#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/43/7004359.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_7004359
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 H18 N1 P Se'
_chemical_formula_sum            'C16 H18 N P Se'
_chemical_formula_weight         334.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.767(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0551(15)
_cell_length_b                   17.944(4)
_cell_length_c                   9.1410(8)
_cell_measurement_reflns_used    5795
_cell_measurement_temperature    160
_cell_measurement_theta_max      32.2947
_cell_measurement_theta_min      2.5337
_cell_measurement_wavelength     0.71073
_cell_volume                     1471.6(4)
_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      160
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       ω-φ
_diffrn_orient_matrix_UB_11      0.0109835982
_diffrn_orient_matrix_UB_12      -0.0063365619
_diffrn_orient_matrix_UB_13      0.0773765523
_diffrn_orient_matrix_UB_21      -0.0273911331
_diffrn_orient_matrix_UB_22      0.0362295342
_diffrn_orient_matrix_UB_23      0.0120130386
_diffrn_orient_matrix_UB_31      -0.0734772906
_diffrn_orient_matrix_UB_32      -0.0144439051
_diffrn_orient_matrix_UB_33      -0.0045108698
_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  0.0914
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14968
_diffrn_reflns_theta_full        32.31
_diffrn_reflns_theta_max         32.31
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.646
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0892P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.13
_refine_ls_wR_factor_ref         0.1603
_reflns_number_gt                3101
_reflns_number_total             4970
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b806325g.txt
_cod_data_source_block           (2Se)
_cod_original_cell_volume        1471.7(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7004359
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8775(4) 0.31026(18) 0.3110(4) 0.0347(7) Uani 1 1 d . . .
H1A H 0.7821 0.2852 0.2894 0.042 Uiso 1 1 calc R . .
H1B H 0.8992 0.318 0.4168 0.042 Uiso 1 1 calc R . .
C2 C 0.8768(6) 0.3814(3) 0.2313(8) 0.0879(19) Uani 1 1 d . . .
H2A H 0.7847 0.3859 0.164 0.105 Uiso 1 1 calc R . .
H2B H 0.8813 0.4223 0.3011 0.105 Uiso 1 1 calc R . .
C3 C 0.9965(7) 0.3856(3) 0.1528(6) 0.0787(17) Uani 1 1 d . . .
H3A H 1.0705 0.4197 0.2015 0.094 Uiso 1 1 calc R . .
H3B H 0.9637 0.4044 0.0543 0.094 Uiso 1 1 calc R . .
C4 C 1.0631(4) 0.31098(17) 0.1432(4) 0.0333(7) Uani 1 1 d . . .
H4A H 1.1708 0.3132 0.1659 0.04 Uiso 1 1 calc R . .
H4B H 1.0371 0.2899 0.0453 0.04 Uiso 1 1 calc R . .
C5 C 0.9318(3) 0.13898(16) 0.3950(3) 0.0263(6) Uani 1 1 d . . .
C6 C 0.9981(4) 0.17093(18) 0.5262(4) 0.0318(6) Uani 1 1 d . . .
H6 H 1.0567 0.2134 0.5245 0.038 Uiso 1 1 calc R . .
C7 C 0.9760(4) 0.1389(2) 0.6597(4) 0.0367(7) Uani 1 1 d . . .
H7 H 1.0178 0.1607 0.748 0.044 Uiso 1 1 calc R . .
C8 C 0.8927(4) 0.0752(2) 0.6617(4) 0.0405(8) Uani 1 1 d . . .
H8 H 0.8797 0.0535 0.7514 0.049 Uiso 1 1 calc R . .
C9 C 0.8284(4) 0.04341(19) 0.5323(4) 0.0377(7) Uani 1 1 d . . .
H9 H 0.7725 0 0.5343 0.045 Uiso 1 1 calc R . .
C10 C 0.8468(3) 0.07583(18) 0.3987(4) 0.0326(6) Uani 1 1 d . . .
H10 H 0.8014 0.0548 0.311 0.039 Uiso 1 1 calc R . .
C11 C 1.1451(3) 0.14152(16) 0.1889(3) 0.0242(5) Uani 1 1 d . . .
C12 C 1.2757(3) 0.17041(19) 0.2659(4) 0.0328(7) Uani 1 1 d . . .
H12 H 1.2724 0.2104 0.3301 0.039 Uiso 1 1 calc R . .
C13 C 1.4108(4) 0.1386(2) 0.2454(4) 0.0399(8) Uani 1 1 d . . .
H13 H 1.4986 0.1582 0.2951 0.048 Uiso 1 1 calc R . .
C14 C 1.4178(4) 0.0791(2) 0.1540(4) 0.0383(7) Uani 1 1 d . . .
H14 H 1.5094 0.0582 0.1422 0.046 Uiso 1 1 calc R . .
C15 C 1.2885(4) 0.05026(19) 0.0792(4) 0.0390(8) Uani 1 1 d . . .
H15 H 1.2924 0.009 0.0182 0.047 Uiso 1 1 calc R . .
C16 C 1.1529(4) 0.08232(17) 0.0943(3) 0.0311(6) Uani 1 1 d . . .
H16 H 1.0663 0.0638 0.0403 0.037 Uiso 1 1 calc R . .
N1 N 0.9975(3) 0.26639(13) 0.2556(3) 0.0251(5) Uani 1 1 d . . .
P1 P 0.96566(8) 0.17768(4) 0.22012(8) 0.02325(17) Uani 1 1 d . . .
Se1 Se 0.79504(3) 0.152862(19) 0.04693(3) 0.03406(13) 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'
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'
Se Se -0.0929 2.2259 '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
C2 C1 N1 104.2(3) . . ?
C3 C2 C1 110.8(4) . . ?
C2 C3 C4 109.7(4) . . ?
C3 C4 N1 104.0(3) . . ?
C10 C5 C6 119.8(3) . . ?
C10 C5 P1 120.1(2) . . ?
C6 C5 P1 120.0(2) . . ?
C7 C6 C5 119.4(3) . . ?
C8 C7 C6 120.1(3) . . ?
C9 C8 C7 120.4(3) . . ?
C8 C9 C10 119.9(3) . . ?
C5 C10 C9 120.3(3) . . ?
C16 C11 C12 119.5(3) . . ?
C16 C11 P1 120.0(2) . . ?
C12 C11 P1 120.4(2) . . ?
C13 C12 C11 118.9(3) . . ?
C14 C13 C12 121.4(3) . . ?
C13 C14 C15 119.5(3) . . ?
C14 C15 C16 120.2(3) . . ?
C11 C16 C15 120.5(3) . . ?
C1 N1 C4 109.2(2) . . ?
C1 N1 P1 117.7(2) . . ?
C4 N1 P1 117.4(2) . . ?
N1 P1 C5 104.12(13) . . ?
N1 P1 C11 103.99(13) . . ?
C5 P1 C11 105.40(13) . . ?
N1 P1 Se1 116.43(9) . . ?
C5 P1 Se1 112.89(10) . . ?
C11 P1 Se1 112.90(10) . . ?
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 C2 1.469(6) . ?
C1 N1 1.485(4) . ?
C2 C3 1.381(7) . ?
C3 C4 1.476(6) . ?
C4 N1 1.488(4) . ?
C5 C10 1.373(4) . ?
C5 C6 1.390(4) . ?
C5 P1 1.807(3) . ?
C6 C7 1.387(4) . ?
C7 C8 1.371(5) . ?
C8 C9 1.371(5) . ?
C9 C10 1.383(5) . ?
C11 C16 1.377(4) . ?
C11 C12 1.393(4) . ?
C11 P1 1.807(3) . ?
C12 C13 1.386(5) . ?
C13 C14 1.362(5) . ?
C14 C15 1.375(5) . ?
C15 C16 1.379(4) . ?
N1 P1 1.642(3) . ?
P1 Se1 2.1049(8) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 10212772
