Unusual Redox Chemistry of Ytterbium Carbazole‒Bis(oxazoline) Compounds: Oxidative Coupling of Primary Phosphines by an Ytterbium Carbazole‒Bis(oxazoline) Dialkyl
Zou, Jin; Berg, David J.; Oliver, Allen; Twamley, Brendan; Organometallics 32 (2013) 6532–; doi:10.1021/om400861d

data_4081987
_publ_section_title
;
 Unusual Redox Chemistry of Ytterbium Carbazole--Bis(oxazoline) Compounds:
 Oxidative Coupling of Primary Phosphines by an Ytterbium
 Carbazole--Bis(oxazoline) Dialkyl
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6532
_journal_paper_doi               10.1021/om400861d
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C30 H38 N3 Na O2, 2(C7 H8)'
_chemical_formula_sum            'C44 H54 N3 Na O2'
_chemical_formula_weight         679.89
_chemical_name_common            'C30H38N3NaO2, 2(C7H8)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.348(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2099(6)
_cell_length_b                   9.5930(3)
_cell_length_c                   21.3759(7)
_cell_measurement_reflns_used    8866
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.33
_cell_volume                     3862.2(2)
_computing_cell_refinement       'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_data_collection       'SMART v. 5.632 (Bruker, 2006)'
_computing_data_reduction        'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_molecular_graphics    'XP, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)'
_computing_structure_refinement  'XL, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_structure_solution    'XS, SHELXTL  v. 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            57701
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.59
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2007/4 (Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+2.2822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                4910
_reflns_number_total             7003
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om400861d_si_010.cif
_cod_data_source_block           bt1175
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4081987