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_4080743
_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         'I, C39 H44 N5 P Rh, 0.25(O)'
_chemical_formula_sum            'C39 H44 I N5 O0.25 P Rh'
_chemical_formula_weight         847.63
_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                97.659(3)
_cell_angle_beta                 107.384(3)
_cell_angle_gamma                111.238(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6257(4)
_cell_length_b                   13.1378(5)
_cell_length_c                   15.8308(6)
_cell_measurement_reflns_used    12681
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7405
_cell_measurement_theta_min      3.7474
_cell_volume                     1891.93(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega  -47.00    9.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   37.0000   90.0000 56

  2 omega -122.00   16.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487    0.0000   60.0000 138

  3 omega -115.00  -66.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487 -149.0000  123.0000 49

  4 omega   28.00   88.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6487 -123.0000  172.0000 60

  5 omega   32.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6487 -125.0000    0.0000 52

  6 omega   29.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000  -90.0000 57

  7 omega   35.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000  150.0000 26

  8 omega   93.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -125.0000  -30.0000 27

  9 omega   30.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -94.0000   30.0000 70

 10 omega   89.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -149.0000  -56.0000 38

 11 omega   47.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  -30.0000 27

 12 omega  133.00  173.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000   90.0000 40

 13 omega   26.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -94.0000   90.0000 83

 14 omega   83.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   30.0000 -180.0000 95

 15 omega   42.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000 -180.0000 51

 16 omega   79.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   30.0000   90.0000 98

 17 omega  117.00  169.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000  -60.0000 52

 18 omega   37.00   62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -149.0000  -56.0000 25

 19 omega   36.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000   60.0000 59

 20 omega   41.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378 -125.0000  -30.0000 49

 21 omega  -96.00   -2.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  125.0000  120.0000 94

 22 omega -115.00  -11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -57.0000   30.0000 104

 23 omega -117.00  -14.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -37.0000  -90.0000 103

 24 omega    7.00  119.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6487   77.0000 -150.0000 112

 25 omega    7.00  119.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.6487   77.0000  120.0000 112

 26 omega -140.00  -28.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000  -77.0000  -30.0000 112

 27 omega   77.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   61.0000 -150.0000 101

 28 omega   77.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   61.0000 -180.0000 81

 29 omega   46.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   15.0000  -30.0000 132

 30 omega   73.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   77.0000   60.0000 105

 31 omega   77.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   61.0000  120.0000 101

 32 omega   73.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0378   77.0000    0.0000 105
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0512850000
_diffrn_orient_matrix_UB_12      0.0358013000
_diffrn_orient_matrix_UB_13      -0.0881874000
_diffrn_orient_matrix_UB_21      -0.0105232000
_diffrn_orient_matrix_UB_22      -0.1089011000
_diffrn_orient_matrix_UB_23      -0.0579170000
_diffrn_orient_matrix_UB_31      -0.1594711000
_diffrn_orient_matrix_UB_32      -0.0628118000
_diffrn_orient_matrix_UB_33      -0.0097127000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27026
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.90
_diffrn_reflns_theta_min         3.75
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.715
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.1182
_exptl_crystal_size_mid          0.0636
_exptl_crystal_size_min          0.0426
_refine_diff_density_max         0.525
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0348P)^2^+1.0263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                6828
_reflns_number_total             7522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400151e_si_001.cif
_cod_data_source_block           fac-6_0.25H2O
_cod_original_cell_volume        1891.93(12)
_cod_database_code               4080743
_chemical_oxdiff_formula         'C39 H44 N5 P Rh I'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97