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_7009980
_publ_contact_author
;
    ENTER NAME
 ENTER ADDRESS
;
_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            'C39 H42 Cl2 O6 P Rh'
_chemical_formula_weight         811.54
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_audit_creation_date             'Sat Apr 17 15:02:24 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.835(7)
_cell_length_b                   9.135(8)
_cell_length_c                   12.305(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    299.2
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      10.2
_cell_volume                     3916(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      299.2
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.02397
_diffrn_orient_matrix_UB_12      0.05640
_diffrn_orient_matrix_UB_13      0.01568
_diffrn_orient_matrix_UB_21      -0.01321
_diffrn_orient_matrix_UB_22      -0.09263
_diffrn_orient_matrix_UB_23      0.02185
_diffrn_orient_matrix_UB_31      0.00866
_diffrn_orient_matrix_UB_32      0.01487
_diffrn_orient_matrix_UB_33      0.07669
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_av_sigmaI/netI    0.142
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3936
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0.31
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1672.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.853
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     442
_refine_ls_number_reflns         2074
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0588
_refine_ls_shift/esd_max         0.1910
_refine_ls_shift/esd_mean        0.0380
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0762
_reflns_number_observed          2074
_reflns_number_total             3936
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            b004984k.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00040|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3915(5)
_cod_original_sg_symbol_H-M      'P c a 21   '
_cod_original_formula_sum        'C39 H42 Cl2 O6 P Rh '
_cod_database_code               7009980