197 0.102 Uiso 1 1 calc R . .
C3 C 0.2861(7) -0.0444(5) 0.2205(3) 0.0617(16) Uani 1 1 d D . .
H3 H 0.319 -0.0942 0.1815 0.074 Uiso 1 1 calc R . .
C4 C 0.3679(5) 0.0671(4) 0.2713(3) 0.0341(10) Uani 1 1 d . . .
H4 H 0.4667 0.1042 0.2712 0.041 Uiso 1 1 calc R . .
C5 C 0.5177(4) 0.2600(4) 0.4389(2) 0.0243(9) Uani 1 1 d . . .
C6 C 0.5410(5) 0.1722(4) 0.5039(3) 0.0353(11) Uani 1 1 d . . .
H6 H 0.4616 0.1145 0.5213 0.042 Uiso 1 1 calc R . .
C7 C 0.6820(5) 0.1705(5) 0.5428(3) 0.0405(11) Uani 1 1 d . . .
H7 H 0.6967 0.1112 0.5864 0.049 Uiso 1 1 calc R . .
C8 C 0.8001(5) 0.2541(5) 0.5186(3) 0.0476(13) Uani 1 1 d . . .
H8 H 0.8947 0.2507 0.5445 0.057 Uiso 1 1 calc R . .
C9 C 0.7789(5) 0.3409(5) 0.4573(3) 0.0454(12) Uani 1 1 d . . .
H9 H 0.8597 0.3994 0.4421 0.054 Uiso 1 1 calc R . .
C10 C 0.6391(4) 0.3457(4) 0.4159(3) 0.0339(10) Uani 1 1 d . . .
H10 H 0.6269 0.4063 0.3729 0.041 Uiso 1 1 calc R . .
C11 C 0.3428(4) 0.3864(4) 0.3136(2) 0.0230(9) Uani 1 1 d D . .
C12 C 0.3623(5) 0.5133(4) 0.3456(3) 0.0395(11) Uani 1 1 d . . .
H12 H 0.3694 0.5318 0.4057 0.047 Uiso 1 1 calc R . .
C13 C 0.3710(5) 0.6108(5) 0.2871(3) 0.0444(12) Uani 1 1 d . . .
H13 H 0.3871 0.6968 0.3086 0.053 Uiso 1 1 calc R . .
C14 C 0.3572(6) 0.5877(6) 0.2000(4) 0.0606(15) Uani 1 1 d . . .
H14 H 0.3601 0.6565 0.1618 0.073 Uiso 1 1 calc R . .
C15 C 0.3399(5) 0.4696(5) 0.1692(4) 0.0547(15) Uani 1 1 d . . .
H15 H 0.3315 0.4538 0.1087 0.066 Uiso 1 1 calc R . .
C16 C 0.3338(4) 0.3689(4) 0.2234(3) 0.0322(10) Uani 1 1 d D . .
H16 H 0.3233 0.285 0.1996 0.039 Uiso 1 1 calc R . .
C17 C 0.7313(5) 0.4673(4) 0.2003(3) 0.0365(11) Uani 1 1 d . . .
H17 H 0.6328 0.458 0.1764 0.044 Uiso 1 1 calc R . .
C18 C 0.8191(7) 0.5656(5) 0.2644(4) 0.0677(19) Uani 1 1 d . . .
H18 H 0.7886 0.6328 0.2901 0.081 Uiso 1 1 calc R . .
C19 C 0.9671(5) 0.5397(4) 0.2817(3) 0.0429(12) Uani 1 1 d . . .
H19 H 1.0482 0.5867 0.3205 0.052 Uiso 1 1 calc R . .
C20 C 0.9608(4) 0.4335(4) 0.2296(3) 0.0355(11) Uani 1 1 d . . .
H20 H 1.0396 0.3958 0.2271 0.043 Uiso 1 1 calc R . .
C21 C 0.9138(4) 0.2430(4) 0.0592(2) 0.0256(9) Uani 1 1 d . . .
C22 C 0.9402(5) 0.3260(4) -0.0092(3) 0.0405(12) Uani 1 1 d . . .
H22 H 0.879 0.382 -0.0273 0.049 Uiso 1 1 calc R . .
C23 C 1.0594(6) 0.3242(5) -0.0503(3) 0.0521(14) Uani 1 1 d . . .
H23 H 1.0783 0.3808 -0.0957 0.062 Uiso 1 1 calc R . .
C24 C 1.1480(5) 0.2431(5) -0.0264(3) 0.0486(13) Uani 1 1 d . . .
H24 H 1.2278 0.2442 -0.0545 0.058 Uiso 1 1 calc R . .
C25 C 1.1207(5) 0.1610(5) 0.0381(3) 0.0445(12) Uani 1 1 d . . .
H25 H 1.1807 0.1032 0.0537 0.053 Uiso 1 1 calc R . .
C26 C 1.0048(4) 0.1601(4) 0.0824(3) 0.0332(10) Uani 1 1 d . . .
H26 H 0.9886 0.1032 0.128 0.04 Uiso 1 1 calc R . .
C27 C 0.7431(4) 0.1162(4) 0.1855(3) 0.0236(9) Uani 1 1 d . . .
C28 C 0.6802(5) -0.0083(4) 0.1493(3) 0.0391(11) Uani 1 1 d . . .
H28 H 0.6501 -0.0212 0.0884 0.047 Uiso 1 1 calc R . .
C29 C 0.6619(5) -0.1136(5) 0.2030(3) 0.0478(13) Uani 1 1 d . . .
H29 H 0.6212 -0.1975 0.1779 0.057 Uiso 1 1 calc R . .
C30 C 0.7021(5) -0.0969(5) 0.2915(4) 0.0483(13) Uani 1 1 d . . .
H30 H 0.688 -0.1688 0.3271 0.058 Uiso 1 1 calc R . .
C31 C 0.7627(5) 0.0240(5) 0.3284(3) 0.0411(12) Uani 1 1 d . . .
H31 H 0.7904 0.0352 0.3894 0.049 Uiso 1 1 calc R . .
C32 C 0.7837(4) 0.1305(4) 0.2767(3) 0.0279(10) Uani 1 1 d . . .
H32 H 0.8258 0.2134 0.3031 0.034 Uiso 1 1 calc R . .
N1 N 0.2819(4) 0.1142(3) 0.3215(2) 0.0348(9) Uani 1 1 d . . .
N2 N 0.8223(3) 0.3886(3) 0.1809(2) 0.0299(8) Uani 1 1 d . . .
P1 P 0.33286(12) 0.25628(11) 0.38786(7) 0.0286(3) Uani 1 1 d . . .
P2 P 0.76150(11) 0.25013(11) 0.11335(7) 0.0277(3) Uani 1 1 d . . .
B1 B 0.2031(6) 0.2615(6) 0.4698(4) 0.0481(15) Uani 1 1 d . . .
H1A H 0.1092 0.268 0.4382 0.072 Uiso 1 1 calc R . .
H1B H 0.243 0.3362 0.51 0.072 Uiso 1 1 calc R . .
H1C H 0.1919 0.183 0.5025 0.072 Uiso 1 1 calc R . .
B2 B 0.5861(6) 0.2525(6) 0.0345(4) 0.0511(16) Uani 1 1 d . . .
H2A H 0.5069 0.245 0.0671 0.077 Uiso 1 1 calc R . .
H2B H 0.564 0.1803 -0.008 0.077 Uiso 1 1 calc R . .
H2C H 0.5986 0.3333 0.0044 0.077 Uiso 1 1 calc R . .
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 0 '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'
B B 0.0013 0.0007 '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
_geom_angle_publ_flag
N1 C1 C2 108.2(4) . . ?
C1 C2 C3 105.3(4) . . ?
C4 C3 C2 105.7(4) . . ?
N1 C4 C3 110.6(4) . . ?
C6 C5 C10 118.2(4) . . ?
C6 C5 P1 118.6(3) . . ?
C10 C5 P1 123.2(3) . . ?
C7 C6 C5 120.0(4) . . ?
C8 C7 C6 121.1(4) . . ?
C9 C8 C7 119.5(5) . . ?
C8 C9 C10 121.5(5) . . ?
C5 C10 C9 119.8(4) . . ?
C12 C11 C16 116.5(4) . . ?
C12 C11 P1 119.8(3) . . ?
C16 C11 P1 123.7(3) . . ?
C13 C12 C11 118.4(4) . . ?
C14 C13 C12 122.5(5) . . ?
C15 C14 C13 119.7(6) . . ?
C14 C15 C16 120.9(6) . . ?
C15 C16 C11 121.9(5) . . ?
N2 C17 C18 106.5(4) . . ?
C17 C18 C19 106.7(4) . . ?
C20 C19 C18 106.1(4) . . ?
C19 C20 N2 111.2(4) . . ?
C26 C21 C22 118.6(4) . . ?
C26 C21 P2 123.3(3) . . ?
C22 C21 P2 118.1(3) . . ?
C21 C22 C23 118.9(4) . . ?
C24 C23 C22 121.8(4) . . ?
C25 C24 C23 119.4(4) . . ?
C24 C25 C26 121.3(4) . . ?
C21 C26 C25 120.1(4) . . ?
C28 C27 C32 117.7(4) . . ?
C28 C27 P2 118.5(3) . . ?
C32 C27 P2 123.8(3) . . ?
C29 C28 C27 120.1(4) . . ?
C30 C29 C28 120.9(5) . . ?
C31 C30 C29 120.0(5) . . ?
C30 C31 C32 120.5(5) . . ?
C31 C32 C27 120.8(4) . . ?
C4 N1 C1 110.2(4) . . ?
C4 N1 P1 126.6(3) . . ?
C1 N1 P1 123.0(3) . . ?
C20 N2 C17 109.6(4) . . ?
C20 N2 P2 126.9(3) . . ?
C17 N2 P2 123.3(3) . . ?
N1 P1 C11 105.32(18) . . ?
N1 P1 C5 103.80(17) . . ?
C11 P1 C5 106.63(18) . . ?
N1 P1 B1 112.8(2) . . ?
C11 P1 B1 113.3(2) . . ?
C5 P1 B1 114.0(2) . . ?
N2 P2 C27 105.68(18) . . ?
N2 P2 C21 104.52(17) . . ?
C27 P2 C21 106.17(18) . . ?
N2 P2 B2 112.1(2) . . ?
C27 P2 B2 113.6(2) . . ?
C21 P2 B2 113.9(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.395(5) . ?
C1 C2 1.442(8) . ?
C2 C3 1.514(6) . ?
C3 C4 1.399(7) . ?
C4 N1 1.378(5) . ?
C5 C6 1.386(5) . ?
C5 C10 1.387(5) . ?
C5 P1 1.793(4) . ?
C6 C7 1.379(6) . ?
C7 C8 1.361(6) . ?
C8 C9 1.334(6) . ?
C9 C10 1.387(6) . ?
C11 C12 1.379(5) . ?
C11 C16 1.381(5) . ?
C11 P1 1.777(4) . ?
C12 C13 1.360(5) . ?
C13 C14 1.338(7) . ?
C14 C15 1.290(7) . ?
C15 C16 1.344(6) . ?
C17 N2 1.389(5) . ?
C17 C18 1.434(7) . ?
C18 C19 1.475(7) . ?
C19 C20 1.353(6) . ?
C20 N2 1.379(5) . ?
C21 C26 1.370(5) . ?
C21 C22 1.383(5) . ?
C21 P2 1.799(4) . ?
C22 C23 1.388(6) . ?
C23 C24 1.341(6) . ?
C24 C25 1.333(6) . ?
C25 C26 1.385(6) . ?
C27 C28 1.379(6) . ?
C27 C32 1.388(5) . ?
C27 P2 1.786(4) . ?
C28 C29 1.377(6) . ?
C29 C30 1.349(6) . ?
C30 C31 1.346(6) . ?
C31 C32 1.368(5) . ?
N1 P1 1.729(4) . ?
N2 P2 1.711(4) . ?
P1 B1 1.910(5) . ?
P2 B2 1.897(5) . ?
