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_7120124
_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         'C22 H30 B N7 O W, C H2 Cl2'
_chemical_formula_sum            'C23 H32 B Cl2 N7 O W'
_chemical_formula_weight         688.11
_chemical_name_systematic
'[(Acetylene)(carbonyl)(cyanido){hydridotris(3,4,5-trimethylpyrazolyl)borate}tungsten(II)]'
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-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-2013
_audit_update_record
;
2016-09-06 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.209(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8346(4)
_cell_length_b                   24.9365(8)
_cell_length_c                   9.9552(3)
_cell_measurement_reflns_used    4523
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.50
_cell_volume                     2679.54(15)
_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-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE 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  0.0737
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35866
_diffrn_reflns_point_group_measured_fraction_full 0.998
_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         2.387
_exptl_absorpt_coefficient_mu    4.541
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       needle
_exptl_crystal_F_000             1360
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, n-pentane'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
The unit cell contains about four dichloromethane molecules which have been 
treated as a diffuse contribution to the overall scattering without specific 
atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7117
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5147
_reflns_number_total             7117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02114c2.cif
_cod_data_source_block           is_sl116
_cod_database_code               7120124
_shelx_estimated_absorpt_t_min   0.495
_shelx_estimated_absorpt_t_max   0.876
_shelxl_version_number           2013-4
_shelx_res_checksum              4228
_shelx_hkl_checksum              85108