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_7038194
_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 Mo2 O4 P4, 0.5(C5 H12)'
_chemical_formula_sum            'C42.5 H72 Mo2 O4 P4'
_chemical_formula_weight         962.76
_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             2014-05-28T12:07:41-00:00
_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                   21.3078(11)
_cell_length_b                   21.3078(11)
_cell_length_c                   8.7689(3)
_cell_measurement_reflns_used    10552
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.387
_cell_measurement_theta_min      3.185
_cell_volume                     3447.9(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1399
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0237121
_diffrn_orient_matrix_UB_12      -0.0375257
_diffrn_orient_matrix_UB_13      -0.012371
_diffrn_orient_matrix_UB_21      -0.0289836
_diffrn_orient_matrix_UB_22      0.0066876
_diffrn_orient_matrix_UB_23      -0.0133241
_diffrn_orient_matrix_UB_31      0.0086186
_diffrn_orient_matrix_UB_32      0.0047536
_diffrn_orient_matrix_UB_33      -0.0788183
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15758
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.89869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1509
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.30(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4529
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+0.7302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                4445
_reflns_number_total             4529
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5dt04983k2.cif
_cod_data_source_block           zal1a
_cod_depositor_comments
'Adding full bibliography for 7038194--7038196.cif.'
_cod_original_sg_symbol_Hall     '-P 32 2"'
_cod_original_formula_sum        'C42.50 H72 Mo2 O4 P4'
_cod_database_code               7038194