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_4118259
_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         'C78 H158 O57 Ti18, C4 H10 O, C7 H14 O2'
_chemical_formula_sum            'C89 H182 O60 Ti18'
_chemical_formula_weight         3074.55
_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                75.1390(10)
_cell_angle_beta                 84.9420(10)
_cell_angle_gamma                77.3480(10)
_cell_formula_units_Z            2
_cell_length_a                   14.2444(6)
_cell_length_b                   19.1492(8)
_cell_length_c                   26.1335(10)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.18
_cell_volume                     6718.8(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART Apex II CCD Detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            114085
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
 The unit cell constrains two t-butanol molecules and two t-butyl propionate
 molecules which have been treated as a diffuse contribution to the overall
 scattering whithout specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         3.332
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         27543
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                17862
_reflns_number_total             27543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303692r_si_010.cif
_cod_data_source_block           Ti18_propionicacid
_cod_database_code               4118259