Synthesis of free and ligated 1,2-thiaphosphetanes ‒ expanding the pool of strained P-ligands
Kyri, Andreas Wolfgang; Gleim, Florian; Becker, David; Schnakenburg, Gregor; Espinosa Ferao, Arturo; Streubel, Rainer; Chemical Communications  (2019) –; doi:10.1039/C8CC09892A

data_7122872
_publ_section_title
;
 Synthesis of free and ligated 1,2-thiaphosphetanes -- expanding the pool
 of strained P-ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09892A
_journal_year                    2019
_chemical_formula_moiety         'C27 H21 Cr O5 P S'
_chemical_formula_sum            'C27 H21 Cr O5 P S'
_chemical_formula_weight         540.47
_chemical_name_systematic        DB-14
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-12-06 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.337(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9943(5)
_cell_length_b                   13.8498(5)
_cell_length_c                   15.1345(7)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.28
_cell_volume                     2456.07(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46113
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.015
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6459
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1242 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.8657. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5905
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0273P)^2^+2.6584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4951
_reflns_number_total             5905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09892a2.cif
_cod_data_source_block           5561f
_cod_database_code               7122872
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.892
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{S, C2S}
{S1S, C2}
3. Uiso/Uaniso restraints and constraints
Uanis(C1S) \\sim Ueq, Uanis(C3S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(S) = Uanis(C2S)
Uanis(S1S) = Uanis(C2)
4. Rigid body (RIGU) restrains
 S, C2S, S1S, C2, C1S, C1, C3S, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=1-FVAR(1)
 Sof(S)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
 Sof(C1S)=Sof(H1S)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=1-FVAR(2)
 Sof(C1)=Sof(H1)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1S(H1S), C1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C2(H2A,H2B)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
6.d Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              76141
_olex2_submission_special_instructions 'No special instructions were received'