Novel insertion of ethynylbenzene derivatives bearing an electron-withdrawing substituent at the 4-position into a P‒C bond and their transannular insertion between a metal atom and an ipso-carbon atom of the phosphine ligand †
Yamamoto, Yasuhiro; Sugawara, Kenichiro; Journal of the Chemical Society, Dalton Transactions  (2000) 2896–; doi:10.1039/b004984k

data_7009979
_publ_section_title
;
 Novel insertion of ethynylbenzene derivatives bearing an
 electron-withdrawing substituent at the 4-position into a P--C bond
 and their transannular insertion between a metal atom and an
 ipso-carbon atom of the phosphine ligand&#x200A;&#x2020;
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2896
_journal_paper_doi               10.1039/b004984k
_journal_year                    2000
_chemical_formula_sum            'C49 H47 F6 O6 P2 Rh'
_chemical_formula_weight         1010.75
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90
_cell_angle_beta                 103.70(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.534(3)
_cell_length_b                   19.986(3)
_cell_length_c                   15.757(3)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    299.2
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      10.1
_cell_volume                     4752.8(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9980
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8992
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_standards_decay_%        3.80
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.97
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8328
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.0995
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.07000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1981
_reflns_number_gt                3298
_reflns_number_total             8370
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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_cod_data_source_block           2
_cod_original_cell_volume        4752(1)
_cod_original_formula_sum        'C49 H47 F6 O6 P2 Rh '
_cod_database_code               7009979