Synthesis, structure and properties of the manganese-doped polyoxotitanate cage [Ti18MnO30(OEt)20(MnPhen)3] (Phen = 1,10-phenanthroline).
Li, Ning; Matthews, Peter D.; Leung, Jane J.; King, Timothy C.; Wood, Paul T.; Luo, He-Kuan; Wright, Dominic S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19090–19096; doi:10.1039/c5dt03617h

data_7036881
_publ_section_title
;
 Synthesis, structure and properties of the manganese-doped
 polyoxotitanate cage [Ti18MnO30(OEt)20(MnPhen)3] (Phen =
 1,10-phenanthroline).
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19090
_journal_page_last               19096
_journal_paper_doi               10.1039/c5dt03617h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C76 H124 Mn4 N6 O50 Ti18'
_chemical_formula_sum            'C76 H124 Mn4 N6 O50 Ti18'
_chemical_formula_weight         3003.76
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2015-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.723(3)
_cell_length_b                   23.832(5)
_cell_length_c                   31.971(6)
_cell_measurement_reflns_used    150352
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.02
_cell_volume                     11904(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
; 
HKL Denzo and Scalepack (Otwinowski & Minor 1997) 
;
_computing_publication_material  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            61565
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.040
_diffrn_reflns_theta_max         25.040
_diffrn_reflns_theta_min         3.516
_exptl_absorpt_coefficient_mu    1.621
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
multi-scan from symmetry-related measurements 
Sortav (Blessing 1995) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             6072
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.460
_exptl_crystal_size_min          0.460
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1317
_refine_ls_number_reflns         19760
_refine_ls_number_restraints     582
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1522
_refine_ls_R_factor_gt           0.0987
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1492P)^2^+66.1369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2706
_refine_ls_wR_factor_ref         0.3139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12059
_reflns_number_total             19760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03617h2.cif
_cod_data_source_block           dw1513
_cod_depositor_comments          'Adding full bibliography for 7036881.cif.'
_cod_original_cell_volume        11905(4)
_cod_database_code               7036881
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.523
_shelx_estimated_absorpt_t_max   0.523
_shelx_res_checksum              5911