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_7709120
_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
'C47 H50 B Br N11 O Ru W +, F6 P +, 1.375(C H2 Cl2)'
_chemical_formula_sum            'C48.38 H52.75 B Br Cl2.75 F6 N11 O P Ru W'
_chemical_formula_weight         1422.36
_chemical_name_systematic
Carbonyl-bromido-tris{hydrido(3,4,5-trimethylpyrazolyl)borato}tungsten(II)-(\m-\h2-C,C?-\k2-C,N-prop-1-in-1,3-diylpyridine)-bis(2,2?-bipyridine)ruthenium(II)-hexafluorophosphate
_chemical_properties_physical    Photo-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.5669(19)
_cell_length_b                   18.0426(12)
_cell_length_c                   19.5693(10)
_cell_measurement_reflns_used    9085
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.23
_cell_measurement_theta_min      2.26
_cell_volume                     10792.6(11)
_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 1.000
_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  0.0840
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            366456
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.185
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.385
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       needle
_exptl_crystal_F_000             5614
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/diethylether'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;
The unit cell contains seven 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         1.063
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         13019
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0151P)^2^+38.5229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11322
_reflns_number_total             13019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02393d2.cif
_cod_data_source_block           is_mh402
_cod_database_code               7709120
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.451
_shelx_estimated_absorpt_t_max   0.876
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              72105