Synthesis and reactivity of NHC-coordinated phosphinidene oxide.
Dhara, Debabrata; Pal, Pradeep Kumar; Dolai, Ramapada; Chrysochos, Nicolas; Rawat, Hemant; Elvers, Benedict J.; Krummenacher, Ivo; Braunschweig, Holger; Schulzke, Carola; Chandrasekhar, Vadapalli; Priyakumar, U. Deva; Jana, Anukul; Chemical communications (Cambridge, England) 57 (2021) 9546–9549; doi:10.1039/d1cc04421d

data_7128887
_publ_section_title
;
 Synthesis and reactivity of NHC-coordinated phosphinidene oxide.
;
_journal_issue                   75
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9546
_journal_page_last               9549
_journal_paper_doi               10.1039/d1cc04421d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C20 H18 Cl2 N2 Ru S2, C3 H6 O'
_chemical_formula_sum            'C23 H24 Cl2 N2 O Ru S2'
_chemical_formula_weight         580.53
_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
_audit_block_doi                 10.5517/ccdc.csd.cc24r7nt
_audit_creation_date             2019-08-08
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-05 deposited with the CCDC.	2021-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                70.756(5)
_cell_angle_beta                 84.677(5)
_cell_angle_gamma                67.243(5)
_cell_formula_units_Z            2
_cell_length_a                   9.5459(14)
_cell_length_b                   11.7033(17)
_cell_length_c                   12.1756(17)
_cell_measurement_reflns_used    4790
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.31
_cell_volume                     1183.3(3)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex II'
_diffrn_measurement_method       'CCD Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_min         2.415
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0544 before and 0.0481 after correction.
The Ratio of minimum to maximum transmission is 0.9176.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       lath-like
_exptl_crystal_F_000             588
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone and DiethylEther'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.827
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0371P)^2^+2.0629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3504
_reflns_number_total             4816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04421d2.cif
_cod_data_source_block           dal193
_cod_depositor_comments
'Adding full bibliography for 7128887--7128892.cif.'
_cod_database_code               7128887
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.881
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C25(H25), C23(H23), C3(H3), C24(H24), C6(H6), C5(H5), C15(H15),
 C12(H12), C4(H4), C14(H14), C13(H13)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C17(H17A,H17B,H17C), C1A(H1AA,H1AB,H1AC), C3A(H3AA,H3AB,
 H3AC)
;
_shelx_res_checksum              34141
_shelx_hkl_checksum              39888
_olex2_submission_special_instructions 'No special instructions were received'