Rhodium Complexes of a New Structurally Adaptive PNN-Pincer Type Ligand
Wanniarachchi, Sarath; Hewage, Jeewantha S.; Lindeman, Sergey V.; Gardinier, James R.; Organometallics 32 (2013) 2885–; doi:10.1021/om400151e

data_4080738
_publ_section_title
;
 Rhodium Complexes of a New Structurally Adaptive PNN-Pincer Type Ligand
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2885
_journal_paper_doi               10.1021/om400151e
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C38 H41 N5 P Rh, C1 H2.4'
_chemical_formula_sum            'C39 H43.4 N5 P Rh'
_chemical_formula_weight         716.09
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2012-05-21
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                63.183(4)
_cell_angle_beta                 89.650(3)
_cell_angle_gamma                74.920(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5283(4)
_cell_length_b                   13.2391(5)
_cell_length_c                   14.1743(5)
_cell_measurement_reflns_used    16522
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5130
_cell_measurement_theta_min      3.3672
_cell_volume                     1848.59(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_details
;
  1 omega -100.00  -75.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  178.0000    0.0000 25

  2 omega  -36.00   54.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -      -11.8259   57.0000   30.0000 90

  3 omega  -79.00   16.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -77.0000  120.0000 95

  4 omega  -86.00   15.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -57.0000 -120.0000 101

  5 omega   34.00  100.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -       11.6697 -178.0000  -30.0000 66

  6 omega   34.00  100.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -       11.6697 -178.0000   60.0000 66

  7 omega  -41.00   62.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -      -11.8259   57.0000  150.0000 103

  8 omega  -20.00   30.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -99.0000  -60.0000 50

  9 omega  -86.00   18.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -57.0000 -180.0000 104

 10 omega  -86.00   18.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -57.0000   30.0000 104

 11 omega  -41.00   -2.00   1.0000   11.7200
omega____ theta____ kappa____ phi______ frames
    -      -11.8259   57.0000  -30.0000 39
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0476664000
_diffrn_orient_matrix_UB_12      0.0439419000
_diffrn_orient_matrix_UB_13      -0.0401589000
_diffrn_orient_matrix_UB_21      -0.0425580000
_diffrn_orient_matrix_UB_22      -0.0275275000
_diffrn_orient_matrix_UB_23      0.0297383000
_diffrn_orient_matrix_UB_31      -0.0067818000
_diffrn_orient_matrix_UB_32      0.0352458000
_diffrn_orient_matrix_UB_33      0.0264616000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41908
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             745
_exptl_crystal_size_max          0.2698
_exptl_crystal_size_mid          0.2502
_exptl_crystal_size_min          0.0651
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         9464
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+1.5668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                8249
_reflns_number_total             9464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400151e_si_001.cif
_cod_data_source_block           4_0.2pentane
_cod_original_cell_volume        1848.59(11)
_cod_original_formula_sum        'C39 H43.40 N5 P Rh'
_cod_database_code               4080738
_chemical_oxdiff_formula         'C38 H41 N5 P Rh'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32