PX3-induced migratory insertion reactions of half-sandwich-type carbenerhodium(I) complexes
Herber, Ulrich; Guerrero Sanchez, Rita; Gevert, Olaf; Laubender, Matthias; Werner, Helmut; New Journal of Chemistry 25 (2001) 396–; doi:10.1039/b008601k

data_7051075
_publ_section_title
;
 PX3-induced migratory insertion reactions of half-sandwich-type
 carbenerhodium(I) complexes
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              396
_journal_paper_doi               10.1039/b008601k
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C45 H51 O3 P2 Rh'
_chemical_formula_weight         804.71
_chemical_melting_point          362.15
_chemical_name_systematic
;
 ?
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                85.68(1)
_cell_angle_beta                 84.78(2)
_cell_angle_gamma                88.03(2)
_cell_formula_units_Z            2
_cell_length_a                   10.170(3)
_cell_length_b                   11.177(2)
_cell_length_c                   17.401(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1963.4(8)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'BEGIN (SDP)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'CAD4 (Enraf-Nonius)'
_diffrn_measurement_method       'Omega/Theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.1013
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6553
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   'empirical (psi-scans)'
_exptl_absorpt_process_details
;
 empirical absorption correction by psi-scans from 6 reflections
 with chi-angles near 90 degrees
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.074
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    'refxyz; H6 refiso'
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6159
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_obs          0.0730
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+3.4371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1943
_refine_ls_wR_factor_obs         0.1633
_reflns_number_observed          4323
_reflns_number_total             6159
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b008601k.txt
_cod_data_source_block           6b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '89_C' was changed to '362.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+3.4371P] where P=(Fo^2^+2Fc^2^)/3' 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^2^)+(0.0973P)^2^+3.4371P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1963.5(7)
_cod_database_code               7051075