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_7711899
_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         'C45 H48 B Br Cl2 N6 O P2 Pd W, 3(C H2 Cl2)'
_chemical_formula_sum            'C48 H54 B Br Cl8 N6 O P2 Pd W'
_chemical_formula_weight         1457.48
_chemical_name_systematic
'Carbonyl-bromido-hydrido{tris(3,4,5-trimethylpyrazolyl)borato}-tungsten(II) {\m-\h2-\k2-bis(diphenylphosphanylethyne)}-palladiumdichloride'
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-08-18 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.629(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3742(16)
_cell_length_b                   16.4883(18)
_cell_length_c                   21.753(2)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.40
_cell_measurement_theta_min      2.80
_cell_volume                     5512.0(10)
_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, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_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  0.0684
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            141896
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         3.073
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.625
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.4985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       plate
_exptl_crystal_F_000             2872
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / n-pentane'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.638
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         19918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0248P)^2^+10.0420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15751
_reflns_number_total             19918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02794a2.cif
_cod_data_source_block           av_fhbrwpppd
_cod_depositor_comments
'Adding full bibliography for 7711895--7711909.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7711899
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.517
_shelx_estimated_absorpt_t_max   0.899
_shelx_res_checksum              43388