Bis(<i>tert</i>-butyldimethylsilyl)(2,6-diisopropylphenyl)phosphane: the first structure of an organophosphane with two <i>tert</i>-butyldimethylsilyl (TBDMS) substituents
Boeré, René T.; Taghavikish, Mona; Acta Crystallographica Section C 68 (2012) o381–o382; doi:10.1107/S0108270112035949

data_2018665
_publ_section_title
;
 Bis(<i>tert</i>-butyldimethylsilyl)(2,6-diisopropylphenyl)phosphane: the
 first structure of an organophosphane with two
 <i>tert</i>-butyldimethylsilyl (TBDMS) substituents
;
_journal_coeditor_code           SK3445
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o381
_journal_page_last               o382
_journal_paper_doi               10.1107/S0108270112035949
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C24 H47 P Si2'
_chemical_formula_moiety         'C24 H47 P Si2'
_chemical_formula_sum            'C24 H47 P Si2'
_chemical_formula_weight         422.77
_chemical_melting_point          330
_chemical_name_systematic
;
Bis(<i>tert</i>-butyldimethylsilyl)(2,6-diisopropylphenyl)phosphane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                80.084(2)
_cell_angle_beta                 88.989(2)
_cell_angle_gamma                88.943(2)
_cell_formula_units_Z            2
_cell_length_a                   10.432(3)
_cell_length_b                   11.237(3)
_cell_length_c                   11.885(3)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.30
_cell_volume                     1372.0(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2008)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0129
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16018
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.319
_exptl_crystal_size_min          0.242
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.199
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         6218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.3449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                5511
_reflns_number_total             6218
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3445.cif
_cod_data_source_block           I
_cod_database_code               2018665
_cod_database_fobs_code          2018665