Formation and properties of phosphaquinomethane tungsten(0) complexes - isolation and conversion of primary radical coupling products.
Junker, Philip; Villalba Franco, José M; Schnakenburg, Gregor; Nesterov, Vitaly; Boere, René T; Qu, Zheng-Wang; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13544–13548; doi:10.1039/d0dt03089a

data_7705578
_publ_section_title
;
 Formation and properties of phosphaquinomethane tungsten(0) complexes -
 isolation and conversion of primary radical coupling products.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13544
_journal_page_last               13548
_journal_paper_doi               10.1039/d0dt03089a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43 H30 Cl O5 P W, C4 H10 O'
_chemical_formula_sum            'C47 H40 Cl O6 P W'
_chemical_formula_weight         951.06
_chemical_name_systematic        PJ-145
_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     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
;
2020-08-18 deposited with the CCDC.	2020-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                80.151(3)
_cell_angle_beta                 84.789(3)
_cell_angle_gamma                82.795(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9641(8)
_cell_length_b                   13.1791(8)
_cell_length_c                   14.2135(10)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      2.29
_cell_volume                     2002.5(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      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55667
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.916
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.041
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5693
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1183 before and 0.0580 after correction. The Ratio of minimum to maximum transmission is 0.7632. 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    1.577
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         9658
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+1.5311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9036
_reflns_number_total             9658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03089a2.cif
_cod_data_source_block           5066f
_cod_depositor_comments          'Adding full bibliography for 7705578.cif.'
_cod_database_code               7705578
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.642
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Cl, P
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C7(H7)
3.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C46(H46A,H46B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
3.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              29589
_olex2_submission_special_instructions 'No special instructions were received'