Synthesis and properties of hypervalent electron-rich pentacoordinate nitrogen compounds
Yan, Chenting; Takeshita, Masato; Nakatsuji, Jun-ya; Kurosaki, Akihiro; Sato, Kaoko; Shang, Rong; Nakamoto, Masaaki; Yamamoto, Yohsuke; Adachi, Yohei; Furukawa, Ko; Kishi, Ryohei; Nakano, Masayoshi; Chemical Science 11 (2020) 5082–5088; doi:10.1039/D0SC00002G

data_1557876
_publ_section_title
;
 Synthesis and properties of hypervalent electron-rich pentacoordinate
 nitrogen compounds
;
_journal_issue                   19
_journal_name_full               'Chemical Science'
_journal_page_first              5082
_journal_page_last               5088
_journal_paper_doi               10.1039/D0SC00002G
_journal_volume                  11
_journal_year                    2020
_chemical_formula_sum            'C30 H33 Cl8 N O4 Sb'
_chemical_formula_weight         876.92
_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
_audit_creation_method           SHELXL-2014/5
_audit_update_record
;
2019-08-05 deposited with the CCDC.	2020-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.770(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.156(3)
_cell_length_b                   15.548(3)
_cell_length_c                   19.482(4)
_cell_measurement_reflns_used    1967
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.77
_cell_measurement_theta_min      2.36
_cell_volume                     3681.8(14)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0860
_diffrn_reflns_av_unetI/netI     0.1375
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20884
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         1.676
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_max  0.9732
_exptl_absorpt_correction_T_min  0.7748
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         8431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0312P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4448
_reflns_number_total             8431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc00002g2.cif
_cod_data_source_block           3iPr_a
_cod_depositor_comments
;Adding full bibliography for 1557869--1557876.cif.

 Adding full bibliography for 1557869--1557876.cif.
;
_cod_original_cell_volume        3681.6(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1557876
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.973
_shelxl_version_number           2014/5
_shelx_res_checksum              75152