A Monometallic Rh(III) Tetraphosphine Complex: Reductive Activation of CH2Cl2 and Selective Meso to Racemic Tetraphosphine Ligand Isomerization
Clinton Hunt; Frank R. Fronczek; Damon R. Billodeaux; George G. Stanley; Inorganic Chemistry 40 (2001) 5192–5198; doi:10.1021/ic010003s

data_4320279
_publ_section_title
;
 A Monometallic Rh(III) Tetraphosphine Complex: Reductive Activation of
 CH2Cl2 and Selective Meso to Racemic Tetraphosphine Ligand Isomerization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5192
_journal_page_last               5198
_journal_paper_doi               10.1021/ic010003s
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C26 H44 B Cl2 F4 O P4 Rh'
_chemical_formula_weight         757.15
_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'
_cell_angle_alpha                90
_cell_angle_beta                 98.21(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.712(1)
_cell_length_b                   14.467(2)
_cell_length_c                   21.619(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      10.9
_cell_volume                     3316.0(6)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1994)
_computing_data_collection       CAD4_(Enraf-Nonius,_1994)
_computing_data_reduction        process_MolEN_(Fair,_1990)
_computing_publication_material  BTABLE_PTABLE_CIF_IN_MolEN_(Fair,_1990)
_computing_structure_refinement  LSFM_MolEN_(Fair,_1990)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      100
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8298
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        0.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   psi_scans_(North,_Phillips,_Mathews,_1968)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.27
_refine_diff_density_min         -0.16
_refine_ls_abs_structure_details ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.281
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    calculated_U=1.3_x_bonding_atom
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.037
_refine_ls_R_factor_obs          0.030
_refine_ls_shift/esd_max         0.047
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^) + 0.0004 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.046
_refine_ls_wR_factor_obs         0.038
_reflns_number_observed          6523
_reflns_number_total             7581
_reflns_observed_criterion       >3.0\s(I)
_cod_data_source_file            ic010003s_2.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) + 0.0004
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w =
4Fo^2^/(\s^2^(Fo^2^) + 0.0004 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3315.9(6)
_cod_original_formula_sum        'C26 H44 O B F4 P4 Cl2 Rh'
_cod_database_code               4320279