Triphosphiranes as Phosphinidene-Transfer Agents – Synthesis of Regular and Chelating NHC Phosphinidene Adducts
Siewert, Jan-Erik; Schumann, André; Wellnitz, Tim; Dankert, Fabian; Hering-Junghans, Christian; Dalton Transactions  (2023) –; doi:10.1039/D3DT02690F

data_7714101
_publ_section_title
;
 Triphosphiranes as Phosphinidene-Transfer Agents -- Synthesis of Regular
 and Chelating NHC Phosphinidene Adducts
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02690F
_journal_year                    2023
_chemical_formula_moiety
'(C36 H44 Ga I2 N4 P2)+, (Ga I4)-, 2.06 (CH2 Cl2)'
_chemical_formula_sum            'C38.06 H48.11 Cl4.11 Ga2 I6 N4 P2'
_chemical_formula_weight         1670.14
_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_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                74.3750(10)
_cell_angle_beta                 74.2030(10)
_cell_angle_gamma                82.8170(10)
_cell_formula_units_Z            4
_cell_length_a                   14.9427(3)
_cell_length_b                   17.0844(3)
_cell_length_c                   23.0489(4)
_cell_measurement_reflns_used    73082
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.50
_cell_volume                     5444.13(18)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            73082
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         1.732
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    4.683
_exptl_absorpt_correction_T_max  0.4260
_exptl_absorpt_correction_T_min  0.2522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_description       plank
_exptl_crystal_F_000             3137
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.026
_refine_diff_density_max         2.083
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         22576
_refine_ls_number_restraints     327
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+8.0462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18054
_reflns_number_total             22576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02690f2.cif
_cod_data_source_block           ks1562_cmpd7
_cod_database_code               7714101
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.735
_shelx_estimated_absorpt_t_max   0.888
_shelx_res_checksum              69923