Development and application of redox-active cyclometallating ligands based on W(II) alkyne complexes
Hüttenschmidt, Mareike; Lange, Helge; Cordero, Miguel A. Argüello; Villinger, Alexander; Lochbrunner, Stefan; Seidel, Wolfram Willy; Dalton Transactions  (2022) –; doi:10.1039/D1DT02393D

data_7709119
_publ_section_title
;
 Development and application of redox-active cyclometallating ligands
 based on W(II) alkyne complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02393D
_journal_year                    2022
_chemical_formula_moiety
'C68 H80 Au2 B2 I2 N12 O2 P2 W2, 2.89(C H2 Cl2)'
_chemical_formula_sum            'C70.89 H84.95 Au2 B2 Cl5.77 I2 N12 O2 P2 W2'
_chemical_formula_weight         2440.62
_chemical_name_systematic
like-Bis[carbonyl-iodido-tris{hydrido(3,4,5-trimethylpyrazolyl)borato}-(\h2-C,C?-2-propin-1,3-diyldiphenylphosphine)-digold(I)
_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-2014/7
_audit_update_record
;
2021-06-30 deposited with the CCDC.	2021-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                97.652(3)
_cell_angle_beta                 93.120(3)
_cell_angle_gamma                92.069(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9589(9)
_cell_length_b                   11.3595(9)
_cell_length_c                   32.950(3)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.42
_cell_volume                     4055.4(6)
_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 0.999
_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  0.0990
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            205863
_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         31.999
_diffrn_reflns_theta_min         1.874
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    7.475
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.5123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_description       block
_exptl_crystal_F_000             2321
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.190
_refine_diff_density_min         -2.071
_refine_diff_density_rms         0.240
_refine_ls_extinction_coef       0.00088(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     981
_refine_ls_number_reflns         28133
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+22.9781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20310
_reflns_number_total             28133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02393d2.cif
_cod_data_source_block           is_hl265
_cod_original_cell_volume        4055.5(6)
_cod_database_code               7709119
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.400
_shelx_estimated_absorpt_t_max   0.807
_shelx_res_checksum              78110