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_1557870
_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            'C26 H25 Cl8 N O4 Sb'
_chemical_formula_weight         820.82
_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-2014/7
_audit_update_record
;
2019-08-05 deposited with the CCDC.	2020-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.070(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6398(8)
_cell_length_b                   18.4868(13)
_cell_length_c                   16.2027(11)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.73
_cell_measurement_theta_min      2.15
_cell_volume                     3295.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_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  0.0246
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15559
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.729
_diffrn_reflns_theta_max         24.729
_diffrn_reflns_theta_min         1.727
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  0.534
_exptl_absorpt_correction_T_min  0.444
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.794
_exptl_crystal_size_mid          0.727
_exptl_crystal_size_min          0.473
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+5.1831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5196
_reflns_number_total             5614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc00002g2.cif
_cod_data_source_block           3Me_a
_cod_depositor_comments
;Adding full bibliography for 1557869--1557876.cif.

 Adding full bibliography for 1557869--1557876.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1557870
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.379
_shelx_estimated_absorpt_t_max   0.534
_shelx_res_checksum              15708