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_4118252
_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         'C92 H160 N4 O48 Ti17, (C1 H2 Cl2)'
_chemical_formula_sum            'C93 H162 Cl2 N4 O48 Ti17'
_chemical_formula_weight         2989.47
_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                90.2760(10)
_cell_angle_beta                 98.6040(10)
_cell_angle_gamma                113.1810(10)
_cell_formula_units_Z            2
_cell_length_a                   15.6980(6)
_cell_length_b                   17.3278(6)
_cell_length_c                   26.4054(10)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.13
_cell_measurement_theta_min      2.26
_cell_volume                     6512.3(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0878
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            89611
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.472
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1546
_refine_ls_number_reflns         18788
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          1.209
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+51.2397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.2154
_reflns_number_gt                11343
_reflns_number_total             18788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303692r_si_003.cif
_cod_data_source_block           Ti17_APA
_cod_database_code               4118252