Synthesis, structure and paramagnetic NMR analysis of a series of lanthanide-containing [LnTi6O3(O(i)Pr)9(salicylate)6] cages.
Li, Ning; García-Rodríguez, Raúl; Matthews, Peter D.; Luo, He-Kuan; Wright, Dominic S.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4287–4295; doi:10.1039/c7dt00049a

data_7042225
_publ_section_title
;
 Synthesis, structure and paramagnetic NMR analysis of a series of
 lanthanide-containing [LnTi6O3(O(i)Pr)9(salicylate)6] cages.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4287
_journal_page_last               4295
_journal_paper_doi               10.1039/c7dt00049a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C69 H87 Nd O30 Ti6'
_chemical_formula_sum            'C69 H87 Nd O30 Ti6'
_chemical_formula_weight         1828.02
_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_Hall           'P -6'
_space_group_name_H-M_alt        'P -6'
_symmetry_space_group_name_Hall  'P -6'
_symmetry_space_group_name_H-M   'P -6'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.9289(4)
_cell_length_b                   14.9289(4)
_cell_length_c                   23.5597(7)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      61.6
_cell_measurement_theta_min      3.4
_cell_volume                     4547.3(2)
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_collection       'Bruker software package, narrow-frames'
_computing_data_reduction
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26755
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        61.253
_diffrn_reflns_theta_max         61.253
_diffrn_reflns_theta_min         3.418
_exptl_absorpt_coefficient_mu    9.130
_exptl_absorpt_correction_T_max  0.407
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (SADABS) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             1866
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   1.00
_exptl_transmission_factor_min   0.792
_refine_diff_density_max         4.636
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Flack x determined using 1864 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4755
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0603
_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^)+(0.1167P)^2^+0.5826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1729
_reflns_Friedel_coverage         0.983
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4263
_reflns_number_total             4755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00049a2.cif
_cod_data_source_block           nd_b
_cod_depositor_comments
'Adding full bibliography for 7042216--7042227.cif.'
_cod_original_cell_volume        4547.3(3)
_cod_database_code               7042225
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.341
_shelx_estimated_absorpt_t_max   0.407
_shelx_res_checksum              97813