Synthesis of a xanthene-based macrocyclic imine ligand and two-step planarization by metalation with Ni<sup>2+</sup> and Na<sup/>.
Akine, Shigehisa; Nakano, Masato; Sakata, Yoko; Tsuzuki, Seiji; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11573–11580; doi:10.1039/d5dt01183c

data_7719066
_publ_section_title
;
 Synthesis of a xanthene-based macrocyclic imine ligand and two-step
 planarization by metalation with Ni<sup>2+</sup> and Na<sup/>.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11573
_journal_page_last               11580
_journal_paper_doi               10.1039/d5dt01183c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         C53H50F3N4NaNi2O12S4
_chemical_formula_sum            'C53 H50 F3 N4 Na Ni2 O12 S4'
_chemical_formula_weight         1260.62
_chemical_name_common            '[LNi2Na(Me2SO)2](CF3SO3)(Me2SO)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2025-05-05 deposited with the CCDC.	2025-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.796(2)
_cell_angle_gamma                90
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_cell_length_b                   9.1083(3)
_cell_length_c                   26.4196(9)
_cell_measurement_reflns_used    19130
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.363
_cell_measurement_theta_min      3.395
_cell_volume                     2541.88(15)
_computing_cell_refinement       'APEX2 v2014.11 (Bruker AXS)'
_computing_data_collection
'Bruker Instrument Service V4.2.2 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
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_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            19130
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.363
_diffrn_reflns_theta_min         3.395
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    3.239
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1300
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMSO/MeOH/Et2O'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.58(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         7753
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0354P)^2^+0.2083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6791
_reflns_number_total             7753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01183c2.cif
_cod_data_source_block           nak004
_cod_depositor_comments
'Adding full bibliography for 7719065--7719067.cif.'
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7719066
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              35344
_shelx_hkl_checksum              19702