A case study on the conversion of Li/Cl phosphinidenoid into phosphinidene complexes.
Junker, Philip; Qu, Zheng-Wang; Kalisch, Tim; Schnakenburg, Gregor; Espinosa Ferao, Arturo; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 50 (2021) 739–745; doi:10.1039/d0dt03884a

data_7705926
_publ_section_title
;
 A case study on the conversion of Li/Cl phosphinidenoid into
 phosphinidene complexes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              739
_journal_page_last               745
_journal_paper_doi               10.1039/d0dt03884a
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H10 Cl2 N O5 P W'
_chemical_formula_sum            'C17 H10 Cl2 N O5 P W'
_chemical_formula_weight         593.98
_chemical_name_systematic        PJ-151
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2019-05-29 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.085(5)
_cell_length_b                   13.306(8)
_cell_length_c                   16.740(11)
_cell_measurement_reflns_used    6316
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.43
_cell_volume                     2024(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29500
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.975
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.078
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4745
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1472 before and 0.0821 after correction. The Ratio of minimum to maximum transmission is 0.6361. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.021(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4866
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0161P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4414
_reflns_number_total             4866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03884a2.cif
_cod_data_source_block           5065g
_cod_depositor_comments
'Adding full bibliography for 7705926--7705927.cif.'
_cod_database_code               7705926
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.529
_shelx_estimated_absorpt_t_min   0.362
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.979(9) 0.021(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12)
;
_shelx_res_checksum              65816
_olex2_submission_special_instructions 'No special instructions were received'