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_7711900
_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         'C33 H39 B Br N6 O P W, C5 H12'
_chemical_formula_sum            'C38 H51 B Br N6 O P W'
_chemical_formula_weight         913.38
_chemical_name_systematic
\h2-{Bis(diphenylphosphanyl)ethyne}-bromido-carbonyl-hydrido{tris(3,4,5-trimethylpyrazolyl)borato}-tungsten(II)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2022-08-24 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5493(5)
_cell_length_b                   10.3618(2)
_cell_length_c                   22.0549(6)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.09
_cell_measurement_theta_min      2.50
_cell_volume                     3781.99(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury 2016 '
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41114
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.000
_diffrn_reflns_theta_min         2.319
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    4.192
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / n-pentane'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_platon_squeeze_details
;
The unit cell contains one n-pentane molecule which has been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON. This was removed from the model, but included 
in the empirical formula.
;
_refine_diff_density_max         1.855
_refine_diff_density_min         -1.908
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         11985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0236P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9887
_reflns_number_total             11985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02794a2.cif
_cod_data_source_block           kh_sl285
_cod_depositor_comments
'Adding full bibliography for 7711895--7711909.cif.'
_cod_database_code               7711900
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
_shelx_res_checksum              72043
_shelx_fab_checksum              29509