Thioether, Dinitrogen, and Olefin Complexes of (PNP)Rh: Kinetics and Thermodynamics of Exchange and Oxidative Addition Reactions
Gatard, Sylvain; Guo, Chengyun; Foxman, Bruce M.; Ozerov, Oleg V.; Organometallics 26 (2007) 6066–; doi:10.1021/om700563k

data_4073704
_publ_section_title
;
 Thioether, Dinitrogen, and Olefin Complexes of (PNP)Rh:&#x00A0; Kinetics
 and Thermodynamics of Exchange and Oxidative Addition Reactions
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              6066
_journal_paper_doi               10.1021/om700563k
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C32 H52 N1 P2 Rh1'
_chemical_formula_sum            'C32 H52 N P2 Rh'
_chemical_formula_weight         615.62
_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
_audit_creation_date             04-12-10
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                85.05(2)
_cell_angle_beta                 81.31(4)
_cell_angle_gamma                62.22(4)
_cell_formula_units_Z            2
_cell_length_a                   9.688(8)
_cell_length_b                   9.940(3)
_cell_length_c                   19.119(5)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    294
_cell_measurement_theta_max      17
_cell_measurement_theta_min      10
_cell_volume                     1610.0(16)
_computing_cell_refinement       'CAD4 Express, (Straver, 1992)'
_computing_data_collection       'CAD4 Express, (Straver, 1992)'
_computing_data_reduction        'RC93 (Watkin, Prout & Lilley, 1994)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      294
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6704
_diffrn_reflns_theta_full        26.272
_diffrn_reflns_theta_max         26.272
_diffrn_reflns_theta_min         2.316
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimutal absorption correction (North et al., 1968) 
;
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       prism
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.59
_refine_diff_density_min         -2.10
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0724
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5180
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000871
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.84 0.967 1.37 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0988
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0661
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              12
_reflns_limit_k_min              -10
_reflns_limit_l_max              23
_reflns_limit_l_min              -23
_reflns_number_gt                5180
_reflns_number_total             6500
_reflns_threshold_expression     I>1.96u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.4632(11)
_oxford_structure_analysis_title OZ030
_cod_data_source_file            om700563k-file002.cif
_cod_data_source_block           Compound21_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C32 H52 N1 P2 Rh1'
_cod_database_code               4073704