Stereoselective formation and catalytic activity of hydrido(acylphosphane)(chlorido)(pyrazole)rhodium(iii) complexes. Experimental and DFT studies.
San Nacianceno, Virginia; Azpeitia, Susan; Ibarlucea, Lourdes; Mendicute-Fierro, Claudio; Rodríguez-Diéguez, Antonio; Seco, José M; San Sebastian, Eider; Garralda, María A; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13141–13155; doi:10.1039/c5dt01705j

data_7035316
_publ_section_title
;
 Stereoselective formation and catalytic activity of
 hydrido(acylphosphane)(chlorido)(pyrazole)rhodium(iii) complexes.
 Experimental and DFT studies.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13141
_journal_page_last               13155
_journal_paper_doi               10.1039/c5dt01705j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C43 H39 Cl4 N2 O P2 Rh'
_chemical_formula_weight         906.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_audit_update_record
;
2015-04-29 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                104.680(5)
_cell_angle_beta                 105.492(5)
_cell_angle_gamma                111.777(5)
_cell_formula_units_Z            2
_cell_length_a                   12.0092(6)
_cell_length_b                   14.0790(9)
_cell_length_c                   14.3161(9)
_cell_measurement_reflns_used    8761
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9793
_cell_measurement_theta_min      3.4842
_cell_volume                     1991.0(3)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14243
_diffrn_reflns_theta_full        74.14
_diffrn_reflns_theta_max         74.14
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    6.988
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.2826
_exptl_crystal_size_mid          0.1256
_exptl_crystal_size_min          0.0617
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7850
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+2.6056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                7267
_reflns_number_total             7850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01705j13.cif
_cod_data_source_block           3aHdmpz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035314--7035316.cif.
;
_cod_original_cell_volume        1991.0(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7035316