A mechanistic investigation into the elimination of phosphonium salts from rhodium‒TRIPHOS complexes under methanol carbonylation conditions
Lamb, Gareth W.; Clarke, Matthew L.; Slawin, Alexandra M. Z.; Williams, Bruce; Dalton Transactions  (2008) 4946–4950; doi:10.1039/B803067G

data_7004141
_publ_section_title
;
 A mechanistic investigation into the elimination of phosphonium salts
 from rhodium--TRIPHOS complexes under methanol carbonylation
 conditions
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              4946
_journal_page_last               4950
_journal_paper_doi               10.1039/B803067G
_journal_year                    2008
_chemical_formula_moiety         'C37 H43 I3 O3 P3 Rh'
_chemical_formula_sum            'C37 H43 I3 O3 P3 Rh'
_chemical_formula_weight         1112.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.263(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.916(3)
_cell_length_b                   11.4403(17)
_cell_length_c                   20.007(4)
_cell_measurement_reflns_used    5275
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      22.91
_cell_measurement_theta_min      1.20
_cell_volume                     3915.5(12)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22382
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    2.959
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.766
_refine_diff_density_min         -2.592
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+145.6472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1749
_refine_ls_wR_factor_ref         0.1949
_reflns_number_gt                5151
_reflns_number_total             6829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B803067G.txt
_cod_data_source_block           5A
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3915.4(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7004141