Selective formation of cis-diacyl, cis-PPh2R rhodium(III) complexes by the reaction of rhodium(III) cis-diacyl, trans-PPh2R complexes with aliphatic diamines
Garralda, María A.; Hernández, Ricardo; Pinilla, Elena; Torres, M. Rosario; Zarandona, Malkoa; Dalton Transactions  (2009) 9860–9869; doi:10.1039/b913244a

data_7002815
_publ_section_title
;
 Selective formation of cis-diacyl, cis-PPh2R rhodium(III) complexes by
 the reaction of rhodium(III) cis-diacyl, trans-PPh2R complexes with
 aliphatic diamines
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              9860
_journal_page_last               9869
_journal_paper_doi               10.1039/b913244a
_journal_year                    2009
_chemical_formula_moiety         'C76 H56 Cl O4 P4 Rh2, B F4, C4 H10 O'
_chemical_formula_sum            'C80 H66 B Cl F4 O5 P4 Rh2'
_chemical_formula_weight         1630.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 92.365(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.918(2)
_cell_length_b                   18.406(2)
_cell_length_c                   20.657(2)
_cell_measurement_temperature    296(2)
_cell_volume                     6806.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1735
_diffrn_reflns_av_sigmaI/netI    0.2341
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25936
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The final refinement show high values of residual non-modelled
electronic density.Therefore, the Squeeze program was used to
calculate to solvent disordered area and to remove its contribution
to the overal intensity data.An improvement was observed in all
refinement parameters and residual when this procedure is applied
;
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.276
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.1841
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1195P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2442
_reflns_number_gt                2267
_reflns_number_total             6001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b913244a.txt
_cod_data_source_block           compound_8a[BF4]
_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        6806.8(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7002815