The reactivity of 1,1-dichloro-2,2-di-tert-butyldiphosphane towards lithiated metal carbonyls: a new entry to phosphanylphosphinidene dimers.
Grubba, Rafał; Zauliczny, Mateusz; Ponikiewski, Łukasz; Pikies, Jerzy; Dalton transactions (Cambridge, England : 2003) 45 (2016) 4961–4964; doi:10.1039/c5dt04983k

data_7038195
_publ_section_title
;
 The reactivity of 1,1-dichloro-2,2-di-tert-butyldiphosphane towards
 lithiated metal carbonyls: a new entry to phosphanylphosphinidene dimers.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4961
_journal_page_last               4964
_journal_paper_doi               10.1039/c5dt04983k
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C40 H66 O4 P4 W2'
_chemical_formula_sum            'C40 H66 O4 P4 W2'
_chemical_formula_weight         1102.51
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_IT_number           154
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-28T16:13:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-12-04 deposited with the CCDC.
2016-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.4329(8)
_cell_length_b                   21.4329(8)
_cell_length_c                   8.8370(3)
_cell_measurement_reflns_used    6973
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3542
_cell_measurement_theta_min      2.19
_cell_volume                     3515.6(2)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0231576
_diffrn_orient_matrix_UB_12      0.0198093
_diffrn_orient_matrix_UB_13      0.0605172
_diffrn_orient_matrix_UB_21      0.0254593
_diffrn_orient_matrix_UB_22      0.024502
_diffrn_orient_matrix_UB_23      -0.0526063
_diffrn_orient_matrix_UB_31      -0.016542
_diffrn_orient_matrix_UB_32      0.0215614
_diffrn_orient_matrix_UB_33      0.0040731
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.065
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14861
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    5.075
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.43874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1638
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
The solvent (O.5 molecule pro unit cell) contribution was modelled
by the SQUEEZE procedure of PLATON
;
_refine_diff_density_max         1.97
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.094
_reflns_number_gt                4161
_reflns_number_total             4537
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5dt04983k2.cif
_cod_data_source_block           zm5a
_cod_depositor_comments
'Adding full bibliography for 7038194--7038196.cif.'
_cod_original_sg_symbol_Hall     '-P 32 2"'
_cod_database_code               7038195