Crystalline, room-temperature stable phosphine-SO<sub>2</sub> adducts: generation of sulfur monoxide from sulfur dioxide.
Buß, Florenz; Rotering, Philipp; Mück-Lichtenfeld, Christian; Dielmann, Fabian; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10420–10424; doi:10.1039/c8dt01484a

data_7046857
_publ_section_title
;
 Crystalline, room-temperature stable phosphine-SO<sub>2</sub> adducts:
 generation of sulfur monoxide from sulfur dioxide.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10420
_journal_page_last               10424
_journal_paper_doi               10.1039/c8dt01484a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C33 H60 N9 O2 P1 S1'
_chemical_formula_sum            'C33 H60 N9 O2 P S'
_chemical_formula_weight         677.93
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_audit_update_record
;
2018-04-15 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   24.5396(3)
_cell_length_b                   24.5396(3)
_cell_length_c                   24.5396(3)
_cell_measurement_reflns_used    9462
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.192
_cell_measurement_theta_min      3.321
_cell_volume                     14777.6(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41644
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.359
_diffrn_reflns_theta_min         3.713
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0861 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.9085.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       block
_exptl_crystal_F_000             5888
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 903 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0391P)^2^+14.7170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                2210
_reflns_number_total             2505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01484a2.cif
_cod_data_source_block           i-43d_pre2
_cod_depositor_comments
'Adding full bibliography for 7046856--7046859.cif.'
_cod_original_cell_volume        14777.6(5)
_cod_database_code               7046857
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Sof: O1(0.6667)
 Fixed Uiso: H4A(0.061) H4B(0.061) H4C(0.061) H5A(0.063) H5B(0.063) H5C(0.063)
 H6(0.032) H7A(0.058) H7B(0.058) H7C(0.058) H8A(0.053) H8B(0.053) H8C(0.053)
 H9(0.034) H10A(0.07) H10B(0.07) H10C(0.07) H11A(0.057) H11B(0.057) H11C(0.057)
 Fixed X: H4A(0.2771) H4B(0.2825) H4C(0.2803) H5A(0.4041) H5B(0.3417)
 H5C(0.3858) H6(0.3952) H7A(0.2928) H7B(0.3127) H7C(0.3437) H8A(0.3641)
 H8B(0.3342) H8C(0.3039) H9(0.523) H10A(0.4898) H10B(0.5353) H10C(0.4721)
 H11A(0.4889) H11B(0.5505) H11C(0.509)
 Fixed Y: H4A(0.5533) H4B(0.6052) H4C(0.6131) H5A(0.6398) H5B(0.622)
 H5C(0.579) H6(0.5531) H7A(0.5194) H7B(0.5088) H7C(0.4803) H8A(0.6448)
 H8B(0.6115) H8C(0.6217) H9(0.5676) H10A(0.5067) H10B(0.5448) H10C(0.5559)
 H11A(0.6546) H11B(0.6405) H11C(0.6623)
 Fixed Z: H4A(-0.0986) H4B(-0.1377) H4C(-0.073) H5A(-0.2072) H5B(-0.2007) H5C(-
 0.2221) H6(0.026) H7A(-0.0165) H7B(0.0447) H7C(-0.0051) H8A(0.0171)
 H8B(0.0645) H8C(0.0076) H9(-0.119) H10A(-0.1836) H10B(-0.2106) H10C(-0.2225)
 H11A(-0.1873) H11B(-0.171) H11C(-0.1257)
;
_shelx_res_checksum              95345