Expanding Reversible Chalcogenide Binding: Supramolecular Receptors for the Hydroselenide (HSe‒) Anion
Fargher, Hazel; Lau, Nathanael; Zakharov, Lev; Haley, Michael M.; Johnson, Darren; Pluth, Michael D.; Chemical Science  (2019) –; doi:10.1039/C8SC03968B

data_1550254
_publ_section_title
;
 Expanding Reversible Chalcogenide Binding: Supramolecular Receptors for
 the Hydroselenide (HSe--) Anion
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03968B
_journal_year                    2019
_chemical_formula_sum            'C74 H111 N5 O6 Se'
_chemical_formula_weight         1245.63
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-11-08 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.476(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5547(4)
_cell_length_b                   30.3155(13)
_cell_length_c                   26.1228(10)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.55
_cell_measurement_theta_min      2.92
_cell_volume                     7566.4(5)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SAPEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49726
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        66.728
_diffrn_reflns_theta_max         66.728
_diffrn_reflns_theta_min         2.233
_diffrn_source                   'Incoatec I\mMS'
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             2688
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF Ether'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
In the crystal there are two solvent molecule, (CH2CH3)2O
42 electrons). On of them is highly disordered and was treated
by SQUEEZE. 
;
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         13148
_refine_ls_number_restraints     647
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0921
_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^)+(0.1046P)^2^+19.7943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2381
_refine_ls_wR_factor_ref         0.2492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9893
_reflns_number_total             13148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03968b2.cif
_cod_data_source_block           cu_dwj219_0m_a_sqd
_cod_database_code               1550254
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.801
_shelx_estimated_absorpt_t_max   0.979
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              12587