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_4080740
_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, 3(C3 H3)'
_chemical_formula_sum            'C48 H53 I N5 P Rh'
_chemical_formula_weight         960.73
_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                81.434(3)
_cell_angle_beta                 77.878(3)
_cell_angle_gamma                87.488(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1383(4)
_cell_length_b                   13.5899(6)
_cell_length_c                   15.4823(5)
_cell_measurement_reflns_used    11073
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5947
_cell_measurement_theta_min      3.4816
_cell_volume                     2265.53(15)
_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 0.992
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_details
;
  1 omega  -34.00   53.00   1.0000    5.8800
omega____ theta____ kappa____ phi______ frames
    -      -11.8259   57.0000 -180.0000 87

  2 omega  -77.00   21.00   1.0000    5.8800
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -77.0000  -90.0000 98

  3 omega  -86.00   17.00   1.0000    5.8800
omega____ theta____ kappa____ phi______ frames
    -      -11.8259  -57.0000   30.0000 103

  4 omega  -15.00   88.00   1.0000    5.8800
omega____ theta____ kappa____ phi______ frames
    -       11.6697   37.0000 -120.0000 103

  5 omega   34.00  100.00   1.0000    5.8800
omega____ theta____ kappa____ phi______ frames
    -       11.6697 -178.0000  120.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0602796000
_diffrn_orient_matrix_UB_12      0.0203113000
_diffrn_orient_matrix_UB_13      0.0033243000
_diffrn_orient_matrix_UB_21      -0.0225612000
_diffrn_orient_matrix_UB_22      -0.0475294000
_diffrn_orient_matrix_UB_23      -0.0016975000
_diffrn_orient_matrix_UB_31      -0.0100237000
_diffrn_orient_matrix_UB_32      -0.0107158000
_diffrn_orient_matrix_UB_33      0.0471980000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       14
_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       -21
_diffrn_reflns_number            27954
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.66
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.819
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             978
_exptl_crystal_size_max          0.2238
_exptl_crystal_size_mid          0.1648
_exptl_crystal_size_min          0.1211
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         11056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+1.0902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                9235
_reflns_number_total             11056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400151e_si_001.cif
_cod_data_source_block           cismer-6_3C6H6
_cod_original_cell_volume        2265.52(15)
_cod_database_code               4080740
_chemical_oxdiff_formula         'C34 H35 N4 P I Rh'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32