Thiazoyl phosphines. Design, reactivity, and complexation.
Zablocka, Maria; Oshovsky, Gennady; Duhayon, Carine; Ladeira, Sonia; Caminade, Anne-Marie; Mignani, Serge; Majoral, Jean-Pierre; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9695–9703; doi:10.1039/c6dt01106c

data_7039261
_publ_section_title
;
 Thiazoyl phosphines. Design, reactivity, and complexation.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9695
_journal_page_last               9703
_journal_paper_doi               10.1039/c6dt01106c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 H11 N4 P S2, 2(C H4 O)'
_chemical_formula_sum            'C14 H19 N4 O2 P S2'
_chemical_formula_weight         370.44
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2016-05-02 deposited with the CCDC.
2016-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                95.209(7)
_cell_angle_beta                 89.257(6)
_cell_angle_gamma                109.426(7)
_cell_formula_units_Z            2
_cell_length_a                   5.8693(4)
_cell_length_b                   8.7664(8)
_cell_length_c                   18.5843(13)
_cell_measurement_reflns_used    2123
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     897.90(13)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8299
_diffrn_reflns_theta_full        25.808
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         3.453
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.32
_refine_ls_extinction_coef       206(14)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3557
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.0002290
_refine_ls_shift/su_mean         0.0000223
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.840 0.392 0.410 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0489
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0437
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                3799
_reflns_number_total             4732
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0371
_oxford_reflns_number_all        4724
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c6dt01106c1.cif
_cod_data_source_block           cpd11
_cod_depositor_comments
'Adding full bibliography for 7039261--7039268.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C14 H19 N4 O2 P1 S2'
_cod_database_code               7039261