Synthesis and Characterization of N-Donor-Functionalized Enantiomerically Pure Pentadienyl Ligands Derived from (1R)-(−)-Myrtenal
Fecker, Ann Christin; Crăciun, Bogdan-Florin; Schweyen, Peter; Freytag, Matthias; Jones, Peter G.; Walter, Marc D.; Organometallics 34 (2015) 146–; doi:10.1021/om501024j

data_4085153
_publ_section_title
;
 Synthesis and Characterization of N-Donor-Functionalized Enantiomerically
 Pure Pentadienyl Ligands Derived from (1R)-(&#x2212;)-Myrtenal
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              146
_journal_paper_doi               10.1021/om501024j
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C36 H64 N2 Si2 V'
_chemical_formula_weight         632.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 112.341(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.1726(4)
_cell_length_b                   10.8238(2)
_cell_length_c                   17.2399(3)
_cell_measurement_reflns_used    62936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.8770
_cell_measurement_theta_min      4.3160
_cell_volume                     3654.28(13)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            84805
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         77.03
_diffrn_reflns_theta_min         4.31
_exptl_absorpt_coefficient_mu    3.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_exptl_crystal_colour            'dark oliv'
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7473
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0394P)^2^+2.1756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                7420
_reflns_number_total             7473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501024j_si_002.cif
_cod_data_source_block           ann43
_cod_depositor_comments
'Adding full bibliography for 4085149--4085163.cif.'
_cod_original_cell_volume        3654.27(12)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4085153