A manganese-doped polymeric framework of polyoxotitanate nanoclusters with a narrow band gap.
Chen, Yang; Sokolow, Jesse D.; Trzop, Elzbieta; Coppens, Philip; Dalton transactions (Cambridge, England : 2003) 42 (2013) 15285–15287; doi:10.1039/c3dt52218k

data_7023803
_publ_section_title
;
 A manganese-doped polymeric framework of polyoxotitanate nanoclusters
 with a narrow band gap.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15285
_journal_page_last               15287
_journal_paper_doi               10.1039/c3dt52218k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C44 H96 Br4 Mn4 O40 Ti13'
_chemical_formula_sum            'C44 H96 Br4 Mn4 O40 Ti13'
_chemical_formula_weight         2426.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           109
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2'
_symmetry_space_group_name_H-M   'I 41 m d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.8012(10)
_cell_length_b                   34.8012(10)
_cell_length_c                   14.7872(6)
_cell_measurement_reflns_used    9664
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.23
_cell_volume                     17909.1(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9472
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    3.490
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.6795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             9647
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
Program SQUEEZE/PLATON (Sluis & Spek, Acta Cryst. 1990, A46, 194) was used only for 
estimation of a diffuse contribution from the content of free unit cell volume to 
the overall scattering whithout specific atom positions. Total electron count comes
most likely from the contribution of disordered unidentified solvent molecules 
and/or side products of the reaction, as well unresolved disorder of the cluster 
ligands and Br-atoms position. 
The data produced by the SQUEEZE program have not been used in final refinement cycle as the Squeeze operation did not affect the structural parameters.
;
_refine_diff_density_max         2.145
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         4957
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0545
_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^)+(0.1216P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                4053
_reflns_number_total             4957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52218k.txt
_cod_data_source_block           CCSD913441
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               7023803