Conformational analysis of triphenylphosphine in square planar [Rh(beta-diketonato)(CO)(PPh3)] complexes. Crystal structure of [Rh(PhCOCHCO(CH2)3CH3)(CO)(PPh3)]
Nomampondomise F. Stuurman; Alfred Muller; Jeanet Conradie; Inorganica Chimica Acta 395 (2013) 237–244; doi:10.1016/j.ica.2012.11.001

data_1512960
_publ_section_title
;
 Conformational analysis of triphenylphosphine in square planar
 [Rh(beta-diketonato)(CO)(PPh3)] complexes. Crystal structure of
 [Rh(PhCOCHCO(CH2)3CH3)(CO)(PPh3)]
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              237
_journal_page_last               244
_journal_paper_doi               10.1016/j.ica.2012.11.001
_journal_volume                  395
_journal_year                    2013
_chemical_formula_moiety         'C32 H30 O3 P Rh'
_chemical_formula_sum            'C32 H30 O3 P Rh'
_chemical_formula_weight         596.44
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 102.4410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2580(3)
_cell_length_b                   25.3880(8)
_cell_length_c                   10.7910(3)
_cell_measurement_reflns_used    5041
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.18
_cell_volume                     2744.31(14)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
        Bruker X8 ApexII 4K Kappa CCD
;
_diffrn_measurement_method       '\w & \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27503
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.8256
_exptl_absorpt_correction_T_min  0.7990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS (Bruker, 1998)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.828
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.339
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         6832
_refine_ls_number_restraints     369
_refine_ls_restrained_S_all      1.313
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+6.1021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                6216
_reflns_number_total             6832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-237-244.cif
_cod_data_source_block           6fms1_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512960