Preparation of 2,4-bis(2,4,6-tri-tert-butylphenyl)-1,3-diphosphacyclobutenes from 2-(2,4,6-tri-tert-butylphenyl)-1-phosphaethyne and alkyllithiums
Ito, Shigekazu; Sugiyama, Hiroki; Yoshifuji, Masaaki; Chemical Communications  (2002) 1744–; doi:10.1039/b204142c

data_7111224
_publ_section_title
;
 Preparation of
 2,4-bis(2,4,6-tri-tert-butylphenyl)-1,3-diphosphacyclobutenes from
 2-(2,4,6-tri-tert-butylphenyl)-1-phosphaethyne and alkyllithiums
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1744
_journal_paper_doi               10.1039/b204142c
_journal_year                    2002
_chemical_formula_moiety         'C42 H68 P2 '
_chemical_formula_sum            'C42 H68 P2'
_chemical_formula_weight         634.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Tue Jun 11 23:20:12 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                98.722(3)
_cell_angle_beta                 98.760(2)
_cell_angle_gamma                67.629(9)
_cell_formula_units_Z            2
_cell_length_a                   13.592(2)
_cell_length_b                   14.861(2)
_cell_length_c                   10.916(2)
_cell_measurement_reflns_used    6523
_cell_measurement_temperature    110.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.5
_cell_volume                     2004.6(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.8592
_diffrn_measured_fraction_theta_max 0.8592
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12670
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.914
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5860
_refine_ls_R_factor_gt           0.1384
_refine_ls_shift/su_max          0.0095
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.10000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3198
_reflns_number_gt                4399
_reflns_number_total             7888
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            b204142csup1.cif
_cod_data_source_block           cyclo
_cod_original_cell_volume        2004.6(5)
_cod_original_sg_symbol_H-M      'P -1         '
_cod_original_formula_sum        'C42 H68 P2 '
_cod_database_code               7111224