Highly distorted d8-rhodium(+I) and d10-rhodium(-I) complexes: synthesis, reactivity, and structures in solution and solid state
Deblon, Stephan; Rüegger, Heinz; Schönberg, Hartmut; Loss, Sandra; Gramlich, Volker; Grützmacher, Hansjörg; New Journal of Chemistry 25 (2001) 83–; doi:10.1039/b002906h

data_7051012
_publ_contact_author             'Sandra Loss'
_publ_section_title
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 Highly distorted d8-rhodium(+I) and d10-rhodium(-I) complexes:
 synthesis, reactivity, and structures in solution and solid state
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              83
_journal_paper_doi               10.1039/b002906h
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C58 H49 F6 N P3 Rh'
_chemical_formula_weight         1069.80
_chemical_name_common            Bis-(Methyltropp)rhodium-hexafluorophosphate
_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
_cell_angle_alpha                91.629(13)
_cell_angle_beta                 91.462(13)
_cell_angle_gamma                101.890(12)
_cell_formula_units_Z            4
_cell_length_a                   10.844(2)
_cell_length_b                   20.697(4)
_cell_length_c                   22.722(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4985.7(17)
_computing_cell_refinement       IPDS0-Package
_computing_data_collection       IPDS0-Package
_computing_data_reduction        IPDS0-Package
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe Image Plate System'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28990
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       prism
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.751
_refine_ls_goodness_of_fit_obs   0.964
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1265
_refine_ls_number_reflns         14653
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.750
_refine_ls_restrained_S_obs      0.964
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_obs          0.0361
_refine_ls_shift/esd_max         1.566
_refine_ls_shift/esd_mean        0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0769
_refine_ls_wR_factor_obs         0.0721
_reflns_number_observed          8381
_reflns_number_total             14653
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002906h.txt
_cod_data_source_block           9
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051012