Synthesis and Characterization of a 1,3-Phenylene-Bridged N-Alkyl Bis(benzimidazole) CCC-NHC Pincer Ligand Precursor: Homobimetallic Silver and Rhodium Complexes and the Catalytic Hydrosilylation of Phenylacetylene
Huckaba, Aron J.; Hollis, T. Keith; Howell, Tyler O.; Valle, Henry U.; Wu, Yunshan; Organometallics 32 (2013) 63–; doi:10.1021/om3008037

data_4079797
_publ_section_title
;
 Synthesis and Characterization of a 1,3-Phenylene-Bridged N-Alkyl
 Bis(benzimidazole) CCC-NHC Pincer Ligand Precursor: Homobimetallic Silver
 and Rhodium Complexes and the Catalytic Hydrosilylation of
 Phenylacetylene
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              63
_journal_paper_doi               10.1021/om3008037
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C44 H54 I2 N4 Rh2'
_chemical_formula_sum            'C44 H54 I2 N4 Rh2'
_chemical_formula_weight         1098.57
_chemical_name_systematic        UMCB0009_AH_I_201
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2012-08-08
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.558(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4719(3)
_cell_length_b                   17.0771(5)
_cell_length_c                   14.8339(5)
_cell_measurement_reflns_used    7636
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.86
_cell_measurement_theta_min      3.06
_cell_volume                     2086.30(12)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      99.65
_diffrn_measured_fraction_theta_full 0.842152
_diffrn_measured_fraction_theta_max 0.842152
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_theta_full        69.392215
_diffrn_reflns_theta_max         69.39
_diffrn_reflns_theta_min         3.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.281
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.7486
_exptl_crystal_description       plate
_exptl_crystal_F_000             1086.4020
_exptl_crystal_recrystallization_method
'grown via vapor diffussion of Hexane into DCM'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.160835
_refine_diff_density_min         -1.210608
_refine_diff_density_rms         0.178633
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.037(5)
_refine_ls_d_res_high            0.823590
_refine_ls_d_res_low             14.420525
_refine_ls_goodness_of_fit_ref   1.011487
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    90
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011487
_refine_ls_R_factor_all          0.034730
_refine_ls_R_factor_gt           0.032240
_refine_ls_shift/su_max          0.0013
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.081171
_reflns_Friedel_coverage         0.719
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              19
_reflns_limit_k_min              -17
_reflns_limit_l_max              17
_reflns_limit_l_min              -17
_reflns_number_gt                6287
_reflns_number_total             6589
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om3008037_si_001.cif
_cod_data_source_block           UMCB0009_AH_I_201
_cod_database_code               4079797