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_7709522
_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_moiety         'C8 H7 N O Se'
_chemical_formula_sum            'C8 H7 N O Se'
_chemical_formula_weight         212.11
_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-2018/3
_audit_update_record
;
2022-02-11 deposited with the CCDC.	2022-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.743(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1882(8)
_cell_length_b                   5.1560(4)
_cell_length_c                   14.7709(11)
_cell_measurement_reflns_used    4379
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.9390
_cell_measurement_theta_min      2.7520
_cell_volume                     850.26(11)
_computing_cell_refinement       'CrysAlis Pro 1.171.41.117a'
_computing_data_collection       'CrysAlis Pro 1.171.41.117a'
_computing_data_reduction        'CrysAlis Pro 1.171.41.117a'
_computing_structure_refinement  'SHELXL 2018/3'
_computing_structure_solution    'SHELXT 2018/2'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku OD Xcalibur E (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4282
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.024
_diffrn_reflns_theta_min         2.215
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.356
_exptl_absorpt_correction_T_max  0.289
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis Pro 1.171.41.117a. Analytical numeric absorption correction using
a multifaceted crystal model based on expressions derived
by R.C. Clark & J.S. Reid. Empirical absorption correction using spherical
harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       prism
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.720
_exptl_crystal_size_mid          0.580
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         4282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0983P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2343
_reflns_number_total             4282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04366h3.cif
_cod_data_source_block           C8H7NOSe
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709522
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.146
_shelx_estimated_absorpt_t_max   0.275
_shelx_res_checksum              26538
_shelx_hkl_checksum              21286