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_4080737
_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         'C28 H24 N3 P'
_chemical_formula_sum            'C28 H24 N3 P'
_chemical_formula_weight         433.47
_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             2011-12-13
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                72.002(3)
_cell_angle_beta                 69.415(3)
_cell_angle_gamma                64.541(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8762(3)
_cell_length_b                   10.5856(3)
_cell_length_c                   12.9701(4)
_cell_measurement_reflns_used    31802
_cell_measurement_temperature    100.6
_cell_measurement_theta_max      29.3987
_cell_measurement_theta_min      3.3664
_cell_volume                     1125.96(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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      100.6
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
  1 omega  -57.00   38.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -37.0000  -90.0000 95

  2 omega  -13.00   82.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134   37.0000   90.0000 95

  3 omega   -4.00   51.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -98.0000  161.0000 55

  4 omega   11.00   42.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134   77.0000 -120.0000 31

  5 omega  -11.00   28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6697  -98.0000  161.0000 39

  6 omega  -67.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -77.0000   90.0000 112

  7 omega  -67.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -77.0000 -120.0000 112

  8 omega  -22.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134   77.0000 -180.0000 112

  9 omega  -21.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -98.0000  -89.0000 74

 10 omega  -22.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134   77.0000    0.0000 112

 11 omega  -21.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -98.0000  -18.0000 74

 12 omega  -28.00   64.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6697   37.0000 -180.0000 92

 13 omega  -53.00    0.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6697   98.0000   18.0000 53

 14 omega  -15.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134   37.0000  -60.0000 103

 15 omega  -67.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -77.0000 -180.0000 112

 16 omega  -67.00   45.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -77.0000    0.0000 112

 17 omega  -78.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134    0.0000 -180.0000 179

 18 omega  -78.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134    0.0000 -150.0000 179

 19 omega  -78.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134    0.0000 -120.0000 179

 20 omega  -78.00    0.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134    0.0000  -90.0000 78

 21 omega  -21.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5134  -98.0000  161.0000 74
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0348869000
_diffrn_orient_matrix_UB_12      0.0361831000
_diffrn_orient_matrix_UB_13      -0.0454725000
_diffrn_orient_matrix_UB_21      -0.0586810000
_diffrn_orient_matrix_UB_22      0.0503960000
_diffrn_orient_matrix_UB_23      0.0328588000
_diffrn_orient_matrix_UB_31      0.0458881000
_diffrn_orient_matrix_UB_32      0.0430993000
_diffrn_orient_matrix_UB_33      -0.0197090000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            63636
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.46
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         6000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.6310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                5515
_reflns_number_total             6000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400151e_si_001.cif
_cod_data_source_block           H(PNN)
_cod_original_cell_volume        1125.96(6)
_cod_database_code               4080737
_chemical_oxdiff_formula         'C28 H24 N3 P'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32