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_7705927
_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_formula_moiety         'C34 H46 N2 O10 P2 W2'
_chemical_formula_sum            'C34 H46 N2 O10 P2 W2'
_chemical_formula_weight         1072.37
_chemical_name_systematic        PJ-237
_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   mixed
_audit_creation_date             2019-04-17
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-05-29 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                78.659(4)
_cell_angle_beta                 82.857(3)
_cell_angle_gamma                62.420(4)
_cell_formula_units_Z            2
_cell_length_a                   11.5880(5)
_cell_length_b                   11.8529(5)
_cell_length_c                   16.5434(7)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.39
_cell_measurement_theta_min      2.39
_cell_volume                     1973.28(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56984
_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         25.248
_diffrn_reflns_theta_min         1.963
_exptl_absorpt_coefficient_mu    5.960
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4373
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1704 before and 0.0989 after correction. The Ratio of minimum to maximum transmission is 0.5864. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_description       needle
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         8.197
_refine_diff_density_min         -2.636
_refine_diff_density_rms         0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7150
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0842
_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^)+(0.1005P)^2^+74.5534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5761
_reflns_number_total             7150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03884a2.cif
_cod_data_source_block           5802
_cod_depositor_comments
'Adding full bibliography for 7705926--7705927.cif.'
_cod_database_code               7705927
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.587
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
2. Rigid bond restraints
 C2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C19, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C18, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C18, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
O9 \\sim C33: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
O3 \\sim C15: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C33) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(C33) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(C20) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4.a Ternary CH refined with riding coordinates:
 C1(H1A), C7(H7), C18(H18), C24(H24)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B),
  C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B)
;
_shelx_res_checksum              26841
_olex2_submission_special_instructions 'No special instructions were received'