Synthesis and activation potential of an open shell diphosphine.
Helmdach, Kai; Ludwig, Stephan; Villinger, Alexander; Hollmann, Dirk; Kösters, Jutta; Seidel, Wolfram W.; Chemical communications (Cambridge, England)  (2017) –; doi:10.1039/c7cc02114c

data_7120125
_publ_section_title
;
 Synthesis and activation potential of an open shell diphosphine.
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/c7cc02114c
_journal_year                    2017
_chemical_formula_moiety         'C45 H48 B F6 I N6 O P3 W, 0.6(C H2 Cl2)'
_chemical_formula_sum            'C45.58 H49.4 B Cl1.2 F6 I N6 O P3 W'
_chemical_formula_weight         1268.15
_chemical_name_systematic
Carbonyl-bis(diphenylphosphino)ethyne-hydridotris(3,4,5-trimethylpyrazolyl)borate-iodido-tungsten(III)-hexafluoroborate
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-03-17 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.1440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1608(4)
_cell_length_b                   19.5011(6)
_cell_length_c                   20.3015(5)
_cell_measurement_reflns_used    9699
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.79
_cell_measurement_theta_min      2.34
_cell_volume                     5004.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury 2016 '
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            161638
_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         29.000
_diffrn_reflns_theta_min         2.255
_exptl_absorpt_coefficient_mu    3.148
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       plate
_exptl_crystal_F_000             2497
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/n-pentane'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         2.316
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         13268
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0458
_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^)+42.8290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10606
_reflns_number_total             13268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02114c2.cif
_cod_data_source_block           kh468
_cod_original_formula_sum        'C45.58 H49.40 B Cl1.20 F6 I N6 O P3 W'
_cod_database_code               7120125
_shelx_estimated_absorpt_t_min   0.633
_shelx_estimated_absorpt_t_max   0.765
_shelxl_version_number           2014-3
_shelx_res_checksum              18046
_shelx_hkl_checksum              59095