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_7120126
_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 H50 B I1 N7 O2 P2 W +, 0.959(B F4 -), I0.041 -, 0.5(C4 H10 O)'
_chemical_formula_sum            'C47 H55 B1.96 F3.84 I1.04 N7 O2.5 P2 W'
_chemical_formula_weight         1229.84
_chemical_name_systematic
'[{Aminodiphenylphosphonium)(diphenylphosphinoxido)acetylene} oiodido){hydridotris(3,4,5-trimethylpyrazolyl)borate}tungsten(II)]'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                78.3940(10)
_cell_angle_beta                 84.6680(10)
_cell_angle_gamma                80.5150(10)
_cell_formula_units_Z            4
_cell_length_a                   12.6321(3)
_cell_length_b                   15.0895(3)
_cell_length_c                   26.9998(5)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.27
_cell_volume                     4962.82(18)
_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      123(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-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  0.0733
_diffrn_reflns_av_unetI/netI     0.1377
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            120390
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.180
_exptl_absorpt_coefficient_mu    3.100
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       plate
_exptl_crystal_F_000             2438
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, diethylether'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.566
_refine_diff_density_min         -2.758
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         27474
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+9.0173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16038
_reflns_number_total             27474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02114c2.cif
_cod_data_source_block           kh258
_cod_original_formula_sum        'C47 H55 B1.96 F3.84 I1.04 N7 O2.50 P2 W'
_cod_database_code               7120126
_shelx_estimated_absorpt_t_min   0.549
_shelx_estimated_absorpt_t_max   0.941
_shelxl_version_number           2013-4
_shelx_res_checksum              71013
_shelx_hkl_checksum              12464