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_4073703
_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         'C56 H90 N4 O1 P4 Rh2'
_chemical_formula_sum            'C56 H90 N4 O P4 Rh2'
_chemical_formula_weight         1165.06
_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             07-05-20
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                60.3685(13)
_cell_angle_beta                 89.1379(15)
_cell_angle_gamma                66.7793(14)
_cell_formula_units_Z            2
_cell_length_a                   13.6205(4)
_cell_length_b                   16.6389(5)
_cell_length_c                   16.7659(5)
_cell_measurement_reflns_used    9054
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2957.24(17)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'KappaCCD ApexII'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67729
_diffrn_reflns_theta_full        30.135
_diffrn_reflns_theta_max         30.135
_diffrn_reflns_theta_min         1.434
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224.000
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9301
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         17360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.006251
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 2.10P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0624
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0624
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              23
_reflns_limit_k_min              -19
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                14881
_reflns_number_total             17409
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.34
_oxford_diffrn_Wilson_scale      10.78
_oxford_refine_ls_scale          0.31588(10)
_oxford_structure_analysis_title 'oz066 in P-1'
_cod_data_source_file            om700563k-file001.cif
_cod_data_source_block           Compound19a_finalcif
_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        'C56 H90 N4 O1 P4 Rh2'
_cod_database_code               4073703