Cation-translocation based isomerism offers a tool for the expansion of compressed helicates.
Mevissen, Christian; Sommer, David; Vasanthakumar, Sabarina; Truong, Khai-Nghi; Rissanen, Kari; Albrecht, Markus; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9372–9375; doi:10.1039/d1dt01707a

data_7707641
_publ_section_title
;
 Cation-translocation based isomerism offers a tool for the expansion of
 compressed helicates.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9372
_journal_page_last               9375
_journal_paper_doi               10.1039/d1dt01707a
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C72 H81 Li3 Na O37.50 Ti2, 2(C3 H7 N O), H O0.50'
_chemical_formula_sum            'C78 H96 Li3 N2 Na O40 Ti2'
_chemical_formula_weight         1841.17
_chemical_name_systematic        Na[Li3(1)3Ti2]
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-03-11 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.797(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6785(2)
_cell_length_b                   40.9426(5)
_cell_length_c                   14.4762(2)
_cell_measurement_reflns_used    23814
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      75.9030
_cell_measurement_theta_min      3.3000
_cell_volume                     8283.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            77475
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.994
_diffrn_reflns_theta_min         2.158
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.537
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration 
over a multifaceted crystal model.
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 4286 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.094(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         15371
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+4.0271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1880
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                12018
_reflns_number_total             15371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01707a2.cif
_cod_data_source_block           Na[Li3(1)3Ti2]
_cod_depositor_comments
'Adding full bibliography for 7707641--7707642.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7707641
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.593
_shelx_estimated_absorpt_t_max   0.905
_oxdiff_exptl_absorpt_empirical_full_min 0.815
_oxdiff_exptl_absorpt_empirical_full_max 1.251
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              66602