Synthesis and reactivity of propionitrilium derivatives of cobalt and iron bis(dicarbollides)
Bogdanova, Ekaterina V.; Stogniy, Marina Yu.; Chekulaeva, Lyubov A.; Anisimov, Aleksei A.; Suponitsky, Kyrill Yu.; Sivaev, Igor B.; Grin, Mikhail A.; Mironov, Andrey F.; Bregadze, Vladimir I.; New Journal of Chemistry 44 (2020) 15836–15848; doi:10.1039/D0NJ03017A

data_7059903
_publ_section_title
;
 Synthesis and reactivity of propionitrilium derivatives of cobalt and
 iron bis(dicarbollides)
;
_journal_issue                   37
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15836
_journal_page_last               15848
_journal_paper_doi               10.1039/D0NJ03017A
_journal_volume                  44
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H34 B18 Co N O, C3 H6 O'
_chemical_formula_sum            'C13 H40 B18 Co N O2'
_chemical_formula_weight         495.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2020-06-03 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1302(3)
_cell_length_b                   16.2436(5)
_cell_length_c                   16.2491(5)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.37
_cell_volume                     2673.80(14)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material
'SHELXL-2014/6 (Sheldrick, 2014) and PLATON (Spek, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72431
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.847
_diffrn_reflns_theta_min         1.773
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker,2014/5)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 2636 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         7626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0473P)^2^+0.1921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                6586
_reflns_number_total             7626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03017a1.cif
_cod_data_source_block           st3
_cod_depositor_comments          'Adding full bibliography for 7059903.cif.'
_cod_original_cell_volume        2673.81(14)
_cod_database_code               7059903
_shelxl_version_number           2014/6
_shelx_res_checksum              98457