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_7711897
_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 Cl2 N7 O P2 Pd W, (C2 H3 N), (C H2 Cl2)'
_chemical_formula_sum            'C48.8 H52.6 B Cl2.6 N8 O P2 Pd W'
_chemical_formula_weight         1222.36
_chemical_name_systematic
'Carbonyl-cyanido-hydrido{tris(3,4,5-trimethylpyrazolyl)borato}-tungsten(II) {\m-\h2-\k2-bis(diphenylphosphanylethyne)}-palladiumdichloride'
_chemical_properties_physical    Moisture-sensitive
_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
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2022-08-18 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                92.352(4)
_cell_angle_beta                 92.815(4)
_cell_angle_gamma                119.240(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5408(11)
_cell_length_b                   13.7166(11)
_cell_length_c                   16.4682(12)
_cell_measurement_reflns_used    9771
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.48
_cell_volume                     2658.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury 2016'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85217
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         2.126
_exptl_absorpt_coefficient_mu    2.805
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       plate
_exptl_crystal_F_000             1268
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile / dichloromethane'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
The unit cell contains 2 CH2Cl2 molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.418
_refine_diff_density_min         -2.066
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         19133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0404P)^2^+8.4770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15229
_reflns_number_total             19133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02794a2.cif
_cod_data_source_block           kh_sl141
_cod_depositor_comments
'Adding full bibliography for 7711895--7711909.cif.'
_cod_original_formula_sum        'C48.80 H52.60 B Cl2.60 N8 O P2 Pd W'
_cod_database_code               7711897
_shelx_estimated_absorpt_t_min   0.767
_shelx_estimated_absorpt_t_max   0.921
_shelxl_version_number           2014-3
_shelx_res_checksum              65821
_shelx_fab_checksum              15957