#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/58/7035809.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_7035809
loop_
_publ_author_name
'Senthan, Selvam Amudhan'
'Alexander, Vedamanickam'
_publ_section_title
;
 Synthesis, luminescence, and electrochemical studies of a new series of
 octanuclear ruthenium(ii) complexes of tolylterpyridine appended
 calixresorcarenes.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14813
_journal_page_last               14822
_journal_paper_doi               10.1039/c5dt02363g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C40 H54 O12'
_chemical_formula_weight         726.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-02-14 deposited with the CCDC.
2015-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.146(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.5771(4)
_cell_length_b                   7.9566(3)
_cell_length_c                   18.3912(6)
_cell_measurement_reflns_used    4079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.3
_cell_volume                     1934.69(11)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17344
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 19990'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3407
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1008P)²+0.5444P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                2576
_reflns_number_total             3407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02363g2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7035809--7035811.cif.'
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               7035809
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
C1 C 0.22561(15) 0.2063(3) 0.44477(11) 0.0342(5) Uani 1 1 d .
C2 C 0.31719(16) 0.1247(3) 0.45437(12) 0.0380(5) Uani 1 1 d .
H2 H 0.3245 0.0166 0.4741 0.046 Uiso 1 1 calc R
C3 C 0.39796(15) 0.2031(3) 0.43482(11) 0.0321(5) Uani 1 1 d .
C4 C 0.38954(14) 0.3629(3) 0.40409(10) 0.0286(5) Uani 1 1 d .
C5 C 0.29509(14) 0.4386(3) 0.39324(10) 0.0303(5) Uani 1 1 d .
H5 H 0.2869 0.5444 0.3712 0.036 Uiso 1 1 calc R
C6 C 0.21210(14) 0.3655(3) 0.41339(10) 0.0296(5) Uani 1 1 d .
C7 C 0.10957(15) 0.4517(3) 0.39912(11) 0.0323(5) Uani 1 1 d .
H7 H 0.0774 0.4158 0.4391 0.039 Uiso 1 1 calc R
C8 C 0.11508(17) 0.6432(3) 0.40244(14) 0.0422(6) Uani 1 1 d .
H8A H 0.1607 0.6766 0.4488 0.051 Uiso 1 1 calc R
H8B H 0.1431 0.6836 0.3616 0.051 Uiso 1 1 calc R
C9 C 0.0138(2) 0.7256(4) 0.3977(2) 0.0722(9) Uani 1 1 d .
H9A H -0.0292 0.7048 0.3493 0.108 Uiso 1 1 calc R
H9B H 0.0229 0.8445 0.4051 0.108 Uiso 1 1 calc R
H9C H -0.0169 0.6798 0.4355 0.108 Uiso 1 1 calc R
C10 C 0.04322(14) 0.3862(3) 0.32606(11) 0.0298(5) Uani 1 1 d .
C11 C -0.03170(15) 0.2677(3) 0.32547(11) 0.0339(5) Uani 1 1 d .
C13 C 0.48007(15) 0.4484(3) 0.38385(11) 0.0307(5) Uani 1 1 d .
H13 H 0.5395 0.4174 0.4227 0.037 Uiso 1 1 calc R
C14 C 0.47416(16) 0.6398(3) 0.38408(12) 0.0371(5) Uani 1 1 d .
H14A H 0.4161 0.6756 0.3461 0.044 Uiso 1 1 calc R
H14B H 0.4641 0.6771 0.4321 0.044 Uiso 1 1 calc R
C15 C 0.5684(2) 0.7228(3) 0.36960(16) 0.0554(7) Uani 1 1 d .
H15A H 0.6271 0.6771 0.4030 0.083 Uiso 1 1 calc R
H15B H 0.5653 0.8417 0.3777 0.083 Uiso 1 1 calc R
H15C H 0.5725 0.7022 0.3189 0.083 Uiso 1 1 calc R
C16 C 0.49871(14) 0.3821(3) 0.31015(11) 0.0288(5) Uani 1 1 d .
C17 C 0.57357(15) 0.2647(3) 0.30788(11) 0.0327(5) Uani 1 1 d .
C18 C -0.09042(15) 0.2072(3) 0.25916(12) 0.0363(5) Uani 1 1 d .
H18 H -0.1409 0.1285 0.2597 0.044 Uiso 1 1 calc R
C19 C 0.05855(14) 0.4383(3) 0.25760(11) 0.0281(5) Uani 1 1 d .
H19 H 0.1100 0.5151 0.2571 0.034 Uiso 1 1 calc R
C20 C 0.7500 0.6118(7) 0.2500 0.0989(18) Uani 1 2 d S
C21 C 0.2500 0.9136(5) 0.2500 0.0527(9) Uani 1 2 d S
C22 C 0.1578(3) 1.0062(5) 0.2557(2) 0.1043(15) Uani 1 1 d .
H22A H 0.1051 0.9277 0.2587 0.157 Uiso 1 1 calc R
H22B H 0.1362 1.0761 0.2125 0.157 Uiso 1 1 calc R
H22C H 0.1720 1.0751 0.2997 0.157 Uiso 1 1 calc R
O1 O 0.15099(11) 0.1211(2) 0.46919(9) 0.0480(5) Uani 1 1 d .
H1 H 0.0993 0.1781 0.4613 0.072 Uiso 1 1 calc R
O2 O 0.48850(12) 0.1176(2) 0.44714(9) 0.0441(5) Uani 1 1 d D
O3 O 0.63181(12) 0.2025(2) 0.37391(9) 0.0461(5) Uani 1 1 d D
O4 O -0.04466(12) 0.2097(2) 0.39310(8) 0.0482(5) Uani 1 1 d .
H4 H -0.0907 0.1407 0.3861 0.072 Uiso 1 1 calc R
O5 O 0.7500 0.7931(4) 0.2500 0.0861(10) Uani 1 2 d S
O6 O -0.20480(13) -0.0056(2) 0.38104(9) 0.0480(5) Uani 1 1 d D
O7 O 0.2500 0.7618(3) 0.2500 0.0666(8) Uani 1 2 d S
H6A H -0.194(4) -0.040(6) 0.4241(12) 0.165(17) Uiso 1 1 d D
H3A H 0.684(3) 0.130(6) 0.369(3) 0.17(2) Uiso 1 1 d D
H2A H 0.540(3) 0.152(8) 0.424(3) 0.18(2) Uiso 1 1 d D
H6B H -0.233(4) -0.066(6) 0.3467(18) 0.165(17) Uiso 1 1 d 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 0.0000 0.0000 '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'
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
O1 C1 C2 115.84(19) . .
O1 C1 C6 123.24(19) . .
C2 C1 C6 120.91(19) . .
C1 C2 C3 120.1(2) . .
C1 C2 H2 119.9 . .
C3 C2 H2 119.9 . .
O2 C3 C2 117.85(19) . .
O2 C3 C4 120.51(18) . .
C2 C3 C4 121.65(19) . .
C3 C4 C5 116.38(18) . .
C3 C4 C13 120.89(17) . .
C5 C4 C13 122.73(18) . .
C4 C5 C6 123.9(2) . .
C4 C5 H5 118.1 . .
C6 C5 H5 118.1 . .
C1 C6 C5 117.01(19) . .
C1 C6 C7 120.86(18) . .
C5 C6 C7 122.09(19) . .
C6 C7 C8 114.12(18) . .
C6 C7 C10 109.37(16) . .
C8 C7 C10 112.89(18) . .
C6 C7 H7 106.7 . .
C8 C7 H7 106.7 . .
C10 C7 H7 106.7 . .
C9 C8 C7 113.3(2) . .
C9 C8 H8A 108.9 . .
C7 C8 H8A 108.9 . .
C9 C8 H8B 108.9 . .
C7 C8 H8B 108.9 . .
H8A C8 H8B 107.7 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 C19 117.28(18) . .
C11 C10 C7 121.58(18) . .
C19 C10 C7 121.09(18) . .
O4 C11 C18 120.95(19) . .
O4 C11 C10 117.78(18) . .
C18 C11 C10 121.26(19) . .
C4 C13 C14 113.56(17) . .
C4 C13 C16 111.58(16) . .
C14 C13 C16 111.52(17) . .
C4 C13 H13 106.6 . .
C14 C13 H13 106.6 . .
C16 C13 H13 106.6 . .
C15 C14 C13 112.79(19) . .
C15 C14 H14A 109.0 . .
C13 C14 H14A 109.0 . .
C15 C14 H14B 109.0 . .
C13 C14 H14B 109.0 . .
H14A C14 H14B 107.8 . .
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 . .
C19 C16 C17 117.10(18) 2 .
C19 C16 C13 120.95(18) 2 .
C17 C16 C13 121.96(17) . .
O3 C17 C18 119.22(19) . 2
O3 C17 C16 119.42(18) . .
C18 C17 C16 121.36(18) 2 .
C17 C18 C11 119.5(2) 2 .
C17 C18 H18 120.2 2 .
C11 C18 H18 120.2 . .
C16 C19 C10 123.47(19) 2 .
C16 C19 H19 118.3 2 .
C10 C19 H19 118.3 . .
O7 C21 C22 119.9(2) . 2
O7 C21 C22 119.9(2) . .
C22 C21 C22 120.1(5) 2 .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C1 O1 H1 109.5 . .
C3 O2 H2A 121(4) . .
C17 O3 H3A 116(3) . .
C11 O4 H4 109.5 . .
H6A O6 H6B 120(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.377(3) .
C1 C2 1.378(3) .
C1 C6 1.387(3) .
C2 C3 1.378(3) .
C2 H2 0.9300 .
C3 O2 1.378(2) .
C3 C4 1.386(3) .
C4 C5 1.390(3) .
C4 C13 1.523(3) .
C5 C6 1.391(3) .
C5 H5 0.9300 .
C6 C7 1.520(3) .
C7 C8 1.526(3) .
C7 C10 1.529(3) .
C7 H7 0.9800 .
C8 C9 1.508(4) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 C11 1.385(3) .
C10 C19 1.386(3) .
C11 O4 1.375(3) .
C11 C18 1.383(3) .
C13 C14 1.525(3) .
C13 C16 1.528(3) .
C13 H13 0.9800 .
C14 C15 1.516(3) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 C19 1.384(3) 2
C16 C17 1.388(3) .
C17 O3 1.381(2) .
C17 C18 1.382(3) 2
C18 C17 1.382(3) 2
C18 H18 0.9300 .
C19 C16 1.384(3) 2
C19 H19 0.9300 .
C20 O5 1.442(6) .
C21 O7 1.207(4) .
C21 C22 1.478(4) 2
C21 C22 1.478(4) .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
O1 H1 0.8200 .
O2 H2A 0.937(10) .
O3 H3A 0.932(10) .
O4 H4 0.8200 .
O6 H6A 0.818(19) .
O6 H6B 0.817(18) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O4 0.82 2.08 2.797(2) 145.2 .
O4 H4 O6 0.82 1.92 2.737(2) 172.0 .
O6 H6A O1 0.818(19) 2.023(19) 2.837(2) 174(5) 3_556
O3 H3A O6 0.932(10) 1.829(15) 2.747(2) 168(5) 1_655
O2 H2A O3 0.937(10) 1.758(12) 2.692(2) 175(6) .
O6 H6B O5 0.817(18) 2.07(3) 2.842(3) 158(5) 1_445
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 C1 C2 C3 -177.03(19) . .
C6 C1 C2 C3 2.0(3) . .
C1 C2 C3 O2 178.52(19) . .
C1 C2 C3 C4 -1.1(3) . .
O2 C3 C4 C5 179.55(17) . .
C2 C3 C4 C5 -0.8(3) . .
O2 C3 C4 C13 -0.5(3) . .
C2 C3 C4 C13 179.12(18) . .
C3 C4 C5 C6 2.1(3) . .
C13 C4 C5 C6 -177.87(18) . .
O1 C1 C6 C5 178.13(18) . .
C2 C1 C6 C5 -0.8(3) . .
O1 C1 C6 C7 -4.3(3) . .
C2 C1 C6 C7 176.80(19) . .
C4 C5 C6 C1 -1.3(3) . .
C4 C5 C6 C7 -178.83(17) . .
C1 C6 C7 C8 151.0(2) . .
C5 C6 C7 C8 -31.6(3) . .
C1 C6 C7 C10 -81.5(2) . .
C5 C6 C7 C10 96.0(2) . .
C6 C7 C8 C9 -172.9(2) . .
C10 C7 C8 C9 61.4(3) . .
C6 C7 C10 C11 101.7(2) . .
C8 C7 C10 C11 -130.1(2) . .
C6 C7 C10 C19 -75.6(2) . .
C8 C7 C10 C19 52.6(3) . .
C19 C10 C11 O4 177.27(18) . .
C7 C10 C11 O4 -0.2(3) . .
C19 C10 C11 C18 -1.6(3) . .
C7 C10 C11 C18 -179.03(19) . .
C3 C4 C13 C14 -154.43(19) . .
C5 C4 C13 C14 25.5(3) . .
C3 C4 C13 C16 78.5(2) . .
C5 C4 C13 C16 -101.6(2) . .
C4 C13 C14 C15 175.64(18) . .
C16 C13 C14 C15 -57.3(2) . .
C4 C13 C16 C19 79.6(2) . 2
C14 C13 C16 C19 -48.6(2) . 2
C4 C13 C16 C17 -100.9(2) . .
C14 C13 C16 C17 131.0(2) . .
C19 C16 C17 O3 -179.00(18) 2 .
C13 C16 C17 O3 1.5(3) . .
C19 C16 C17 C18 0.3(3) 2 2
C13 C16 C17 C18 -179.2(2) . 2
O4 C11 C18 C17 -178.2(2) . 2
C10 C11 C18 C17 0.6(3) . 2
C11 C10 C19 C16 2.0(3) . 2
C7 C10 C19 C16 179.47(18) . 2
