The complicating role of pnictogen bond formation in the solution-phase and solid-state structures of the heavier pnictogen atranes.
Moaven, Shiva; Villanueva, Olivia; Unruh, Daniel K.; Cozzolino, Anthony Frank; Dalton Transactions  (2022) –; doi:10.1039/D2DT01377K

data_7710675
_publ_section_title
;
 The complicating role of pnictogen bond formation in the solution-phase
 and solid-state structures of the heavier pnictogen atranes.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01377K
_journal_year                    2022
_chemical_formula_sum            'C27 H54 N3 O9 Sb3'
_chemical_formula_weight         929.98
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-09-10T09:52:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2022-04-26 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                118.198(6)
_cell_angle_beta                 107.187(6)
_cell_angle_gamma                101.120(4)
_cell_formula_units_Z            2
_cell_length_a                   12.661(3)
_cell_length_b                   13.388(4)
_cell_length_c                   13.591(6)
_cell_measurement_reflns_used    4835
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.78
_cell_measurement_theta_min      2.62
_cell_volume                     1782.0(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.545
_diffrn_reflns_theta_min         1.901
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6622
_refine_ls_number_restraints     387
_refine_ls_restrained_S_all      0.94
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0
_reflns_number_gt                4606
_reflns_number_total             6622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01377k3.cif
_cod_data_source_block           Sb-2
_cod_original_cell_volume        1781.9(10)
_cod_database_code               7710675
_shelx_estimated_absorpt_t_min   0.828
_shelx_estimated_absorpt_t_max   0.966
_shelx_res_checksum              30207
_shelx_hkl_checksum              99761