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#$Date: 2025-08-23 00:12:46 +0300 (Sat, 23 Aug 2025) $
#$Revision: 301866 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/54/7235438.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_7235438
loop_
_publ_author_name
'Murray, Niamh S.'
'Rudd, Jennifer A.'
'Chamayou, Anne-Christine'
'Constable, Edwin C.'
'Housecroft, Catherine E.'
'Neuburger, Markus'
'Zampese, Jennifer A.'
_publ_section_title
;
 Assembling model tris(bipyridine)ruthenium(ii) photosensitizers into
 ordered monolayers in the presence of the polyoxometallate anion
 [Co4(H2O)2(α-PW9O34)2]10−
;
_journal_issue                   23
_journal_name_full               'RSC Adv.'
_journal_page_first              11766
_journal_paper_doi               10.1039/C4RA00085D
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C48 H80 N2 O4'
_chemical_formula_sum            'C48 H80 N2 O4'
_chemical_formula_weight         749.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                85.669(15)
_cell_angle_beta                 89.406(16)
_cell_angle_gamma                76.688(15)
_cell_formula_units_Z            1
_cell_length_a                   5.3390(11)
_cell_length_b                   7.4715(16)
_cell_length_c                   28.443(6)
_cell_measurement_reflns_used    1829
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      66.40
_cell_measurement_theta_min      3.12
_cell_volume                     1100.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.1704
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            11259
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.429
_diffrn_reflns_theta_min         3.116
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   scale
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       plate
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[σ²(Fo²)+(0.1326P)²+0.2071P] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2239
_refine_ls_wR_factor_ref         0.2562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2223
_reflns_number_total             3750
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4ra00085d2.cif
_cod_data_source_block           jar127
_cod_database_code               7235438
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.794
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
N1 N 0.7557(5) 0.8874(3) 0.52416(8) 0.0252(6) Uani 1 1 d . .
O1 O 1.1985(5) 0.5656(3) 0.38628(7) 0.0354(6) Uani 1 1 d . .
O2 O 0.8651(4) 0.4329(2) 0.40325(7) 0.0266(6) Uani 1 1 d . .
C1 C 0.6430(6) 0.7534(3) 0.51441(10) 0.0269(8) Uani 1 1 d . .
H1A H 0.5103 0.7292 0.5347 0.032 Uiso 1 1 calc R U
C2 C 0.7075(6) 0.6464(3) 0.47631(10) 0.0258(7) Uani 1 1 d . .
H2A H 0.6178 0.5545 0.4702 0.031 Uiso 1 1 calc R U
C3 C 0.9074(6) 0.6778(3) 0.44740(9) 0.0222(7) Uani 1 1 d . .
C4 C 1.0257(6) 0.8172(3) 0.45642(10) 0.0251(7) Uani 1 1 d . .
H4A H 1.1615 0.8416 0.4369 0.030 Uiso 1 1 calc R U
C5 C 0.9429(6) 0.9226(3) 0.49472(9) 0.0213(7) Uani 1 1 d . .
C6 C 1.0104(6) 0.5552(4) 0.40872(10) 0.0247(7) Uani 1 1 d . .
C7 C 0.9593(6) 0.2972(4) 0.36955(10) 0.0264(7) Uani 1 1 d . .
H7A H 1.1225 0.2137 0.3810 0.032 Uiso 1 1 calc R U
H7B H 0.9916 0.3592 0.3388 0.032 Uiso 1 1 calc R U
C8 C 0.7555(6) 0.1888(4) 0.36410(10) 0.0256(7) Uani 1 1 d . .
H8A H 0.5948 0.2738 0.3520 0.031 Uiso 1 1 calc R U
H8B H 0.7187 0.1333 0.3954 0.031 Uiso 1 1 calc R U
C9 C 0.8390(6) 0.0376(4) 0.33077(10) 0.0254(7) Uani 1 1 d . .
H9A H 0.9965 -0.0493 0.3436 0.031 Uiso 1 1 calc R U
H9B H 0.8830 0.0932 0.3000 0.031 Uiso 1 1 calc R U
C10 C 0.6342(6) -0.0697(4) 0.32302(10) 0.0262(8) Uani 1 1 d . .
H10A H 0.5912 -0.1256 0.3538 0.031 Uiso 1 1 calc R U
H10B H 0.4764 0.0176 0.3105 0.031 Uiso 1 1 calc R U
C11 C 0.7144(6) -0.2205(4) 0.28950(10) 0.0265(8) Uani 1 1 d . .
H11A H 0.8701 -0.3092 0.3024 0.032 Uiso 1 1 calc R U
H11B H 0.7610 -0.1649 0.2589 0.032 Uiso 1 1 calc R U
C12 C 0.5078(6) -0.3251(4) 0.28097(10) 0.0274(8) Uani 1 1 d . .
H12A H 0.4599 -0.3793 0.3116 0.033 Uiso 1 1 calc R U
H12B H 0.3529 -0.2364 0.2678 0.033 Uiso 1 1 calc R U
C13 C 0.5871(6) -0.4774(4) 0.24790(10) 0.0256(7) Uani 1 1 d . .
H13A H 0.7412 -0.5668 0.2612 0.031 Uiso 1 1 calc R U
H13B H 0.6361 -0.4235 0.2173 0.031 Uiso 1 1 calc R U
C14 C 0.3784(6) -0.5804(4) 0.23928(10) 0.0266(8) Uani 1 1 d . .
H14A H 0.3263 -0.6316 0.2700 0.032 Uiso 1 1 calc R U
H14B H 0.2259 -0.4915 0.2253 0.032 Uiso 1 1 calc R U
C15 C 0.4591(6) -0.7362(4) 0.20711(10) 0.0270(8) Uani 1 1 d . .
H15A H 0.6096 -0.8263 0.2214 0.032 Uiso 1 1 calc R U
H15B H 0.5140 -0.6855 0.1766 0.032 Uiso 1 1 calc R U
C16 C 0.2496(6) -0.8367(4) 0.19788(10) 0.0281(8) Uani 1 1 d . .
H16A H 0.0994 -0.7468 0.1834 0.034 Uiso 1 1 calc R U
H16B H 0.1939 -0.8869 0.2284 0.034 Uiso 1 1 calc R U
C17 C 0.3315(6) -0.9936(4) 0.16582(10) 0.0278(8) Uani 1 1 d . .
H17A H 0.3911 -0.9440 0.1355 0.033 Uiso 1 1 calc R U
H17B H 0.4791 -1.0851 0.1806 0.033 Uiso 1 1 calc R U
C18 C 0.1195(6) -1.0910(4) 0.15575(10) 0.0283(8) Uani 1 1 d . .
H18A H 0.0594 -1.1402 0.1860 0.034 Uiso 1 1 calc R U
H18B H -0.0278 -0.9997 0.1408 0.034 Uiso 1 1 calc R U
C19 C 0.2020(6) -1.2483(4) 0.12390(10) 0.0286(8) Uani 1 1 d . .
H19A H 0.3452 -1.3419 0.1393 0.034 Uiso 1 1 calc R U
H19B H 0.2675 -1.2002 0.0940 0.034 Uiso 1 1 calc R U
C20 C -0.0143(7) -1.3410(4) 0.11269(11) 0.0326(8) Uani 1 1 d . .
H20A H -0.0883 -1.3806 0.1427 0.039 Uiso 1 1 calc R U
H20B H -0.1520 -1.2492 0.0953 0.039 Uiso 1 1 calc R U
C21 C 0.0696(6) -1.5076(4) 0.08365(10) 0.0304(8) Uani 1 1 d . .
H21A H 0.1515 -1.4699 0.0543 0.036 Uiso 1 1 calc R U
H21B H 0.2003 -1.6027 0.1018 0.036 Uiso 1 1 calc R U
C22 C -0.1525(7) -1.5919(4) 0.07077(11) 0.0320(8) Uani 1 1 d . .
H22A H -0.2356 -1.6276 0.1002 0.038 Uiso 1 1 calc R U
H22B H -0.2820 -1.4967 0.0524 0.038 Uiso 1 1 calc R U
C23 C -0.0737(7) -1.7596(4) 0.04230(10) 0.0339(8) Uani 1 1 d . .
H23A H 0.0516 -1.8567 0.0609 0.041 Uiso 1 1 calc R U
H23B H 0.0131 -1.7253 0.0132 0.041 Uiso 1 1 calc R U
C24 C -0.3001(7) -1.8373(4) 0.02888(12) 0.0409(9) Uani 1 1 d . .
H24A H -0.3873 -1.8715 0.0575 0.061 Uiso 1 1 calc R U
H24B H -0.2379 -1.9467 0.0113 0.061 Uiso 1 1 calc R U
H24C H -0.4212 -1.7439 0.0092 0.061 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_3
C1 N1 C5 117.7(2) .
C6 O2 C7 115.7(2) .
N1 C1 C2 123.9(3) .
N1 C1 H1A 118.0 .
C2 C1 H1A 118.0 .
C1 C2 C3 118.0(3) .
C1 C2 H2A 121.0 .
C3 C2 H2A 121.0 .
C4 C3 C2 119.2(3) .
C4 C3 C6 118.9(3) .
C2 C3 C6 121.8(2) .
C3 C4 C5 119.0(3) .
C3 C4 H4A 120.5 .
C5 C4 H4A 120.5 .
N1 C5 C4 122.0(2) .
N1 C5 C5 116.5(3) 2_776
C4 C5 C5 121.5(3) 2_776
O1 C6 O2 125.2(3) .
O1 C6 C3 123.9(3) .
O2 C6 C3 110.9(3) .
O2 C7 C8 107.6(2) .
O2 C7 H7A 110.2 .
C8 C7 H7A 110.2 .
O2 C7 H7B 110.2 .
C8 C7 H7B 110.2 .
H7A C7 H7B 108.5 .
C7 C8 C9 112.0(3) .
C7 C8 H8A 109.2 .
C9 C8 H8A 109.2 .
C7 C8 H8B 109.2 .
C9 C8 H8B 109.2 .
H8A C8 H8B 107.9 .
C8 C9 C10 113.3(3) .
C8 C9 H9A 108.9 .
C10 C9 H9A 108.9 .
C8 C9 H9B 108.9 .
C10 C9 H9B 108.9 .
H9A C9 H9B 107.7 .
C11 C10 C9 113.9(3) .
C11 C10 H10A 108.8 .
C9 C10 H10A 108.8 .
C11 C10 H10B 108.8 .
C9 C10 H10B 108.8 .
H10A C10 H10B 107.7 .
C10 C11 C12 113.9(3) .
C10 C11 H11A 108.8 .
C12 C11 H11A 108.8 .
C10 C11 H11B 108.8 .
C12 C11 H11B 108.8 .
H11A C11 H11B 107.7 .
C13 C12 C11 114.3(3) .
C13 C12 H12A 108.7 .
C11 C12 H12A 108.7 .
C13 C12 H12B 108.7 .
C11 C12 H12B 108.7 .
H12A C12 H12B 107.6 .
C12 C13 C14 114.0(3) .
C12 C13 H13A 108.8 .
C14 C13 H13A 108.8 .
C12 C13 H13B 108.8 .
C14 C13 H13B 108.8 .
H13A C13 H13B 107.7 .
C15 C14 C13 114.2(3) .
C15 C14 H14A 108.7 .
C13 C14 H14A 108.7 .
C15 C14 H14B 108.7 .
C13 C14 H14B 108.7 .
H14A C14 H14B 107.6 .
C14 C15 C16 114.2(3) .
C14 C15 H15A 108.7 .
C16 C15 H15A 108.7 .
C14 C15 H15B 108.7 .
C16 C15 H15B 108.7 .
H15A C15 H15B 107.6 .
C15 C16 C17 114.0(3) .
C15 C16 H16A 108.7 .
C17 C16 H16A 108.7 .
C15 C16 H16B 108.7 .
C17 C16 H16B 108.7 .
H16A C16 H16B 107.6 .
C18 C17 C16 113.9(3) .
C18 C17 H17A 108.8 .
C16 C17 H17A 108.8 .
C18 C17 H17B 108.8 .
C16 C17 H17B 108.8 .
H17A C17 H17B 107.7 .
C19 C18 C17 113.8(3) .
C19 C18 H18A 108.8 .
C17 C18 H18A 108.8 .
C19 C18 H18B 108.8 .
C17 C18 H18B 108.8 .
H18A C18 H18B 107.7 .
C18 C19 C20 113.4(3) .
C18 C19 H19A 108.9 .
C20 C19 H19A 108.9 .
C18 C19 H19B 108.9 .
C20 C19 H19B 108.9 .
H19A C19 H19B 107.7 .
C21 C20 C19 114.1(3) .
C21 C20 H20A 108.7 .
C19 C20 H20A 108.7 .
C21 C20 H20B 108.7 .
C19 C20 H20B 108.7 .
H20A C20 H20B 107.6 .
C22 C21 C20 113.1(3) .
C22 C21 H21A 109.0 .
C20 C21 H21A 109.0 .
C22 C21 H21B 109.0 .
C20 C21 H21B 109.0 .
H21A C21 H21B 107.8 .
C23 C22 C21 114.2(3) .
C23 C22 H22A 108.7 .
C21 C22 H22A 108.7 .
C23 C22 H22B 108.7 .
C21 C22 H22B 108.7 .
H22A C22 H22B 107.6 .
C22 C23 C24 113.0(3) .
C22 C23 H23A 109.0 .
C24 C23 H23A 109.0 .
C22 C23 H23B 109.0 .
C24 C23 H23B 109.0 .
H23A C23 H23B 107.8 .
C23 C24 H24A 109.5 .
C23 C24 H24B 109.5 .
H24A C24 H24B 109.5 .
C23 C24 H24C 109.5 .
H24A C24 H24C 109.5 .
H24B C24 H24C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.329(3) .
N1 C5 1.357(4) .
O1 C6 1.199(3) .
O2 C6 1.346(3) .
O2 C7 1.450(3) .
C1 C2 1.389(4) .
C1 H1A 0.9500 .
C2 C3 1.392(4) .
C2 H2A 0.9500 .
C3 C4 1.378(4) .
C3 C6 1.503(4) .
C4 C5 1.400(4) .
C4 H4A 0.9500 .
C5 C5 1.477(5) 2_776
C7 C8 1.514(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.515(4) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.524(4) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.515(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.522(4) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.513(4) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.525(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.516(4) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.518(4) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 C17 1.521(4) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.521(4) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 C19 1.520(4) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C20 1.525(4) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C21 1.524(4) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 C22 1.524(4) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 C23 1.519(4) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C24 1.520(4) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 85908365
