Tuning the potential of redox-active diphosphine ligands based on the alkyne complexes [Tp*W(CO)L{η<sup>2</sup>-C<sub>2</sub>(PPh<sub>2</sub>)<sub>2</sub>}].
Ludwig, Stephan; Hamann, Friederike M.; Helmdach, Kai; Villinger, Alexander; Seidel, Wolfram W.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 326–337; doi:10.1039/d2dt02794a

data_7711909
_publ_section_title
;
 Tuning the potential of redox-active diphosphine ligands based on the
 alkyne complexes
 [Tp*W(CO)L{&#x3b7;<sup>2</sup>-C<sub>2</sub>(PPh<sub>2</sub>)<sub>2</sub>}].
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              326
_journal_page_last               337
_journal_paper_doi               10.1039/d2dt02794a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety
'C46 H48 B F3 N6 O4.157 P2 S W, 0.333(C5 H12), 1.333(C4 H8 O)'
_chemical_formula_sum            'C53 H62.67 B F3 N6 O5.49 P2 S W'
_chemical_formula_weight         1217.20
_chemical_name_systematic
\h2-{Bis(diphenylphosphanyl)ethyne}-carbonyl-hydrido{tris(3,4,5-trimethylpyrazolyl)borato}-\k1-trifluoromethansulfonate-tungsten(II)
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-11-02 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                98.383(3)
_cell_angle_beta                 104.409(4)
_cell_angle_gamma                93.786(3)
_cell_formula_units_Z            6
_cell_length_a                   15.1651(9)
_cell_length_b                   21.3862(12)
_cell_length_c                   25.7029(16)
_cell_measurement_reflns_used    9745
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.41
_cell_volume                     7941.9(8)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex Kappa-II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0921
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            212014
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.231
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.346
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             3711
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofurane / n-pentane'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
The unit cell contains about eight THF and two n-pentane molecules 
which have been treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 22035 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3610
_refine_ls_number_reflns         69859
_refine_ls_number_restraints     1449
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.956
_reflns_Friedel_fraction_max     0.916
_reflns_number_gt                56838
_reflns_number_total             69859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02794a2.cif
_cod_data_source_block           is_sl364
_cod_depositor_comments
'Adding full bibliography for 7711895--7711909.cif.'
_cod_database_code               7711909
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.664
_shelx_estimated_absorpt_t_max   0.835
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              11453
_shelx_fab_checksum              21379