Structure-reactivity studies on hypervalent square-pyramidal dithieno[3,2-b:2',3'-d]phospholes.
Asok, Nayanthara; Gaffen, Joshua R.; Pradhan, Ekadashi; Zeng, Tao; Baumgartner, Thomas; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2243–2252; doi:10.1039/d1dt00062d

data_7706520
_publ_section_title
;
 Structure-reactivity studies on hypervalent square-pyramidal
 dithieno[3,2-b:2',3'-d]phospholes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2243
_journal_page_last               2252
_journal_paper_doi               10.1039/d1dt00062d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C14 H9 O P S2, C6 H2 Cl4 O2'
_chemical_formula_sum            'C20 H11 Cl4 O3 P S2'
_chemical_formula_weight         536.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_date             2020-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-13 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                116.199(3)
_cell_angle_beta                 104.509(3)
_cell_angle_gamma                91.081(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4476(7)
_cell_length_b                   12.5959(13)
_cell_length_c                   13.2064(13)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.86
_cell_volume                     1064.13(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46942
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         2.857
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         6527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0321P)^2^+0.5391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5723
_reflns_number_total             6527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00062d2.cif
_cod_data_source_block           na_p3_27a_0m_a
_cod_depositor_comments
'Adding full bibliography for 7706518--7706522.cif.'
_cod_original_cell_volume        1064.13(18)
_cod_database_code               7706520
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00J(H00J), C00M(H00M), C00P(H00P), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00U(H00U)
2.b Idealised tetrahedral OH refined as rotating group:
 O009(H009), O00A(H00A)
;
_shelx_res_checksum              50980
_shelx_hkl_checksum              39011
_olex2_submission_special_instructions 'No special instructions were received'