Rhodium Cyclopentyl Phosphine Complexes of Wide-Bite-Angle Ligands DPEphos and Xantphos
Dallanegra, Romaeo; Chaplin, Adrian B.; Weller, Andrew S.; Organometallics 31 (2012) 2720–; doi:10.1021/om201034m

data_4077906
_publ_section_title
;
 Rhodium Cyclopentyl Phosphine Complexes of Wide-Bite-Angle Ligands
 DPEphos and Xantphos
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2720
_journal_paper_doi               10.1021/om201034m
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C54 H59 O P3 Rh, C32 H12 B F24'
_chemical_formula_sum            'C86 H71 B F24 O P3 Rh'
_chemical_formula_weight         1783.06
_chemical_melting_point          ?
_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-97
_cell_angle_alpha                99.1448(4)
_cell_angle_beta                 106.8047(4)
_cell_angle_gamma                100.7042(4)
_cell_formula_units_Z            2
_cell_length_a                   12.85900(10)
_cell_length_b                   17.13950(10)
_cell_length_c                   21.8146(2)
_cell_measurement_reflns_used    21368
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.575
_cell_measurement_theta_min      5.097
_cell_volume                     4405.41(6)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27541
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         5.12
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_platon_squeeze_details          ' '
_refine_diff_density_max         1.466
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1365
_refine_ls_number_reflns         15395
_refine_ls_number_restraints     3812
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+57.9965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2533
_refine_ls_wR_factor_ref         0.2549
_reflns_number_gt                14204
_reflns_number_total             15395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201034m_si_001.cif
_cod_data_source_block           005rd08
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' 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_cell_volume        4405.40(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077906