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_7051013
_publ_contact_author             'Hansjoerg Gruetzmacher'
_publ_section_title
;
 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            'C56.5 H45.5 Cl1.5 P2 Rh'
_chemical_formula_weight         942.45
_chemical_name_common            Allyltropp-methyltropp-rhodium
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.27(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   45.899(51)
_cell_length_b                   10.159(10)
_cell_length_c                   19.773(19)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     9009(16)
_computing_cell_refinement       'STOE DIF4'
_computing_data_collection       'PICKER STOE DIF4'
_computing_data_reduction        'STOE REDU4'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'PICKER 4-circle Stoe upgrade'
_diffrn_measurement_method       ' \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4804
_diffrn_reflns_theta_max         49.99
_diffrn_reflns_theta_min         1.97
_diffrn_standards_interval_count 120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    4.842
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       prism
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         4620
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_obs          0.0455
_refine_ls_shift/esd_max         0.355
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+10.6119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1218
_refine_ls_wR_factor_obs         0.1132
_reflns_number_observed          3759
_reflns_number_total             4620
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002906h.txt
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+10.6119P] 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^)+(0.0745P)^2^+10.6119P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9009.3(159)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C56.50 H45.50 Cl1.50 P2 Rh'
_cod_database_code               7051013