Binding Modes of Carboxylate- and Acetylacetonate-Linked Chromophores to Homodisperse Polyoxotitanate Nanoclusters
Jesse D. Sokolow; Elzbieta Trzop; Yang Chen; Jiji Tang; Laura J. Allen; Robert H. Crabtree; Jason B. Benedict; Philip Coppens; Journal of the American Chemical Society 134 (2012) 11695–11700; doi:10.1021/ja303692r

data_4118253
_publ_section_title
;
 Binding Modes of Carboxylate- and Acetylacetonate-Linked Chromophores to
 Homodisperse Polyoxotitanate Nanoclusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11695
_journal_page_last               11700
_journal_paper_doi               10.1021/ja303692r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C86 H154 N2 O50 Ti17, 3(C3 H8 O1)'
_chemical_formula_sum            'C95 H178 N2 O53 Ti17'
_chemical_formula_weight         3010.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.3650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.948(2)
_cell_length_b                   13.7625(10)
_cell_length_c                   32.938(3)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.15
_cell_measurement_theta_min      2.38
_cell_volume                     13151.3(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART Apex II CCD Detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0873
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            75218
_diffrn_reflns_theta_full        23.33
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       prism
_exptl_crystal_F_000             6240
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
 The unit cell constrains 12 isopropanol molecules, which have been treated
 as a diffuse contribution to the overall scattering whithout specific
 atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         9512
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0618
_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/[\s^2^(Fo^2^)+(0.0847P)^2^+54.5139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1727
_reflns_number_gt                6909
_reflns_number_total             9512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303692r_si_004.cif
_cod_data_source_block           Ti17_coumarine343
_cod_original_cell_volume        13151.0(17)
_cod_database_code               4118253