Stabilizing an exotic dianionic tetrazine bridge in a Ln<sub>2</sub> metallocene.
Mavragani, Niki; Kitos, Alexandros A.; Mansikkamäki, Akseli; Murugesu, Muralee; Chemical science 15 (2024) 16234–16242; doi:10.1039/d4sc03734k

data_1572539
_publ_section_title
;
 Stabilizing an exotic dianionic tetrazine bridge in a Ln<sub>2</sub>
 metallocene.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              16234
_journal_page_last               16242
_journal_paper_doi               10.1039/d4sc03734k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C50 H78 Gd2 N4 O2, 2(C4 H8 O)'
_chemical_formula_sum            'C58 H94 Gd2 N4 O4'
_chemical_formula_weight         1225.87
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-05-29 deposited with the CCDC.	2024-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3222(4)
_cell_length_b                   13.3614(3)
_cell_length_c                   14.9998(4)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.43
_cell_volume                     2859.61(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            64834
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.611
_diffrn_reflns_theta_min         1.886
_exptl_absorpt_coefficient_mu    2.345
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            violet
_exptl_crystal_colour_modifier   pale
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1260
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.737
_refine_diff_density_min         -1.923
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6637
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0520P)^2^+16.8278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5618
_reflns_number_total             6637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03734k2.cif
_cod_data_source_block           Gd2tz
_cod_depositor_comments
'Adding full bibliography for 1572537--1572539.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1572539
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.560
_shelx_estimated_absorpt_t_max   0.872
_shelx_res_checksum              74312