Synthesis and Reactivity of Fluoro Complexes: Part 2.1 Rhodium(I) Fluoro Complexes with Alkene and Phosphine Ligands. Synthesis of the First Isolated Rhodium(I) Bifluoride Complexes. Structure of [Rh3(μ3-OH)2(COD)3](HF2) by X-ray Powder Diffraction
José Vicente; Juan Gil-Rubio; Delia Bautista; Angelo Sironi; Norberto Masciocchi; Inorganic Chemistry 43 (2004) 5665–5675; doi:10.1021/ic049585e

data_4311512
_publ_section_title
;
 Synthesis and Reactivity of Fluoro Complexes: Part 2.1 Rhodium(I) Fluoro
 Complexes with Alkene and Phosphine Ligands. Synthesis of the First
 Isolated Rhodium(I) Bifluoride Complexes. Structure of
 [Rh3(\m3-OH)2(COD)3](HF2) by X-ray Powder Diffraction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5665
_journal_page_last               5675
_journal_paper_doi               10.1021/ic049585e
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C26 H27 F P Rh'
_chemical_formula_weight         492.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.728(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7652(7)
_cell_length_b                   11.3795(7)
_cell_length_c                   14.6419(8)
_cell_measurement_reflns_used    83
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      5.41
_cell_volume                     2116.3(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w-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  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3891
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0.8
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.79798
_exptl_absorpt_correction_T_min  0.75555
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3720
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.027
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_obs          0.0205
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+1.4555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0498
_refine_ls_wR_factor_obs         0.0490
_reflns_number_observed          3313
_reflns_number_total             3720
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic049585e_1.cif
_cod_data_source_block           3
_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 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+1.4555P] 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^)+(0.0236P)^2^+1.4555P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4311512