Cycloaddition of isoselenocyanates to sodium and magnesium metallacycles
Dodonov, Vladimir Alekseevich; Kushnerova, Olga A.; Rumyantcev, Roman V.; Novikov, Alexander S.; Osmanov, Vladimir K.; Fedushkin, Igor Leonidovich; Dalton Transactions  (2022) –; doi:10.1039/D1DT04366H

data_7709525
_publ_section_title
;
 Cycloaddition of isoselenocyanates to sodium and magnesium metallacycles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04366H
_journal_year                    2022
_chemical_formula_sum            'C60 H79 Mg N3 O4 Se'
_chemical_formula_weight         1009.53
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.274(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9342(9)
_cell_length_b                   24.5967(17)
_cell_length_c                   17.0576(12)
_cell_measurement_reflns_used    9725
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.80
_cell_measurement_theta_min      2.39
_cell_volume                     5417.8(7)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX3
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXL-2018/3
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67800
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.043
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_correction_T_min  0.6233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.384
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         11079
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0754
_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^)+(0.0979P)^2^+2.6883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7543
_reflns_number_total             11079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04366h3.cif
_cod_data_source_block           13
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709525
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.789
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              94203
_shelx_hkl_checksum              70682