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_7709118
_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         'C49 H50 B Br Ir N9 O W, 4(C H2 Cl2)'
_chemical_formula_sum            'C53 H58 B Br Cl8 Ir N9 O W'
_chemical_formula_weight         1587.45
_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-phendiylpyridine)iridium(III)
_chemical_properties_physical    Photo-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-2014/7
_audit_update_record
;
2021-06-30 deposited with the CCDC.	2021-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                85.391(6)
_cell_angle_beta                 75.116(5)
_cell_angle_gamma                75.734(5)
_cell_formula_units_Z            2
_cell_length_a                   10.103(2)
_cell_length_b                   16.208(4)
_cell_length_c                   18.094(4)
_cell_measurement_reflns_used    7977
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.81
_cell_measurement_theta_min      2.23
_cell_volume                     2774.7(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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.1275
_diffrn_reflns_av_unetI/netI     0.1086
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63910
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.863
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.621
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_description       needle
_exptl_crystal_F_000             1548
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/diethylether'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
The unit cell contains eight CH2Cl2 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         3.562
_refine_diff_density_min         -3.399
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         12082
_refine_ls_number_restraints     382
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0781P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1518
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7632
_reflns_number_total             12082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02393d2.cif
_cod_data_source_block           is_mh367
_cod_original_cell_volume        2774.7(10)
_cod_database_code               7709118
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.165
_shelx_estimated_absorpt_t_max   0.896
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              57378