#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:11:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179049 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/11/4301115.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_4301115
loop_
_publ_author_name
'Serena J. Smalley'
'Mark R. Waterland'
'Shane G. Telfer'
_publ_section_title
;
Heteroleptic Dipyrrin/Bipyridine Complexes of Ruthenium(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13
_journal_page_last               15
_journal_paper_doi               10.1021/ic8016497
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '(C36 H26 N6 O2 Ru1), (C1 H4 O1), 6(O1 H2)'
_chemical_formula_sum            'C37 H42 N6 O9 Ru'
_chemical_formula_weight         815.83
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.0700(10)
_cell_angle_beta                 90.1170(10)
_cell_angle_gamma                92.8580(10)
_cell_formula_units_Z            2
_cell_length_a                   8.76980(10)
_cell_length_b                   12.46720(10)
_cell_length_c                   17.3089(2)
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      0.992
_cell_volume                     1796.58(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXL
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       ω
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            73884
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.9241
_exptl_absorpt_correction_T_min  0.8807
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.814
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         10474
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0728P)²+3.4577P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1341
_reflns_number_gt                9232
_reflns_number_total             10474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8016497_si_002.cif
_cod_data_source_block           1b
_cod_database_code               4301115
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
Ru01 Ru 0.45253(2) 0.175721(16) 0.814590(11) 0.01485(7) Uani 1 1 d . . .
C1 C 0.2943(3) 0.0325(2) 0.90881(16) 0.0222(5) Uani 1 1 d . . .
H1 H 0.2467 -0.0147 0.8616 0.027 Uiso 1 1 calc R . .
C2 C 0.2762(4) 0.0189(3) 0.98626(17) 0.0280(6) Uani 1 1 d . . .
H2 H 0.2149 -0.0360 0.9991 0.034 Uiso 1 1 calc R . .
C3 C 0.3672(4) 0.1029(3) 1.03888(17) 0.0280(6) Uani 1 1 d . . .
H3 H 0.3808 0.1150 1.0943 0.034 Uiso 1 1 calc R . .
C4 C 0.4372(3) 0.1682(2) 0.99253(16) 0.0211(5) Uani 1 1 d . . .
C5 C 0.5373(3) 0.2637(2) 1.02121(16) 0.0213(5) Uani 1 1 d . . .
C6 C 0.5945(3) 0.3332(2) 0.97748(15) 0.0188(5) Uani 1 1 d . . .
C7 C 0.6800(3) 0.4385(2) 1.00971(16) 0.0214(5) Uani 1 1 d . . .
H7 H 0.7175 0.4697 1.0627 0.026 Uiso 1 1 calc R . .
C8 C 0.6964(3) 0.4848(2) 0.94790(16) 0.0211(5) Uani 1 1 d . . .
H8 H 0.7458 0.5537 0.9508 0.025 Uiso 1 1 calc R . .
C9 C 0.6228(3) 0.4067(2) 0.87853(16) 0.0194(5) Uani 1 1 d . . .
H9 H 0.6174 0.4172 0.8277 0.023 Uiso 1 1 calc R . .
C11 C 0.5877(4) 0.2970(2) 1.10867(17) 0.0275(6) Uani 1 1 d . . .
C12 C 0.4862(4) 0.3435(3) 1.17062(17) 0.0320(7) Uani 1 1 d . . .
H12 H 0.3846 0.3505 1.1582 0.038 Uiso 1 1 calc R . .
C13 C 0.5384(5) 0.3796(3) 1.25139(19) 0.0425(9) Uani 1 1 d . . .
H13 H 0.4710 0.4112 1.2926 0.051 Uiso 1 1 calc R . .
C14 C 0.6882(6) 0.3692(3) 1.2709(2) 0.0467(11) Uani 1 1 d . . .
C15 C 0.7863(5) 0.3223(3) 1.2097(2) 0.0473(11) Uani 1 1 d . . .
H15 H 0.8873 0.3141 1.2224 0.057 Uiso 1 1 calc R . .
C16 C 0.7369(5) 0.2866(3) 1.1286(2) 0.0372(8) Uani 1 1 d . . .
H16 H 0.8054 0.2557 1.0878 0.045 Uiso 1 1 calc R . .
C17 C 0.7444(8) 0.4116(3) 1.3588(3) 0.0667(18) Uani 1 1 d U . .
C21 C 0.7697(3) 0.1031(2) 0.84037(16) 0.0214(5) Uani 1 1 d . . .
H21 H 0.7863 0.1759 0.8761 0.026 Uiso 1 1 calc R . .
C22 C 0.8852(3) 0.0282(3) 0.83005(19) 0.0272(6) Uani 1 1 d . . .
H22 H 0.9776 0.0508 0.8583 0.033 Uiso 1 1 calc R . .
C23 C 0.8617(4) -0.0802(3) 0.7774(2) 0.0302(6) Uani 1 1 d . . .
H23 H 0.9379 -0.1316 0.7698 0.036 Uiso 1 1 calc R . .
C24 C 0.7232(3) -0.1113(2) 0.73605(18) 0.0261(6) Uani 1 1 d . . .
H24 H 0.7049 -0.1840 0.7005 0.031 Uiso 1 1 calc R . .
C25 C 0.6111(3) -0.0322(2) 0.74831(15) 0.0186(5) Uani 1 1 d . . .
C26 C 0.4610(3) -0.0560(2) 0.70676(15) 0.0183(5) Uani 1 1 d . . .
C27 C 0.4188(4) -0.1566(2) 0.64679(17) 0.0240(5) Uani 1 1 d . . .
H27 H 0.4870 -0.2139 0.6309 0.029 Uiso 1 1 calc R . .
C28 C 0.2752(4) -0.1711(2) 0.61078(16) 0.0265(6) Uani 1 1 d . . .
H28 H 0.2456 -0.2380 0.5706 0.032 Uiso 1 1 calc R . .
C29 C 0.1765(4) -0.0842(2) 0.63564(17) 0.0262(6) Uani 1 1 d . . .
H29 H 0.0792 -0.0919 0.6125 0.031 Uiso 1 1 calc R . .
C30 C 0.2244(3) 0.0144(2) 0.69544(16) 0.0217(5) Uani 1 1 d . . .
H30 H 0.1575 0.0725 0.7118 0.026 Uiso 1 1 calc R . .
C34 C 0.1573(3) 0.2885(2) 0.8737(2) 0.0330(7) Uani 1 1 d . . .
H34 H 0.1670 0.2597 0.9169 0.040 Uiso 1 1 calc R . .
C35 C 0.0327(4) 0.3508(3) 0.8708(4) 0.0555(13) Uani 1 1 d . . .
H35 H -0.0394 0.3641 0.9116 0.067 Uiso 1 1 calc R . .
C36 C 0.0167(4) 0.3929(4) 0.8070(4) 0.0734(19) Uani 1 1 d . . .
H36 H -0.0674 0.4337 0.8033 0.088 Uiso 1 1 calc R . .
C37 C 0.1264(5) 0.3739(4) 0.7489(4) 0.0616(15) Uani 1 1 d . . .
H37 H 0.1174 0.4026 0.7056 0.074 Uiso 1 1 calc R . .
C38 C 0.2516(4) 0.3116(3) 0.7543(2) 0.0347(8) Uani 1 1 d . . .
C39 C 0.3788(4) 0.2903(2) 0.69793(19) 0.0322(7) Uani 1 1 d . . .
C40 C 0.3875(7) 0.3267(3) 0.6293(2) 0.0556(14) Uani 1 1 d . . .
H40 H 0.3057 0.3612 0.6144 0.067 Uiso 1 1 calc R . .
C41 C 0.5181(8) 0.3111(3) 0.5839(2) 0.0739(19) Uani 1 1 d . . .
H41 H 0.5256 0.3352 0.5383 0.089 Uiso 1 1 calc R . .
C42 C 0.6380(8) 0.2592(4) 0.6072(2) 0.0675(17) Uani 1 1 d . . .
H42 H 0.7281 0.2497 0.5782 0.081 Uiso 1 1 calc R . .
C43 C 0.6221(5) 0.2214(3) 0.67427(19) 0.0388(8) Uani 1 1 d . . .
H43 H 0.7021 0.1850 0.6890 0.047 Uiso 1 1 calc R . .
N1 N 0.3883(3) 0.12169(18) 0.91151(13) 0.0179(4) Uani 1 1 d . . .
N10 N 0.5625(2) 0.31632(18) 0.89528(13) 0.0172(4) Uani 1 1 d . . .
N20 N 0.6339(3) 0.07438(18) 0.80053(12) 0.0166(4) Uani 1 1 d . . .
N31 N 0.3641(3) 0.02950(18) 0.73099(13) 0.0174(4) Uani 1 1 d . . .
N33 N 0.2649(3) 0.26788(19) 0.81673(17) 0.0255(5) Uani 1 1 d . . .
N44 N 0.4950(3) 0.23557(19) 0.71871(14) 0.0243(5) Uani 1 1 d . . .
O18 O 0.6461(6) 0.4334(2) 1.41377(17) 0.0761(14) Uani 1 1 d U . .
O19 O 0.8872(6) 0.4225(3) 1.3710(2) 0.0844(15) Uani 1 1 d U . .
O100 O 0.9347(6) 0.3987(4) 1.5242(3) 0.0902(14) Uani 1 1 d . . .
C101 C 0.9528(7) 0.3200(6) 1.5714(4) 0.0749(16) Uani 1 1 d . . .
H10A H 1.0426 0.2786 1.5542 0.112 Uiso 1 1 calc R . .
H10B H 0.8650 0.2682 1.5625 0.112 Uiso 1 1 calc R . .
H10C H 0.9626 0.3618 1.6281 0.112 Uiso 1 1 calc R . .
O1W O 0.3448(5) 0.4212(2) 1.43072(16) 0.0656(11) Uani 1 1 d . . .
O2W O 0.1160(7) 0.2915(4) 1.4300(3) 0.0420(12) Uani 0.50 1 d P . .
O3W O 0.1451(7) 0.2413(4) 1.4628(4) 0.0473(13) Uani 0.50 1 d P . .
O4W O -0.0258(7) 0.1194(4) 0.6092(4) 0.116(2) Uani 1 1 d . . .
O5W O 0.1249(8) 0.4636(9) 1.3178(5) 0.071(2) Uani 0.50 1 d P . .
O6W O 0.8001(14) -0.0377(8) 0.5185(9) 0.096(4) Uani 0.50 1 d P . .
O7W O 0.1107(13) 0.2816(11) 1.1063(8) 0.120(4) Uani 0.50 1 d P . .
O8W O 0.7934(10) -0.0867(9) 0.5232(6) 0.070(2) Uani 0.50 1 d P . .
O9W O 0.5000 0.0000 0.5000 0.132(3) Uani 1 2 d S . .
O10W O 0.1871(7) 0.4309(7) 1.2808(3) 0.0556(18) Uani 0.50 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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
N33 Ru01 N44 78.99(11) . . ?
N33 Ru01 N20 174.18(9) . . ?
N44 Ru01 N20 97.82(10) . . ?
N33 Ru01 N31 96.08(9) . . ?
N44 Ru01 N31 87.14(9) . . ?
N20 Ru01 N31 78.82(9) . . ?
N33 Ru01 N1 95.35(10) . . ?
N44 Ru01 N1 174.26(10) . . ?
N20 Ru01 N1 87.75(8) . . ?
N31 Ru01 N1 92.61(8) . . ?
N33 Ru01 N10 89.25(9) . . ?
N44 Ru01 N10 91.87(9) . . ?
N20 Ru01 N10 95.75(9) . . ?
N31 Ru01 N10 174.28(9) . . ?
N1 Ru01 N10 88.93(9) . . ?
N1 C1 C2 111.9(2) . . ?
C3 C2 C1 106.2(3) . . ?
C2 C3 C4 107.2(2) . . ?
N1 C4 C5 124.3(2) . . ?
N1 C4 C3 108.5(2) . . ?
C5 C4 C3 127.2(2) . . ?
C6 C5 C4 127.0(2) . . ?
C6 C5 C11 115.6(2) . . ?
C4 C5 C11 117.3(2) . . ?
C5 C6 N10 124.6(2) . . ?
C5 C6 C7 126.5(2) . . ?
N10 C6 C7 108.6(2) . . ?
C8 C7 C6 107.1(2) . . ?
C7 C8 C9 106.3(2) . . ?
N10 C9 C8 111.6(2) . . ?
C16 C11 C12 119.2(3) . . ?
C16 C11 C5 120.1(3) . . ?
C12 C11 C5 120.7(3) . . ?
C11 C12 C13 119.5(4) . . ?
C14 C13 C12 121.1(4) . . ?
C15 C14 C13 119.0(3) . . ?
C15 C14 C17 120.5(4) . . ?
C13 C14 C17 120.5(4) . . ?
C14 C15 C16 120.9(4) . . ?
C11 C16 C15 120.4(4) . . ?
O18 C17 O19 125.0(4) . . ?
O18 C17 C14 118.0(5) . . ?
O19 C17 C14 117.0(5) . . ?
N20 C21 C22 122.5(3) . . ?
C23 C22 C21 119.3(3) . . ?
C22 C23 C24 119.0(3) . . ?
C23 C24 C25 119.2(3) . . ?
N20 C25 C24 121.7(3) . . ?
N20 C25 C26 114.7(2) . . ?
C24 C25 C26 123.6(2) . . ?
N31 C26 C27 121.5(3) . . ?
N31 C26 C25 114.7(2) . . ?
C27 C26 C25 123.9(2) . . ?
C28 C27 C26 119.8(3) . . ?
C27 C28 C29 118.7(3) . . ?
C28 C29 C30 119.2(3) . . ?
N31 C30 C29 122.6(3) . . ?
N33 C34 C35 122.7(4) . . ?
C36 C35 C34 119.1(4) . . ?
C37 C36 C35 119.0(4) . . ?
C36 C37 C38 120.3(4) . . ?
N33 C38 C37 120.4(4) . . ?
N33 C38 C39 114.5(3) . . ?
C37 C38 C39 125.1(4) . . ?
N44 C39 C40 121.0(4) . . ?
N44 C39 C38 115.0(3) . . ?
C40 C39 C38 123.9(3) . . ?
C41 C40 C39 119.5(4) . . ?
C40 C41 C42 119.2(3) . . ?
C41 C42 C43 119.2(5) . . ?
N44 C43 C42 122.1(4) . . ?
C1 N1 C4 106.2(2) . . ?
C1 N1 Ru01 126.61(18) . . ?
C4 N1 Ru01 127.18(18) . . ?
C9 N10 C6 106.5(2) . . ?
C9 N10 Ru01 126.80(18) . . ?
C6 N10 Ru01 126.68(17) . . ?
C21 N20 C25 118.2(2) . . ?
C21 N20 Ru01 125.75(18) . . ?
C25 N20 Ru01 115.99(18) . . ?
C30 N31 C26 118.2(2) . . ?
C30 N31 Ru01 125.94(18) . . ?
C26 N31 Ru01 115.71(17) . . ?
C34 N33 C38 118.5(3) . . ?
C34 N33 Ru01 125.9(2) . . ?
C38 N33 Ru01 115.7(2) . . ?
C43 N44 C39 118.9(3) . . ?
C43 N44 Ru01 125.9(2) . . ?
C39 N44 Ru01 115.1(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
Ru01 N33 2.047(2) . ?
Ru01 N44 2.048(2) . ?
Ru01 N20 2.049(2) . ?
Ru01 N31 2.058(2) . ?
Ru01 N1 2.062(2) . ?
Ru01 N10 2.064(2) . ?
C1 N1 1.340(3) . ?
C1 C2 1.411(4) . ?
C2 C3 1.373(4) . ?
C3 C4 1.429(4) . ?
C4 N1 1.398(3) . ?
C4 C5 1.400(4) . ?
C5 C6 1.393(4) . ?
C5 C11 1.500(4) . ?
C6 N10 1.398(3) . ?
C6 C7 1.430(4) . ?
C7 C8 1.369(4) . ?
C8 C9 1.419(3) . ?
C9 N10 1.333(3) . ?
C11 C16 1.375(5) . ?
C11 C12 1.396(5) . ?
C12 C13 1.398(4) . ?
C13 C14 1.378(6) . ?
C14 C15 1.368(7) . ?
C14 C17 1.520(5) . ?
C15 C16 1.396(5) . ?
C17 O18 1.260(8) . ?
C17 O19 1.263(7) . ?
C21 N20 1.349(3) . ?
C21 C22 1.386(4) . ?
C22 C23 1.382(5) . ?
C23 C24 1.384(5) . ?
C24 C25 1.397(4) . ?
C25 N20 1.360(3) . ?
C25 C26 1.471(4) . ?
C26 N31 1.359(3) . ?
C26 C27 1.390(3) . ?
C27 C28 1.382(4) . ?
C28 C29 1.384(4) . ?
C29 C30 1.384(4) . ?
C30 N31 1.348(3) . ?
C34 N33 1.342(4) . ?
C34 C35 1.381(5) . ?
C35 C36 1.371(8) . ?
C36 C37 1.368(8) . ?
C37 C38 1.396(5) . ?
C38 N33 1.360(4) . ?
C38 C39 1.463(6) . ?
C39 N44 1.362(4) . ?
C39 C40 1.398(5) . ?
C40 C41 1.378(8) . ?
C41 C42 1.384(8) . ?
C42 C43 1.387(5) . ?
C43 N44 1.343(5) . ?
O100 C101 1.472(8) . ?
O2W O3W 1.007(7) . ?
O5W O10W 0.858(8) . ?
O6W O8W 0.640(10) . ?
