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_7709116
_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
'C34 H41 B I N6 O P W, 0.3(C H2 Cl2), 0.5(C5 H12)'
_chemical_formula_sum            'C36.8 H47.61 B Cl0.61 I N6 O P W'
_chemical_formula_weight         964.06
_chemical_name_systematic
Carbonyl-iodido-tris{hydrido(3,4,5-trimethylpyrazolyl)borato}-(\h2-C,C?-2-propinyldiphenylphosphine)-tungsten(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 102.482(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.299(16)
_cell_length_b                   10.596(4)
_cell_length_c                   16.986(6)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.31
_cell_measurement_theta_min      2.28
_cell_volume                     7785(5)
_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 0.938
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83830
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         2.275
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.881
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       block
_exptl_crystal_F_000             3806
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/n-pentane'
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.691
_refine_diff_density_min         -2.094
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       0.00029(3)
_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   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         14069
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0369P)^2^+173.9951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10616
_reflns_number_total             14069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02393d2.cif
_cod_data_source_block           is_hl255b
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C36.80 H47.61 B Cl0.61 I N6 O P W'
_cod_database_code               7709116
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.361
_shelx_estimated_absorpt_t_max   0.698
_shelx_res_checksum              81931