Rhodium(i) complexes of unsymmetrical diphosphines: efficient and stable methanol carbonylation catalysts
Carraz, Charles-Antoine; Orpen, A. Guy; Ellis, Dianne D.; Pringle, Paul G.; Ditzel, Evert J.; Sunley, Glenn J.; Chemical Communications  (2000) 1277–; doi:10.1039/b002802i

data_7110964
_publ_section_title
;
 Rhodium(i) complexes of unsymmetrical diphosphines: efficient and stable
 methanol carbonylation catalysts
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1277
_journal_paper_doi               10.1039/b002802i
_journal_year                    2000
_chemical_formula_sum            'C29.5 H22 F2 I3 O P2 Rh'
_chemical_formula_weight         976.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.850(3)
_cell_length_b                   15.338(4)
_cell_length_c                   20.992(4)
_cell_measurement_temperature    173(2)
_cell_volume                     6069(2)
_computing_cell_refinement       'SMART (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SMART (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33277
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    3.755
_exptl_absorpt_correction_T_max  0.8149
_exptl_absorpt_correction_T_min  0.3001
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_description       disks
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.856
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.165
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6871
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.177
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_obs          0.0382
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+28.1604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0981
_refine_ls_wR_factor_obs         0.0854
_reflns_number_observed          5701
_reflns_number_total             6885
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002802isup1.cif
_cod_data_source_block           12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+28.1604P] 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^)+(0.0288P)^2^+28.1604P] 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        6069.0(23)
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C29.50 H22 F2 I3 O P2 Rh'
_cod_database_code               7110964