Probing the steric and electronic characteristics of a new bis-pyrrolide pincer ligand.
Komine, Nobuyuki; Buell, René W; Chen, Chun-Hsing; Hui, Alice K.; Pink, Maren; Caulton, Kenneth G.; Inorganic chemistry 53 (2014) 1361–1369; doi:10.1021/ic402120r

data_4337341
_publ_section_title
;
 Probing the steric and electronic characteristics of a new bis-pyrrolide
 pincer ligand.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1361
_journal_page_last               1369
_journal_paper_doi               10.1021/ic402120r
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C29 H43 N3, C2 H3 N'
_chemical_formula_sum            'C31 H46 N4'
_chemical_formula_weight         474.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                81.777(8)
_cell_angle_beta                 74.700(8)
_cell_angle_gamma                72.946(8)
_cell_formula_units_Z            2
_cell_length_a                   9.992(2)
_cell_length_b                   10.534(2)
_cell_length_c                   15.403(4)
_cell_measurement_reflns_used    7476
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.30
_cell_volume                     1491.2(6)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2012)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2012)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2012)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2010)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2010)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.749
_diffrn_measured_fraction_theta_max 0.749
_diffrn_measurement_details
'0.50 degree frames measured for 20 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19516
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.9871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS, G. Sheldrick, 2008'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0872P)^2^+0.1091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                4724
_reflns_number_total             6049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402120r_si_005.cif
_cod_data_source_block           13018
_cod_original_cell_volume        1491.3(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4337341