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_7706521
_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         'C28 H12 F5 O2 P S2, 0.5(C H Cl3)'
_chemical_formula_sum            'C28.5 H12.5 Cl1.5 F5 O2 P S2'
_chemical_formula_weight         630.18
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2020-11-13 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                108.018(5)
_cell_angle_beta                 106.995(6)
_cell_angle_gamma                93.965(6)
_cell_formula_units_Z            4
_cell_length_a                   11.358(2)
_cell_length_b                   14.516(2)
_cell_length_c                   16.549(3)
_cell_measurement_reflns_used    9091
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      34.95
_cell_measurement_theta_min      2.60
_cell_volume                     2442.9(7)
_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      173.00
_diffrn_measured_fraction_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.862
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14683
_diffrn_reflns_point_group_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.676
_diffrn_reflns_theta_min         2.355
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       yellow
_exptl_crystal_F_000             1169
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         7920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+8.3879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5548
_reflns_number_total             7920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00062d2.cif
_cod_data_source_block           compounddcopy
_cod_depositor_comments
;
Adding full bibliography for 7706518--7706522.cif.

2024-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2442.8(7)
_cod_original_formula_moiety     '2(C28 H12 F5 O2 P S2), (C H Cl3)'
_cod_original_formula_sum        'C57 H25 Cl3 F10 O4 P2 S4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1260.36
_cod_database_code               7706521
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C028(H028)
2.b Aromatic/amide H refined with riding coordinates:
 C00V(H00V), C00W(H00W), C010(H010), C014(H014), C015(H015), C018(H018),
 C01D(H01D), C01E(H01E), C01K(H01K), C01O(H01O), C01P(H01P), C01Q(H01Q),
 C01R(H01R), C01S(H01S), C01V(H01V), C01Z(H01Z), C020(H020), C021(H021),
 C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C027(H027)
;
_olex2_submission_special_instructions 'No special instructions were received'