Intramolecular Dehydrofluorinative Coupling of η5-Pentamethylcyclopentadienyl and Pentafluorophenylphosphine Ligands in Rhodium Complexes
Bellabarba, Ronan M.; Nieuwenhuyzen, Mark; Saunders, Graham C.; Organometallics 21 (2002) 5726–; doi:10.1021/om020612n

data_4077117
_publ_section_title
;
 Intramolecular Dehydrofluorinative Coupling of
 \h5-Pentamethylcyclopentadienyl and Pentafluorophenylphosphine Ligands in
 Rhodium Complexes
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5726
_journal_paper_doi               10.1021/om020612n
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C35.5 H35 B Cl2 F8 N P2 Rh'
_chemical_formula_weight         874.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.1340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6204(7)
_cell_length_b                   23.2170(19)
_cell_length_c                   18.0923(15)
_cell_measurement_temperature    153(2)
_cell_volume                     3540.1(5)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38821
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8049
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          1.176
_refine_ls_shift/su_mean         0.038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+1.8492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                7065
_reflns_number_total             8049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020612n_2.cif
_cod_data_source_block           gcs23m
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C35.50 H35 B Cl2 F8 N P2 Rh'
_cod_database_code               4077117