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_7711905
_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 Cl N6 O P W, 4(C H2 Cl2)'
_chemical_formula_sum            'C37 H47 B Cl9 N6 O P W'
_chemical_formula_weight         1136.48
_chemical_name_systematic
Carbonyl-chlorido-\h2-diphenylphosphanylethyne-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-2014/7
_audit_update_record
;
2022-08-23 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                   16.460(3)
_cell_length_b                   10.3892(18)
_cell_length_c                   22.022(4)
_cell_measurement_reflns_used    9177
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      34.95
_cell_measurement_theta_min      2.70
_cell_volume                     3765.9(12)
_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_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68897
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         3.291
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.794
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.4697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS-2016/2; Sheldrick, 2015)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane / n-pentane'
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_platon_squeeze_details
;
The unit cell contains 16 dichloromethane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON. These were removed from the model, but included 
in the empirical formula.
;
_refine_diff_density_max         1.627
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.028(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         13552
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0251P)^2^+2.4134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12521
_reflns_number_total             13552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02794a2.cif
_cod_data_source_block           is_mr012
_cod_depositor_comments
'Adding full bibliography for 7711895--7711909.cif.'
_cod_original_cell_volume        3765.9(11)
_cod_database_code               7711905
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.280
_shelx_estimated_absorpt_t_max   0.726
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              26623
_shelx_fab_checksum              11642