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_7120122
_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         'C33 H39 B I N6 O P W, C5 H12'
_chemical_formula_sum            'C38 H51 B I N6 O P W'
_chemical_formula_weight         960.38
_chemical_name_systematic
'[(Carbonyl)(ethinyldiphenylphosphine)(iodido){hydridotris(3,4,5-trimethylpyrazolyl)borate}tungsten(II)]'
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9669(5)
_cell_length_b                   10.4622(3)
_cell_length_c                   22.0079(7)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.88
_cell_measurement_theta_min      2.29
_cell_volume                     3906.6(2)
_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    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57393
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.999
_diffrn_reflns_theta_min         1.947
_exptl_absorpt_coefficient_mu    3.826
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, n-pentane'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.315
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
 Flack x determined using 3614 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         11563
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0265P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.854
_reflns_number_gt                9396
_reflns_number_total             11563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02114c2.cif
_cod_data_source_block           is_kh197
_cod_database_code               7120122
_shelx_estimated_absorpt_t_min   0.580
_shelx_estimated_absorpt_t_max   0.657
_shelxl_version_number           2013-4
_shelx_res_checksum              40647
_shelx_hkl_checksum              99164