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_7709117
_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
'0.77(C54 H52 Cl1 P4 Ru), 0.23(C54 H52 Cl2 P4 Ru),0.89(C4 H8 O)'
_chemical_formula_sum            'C57.57 H59.14 Cl1.23 O0.89 P4 Ru'
_chemical_formula_weight         1033.77
_chemical_name_systematic
Bis(1,3-diphenylphosphinyl)propane-ruthenium(I)chloride
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 100.466(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1304(9)
_cell_length_b                   10.5290(7)
_cell_length_c                   35.658(2)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.07
_cell_measurement_theta_min      2.26
_cell_volume                     4847.7(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 0.999
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            106999
_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         30.000
_diffrn_reflns_theta_min         2.256
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             2146
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/n-pentane'
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_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         14139
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+14.1107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11797
_reflns_number_total             14139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02393d2.cif
_cod_data_source_block           is_hl357
_cod_original_cell_volume        4847.7(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709117
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.863
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              16502