New Chiral Zinc Complexes: Synthesis, Structure, and Induction of Axial Chirality
Helmut Degenbeck; Anne-Sophie Felten; Eduardo C. Escudero-Adán; Jordi Benet-Buchholz; Lorenzo Di Bari; Gennaro Pescitelli; Anton Vidal-Ferran; Inorganic Chemistry 51 (2012) 8643–8645; doi:10.1021/ic300915p

data_4330057
_publ_section_title
;
 New Chiral Zinc Complexes: Synthesis, Structure, and Induction of Axial
 Chirality
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8643
_journal_page_last               8645
_journal_paper_doi               10.1021/ic300915p
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C36 H56 N2 O6.67 Zn'
_chemical_formula_weight         688.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   16.1449(13)
_cell_length_b                   24.1265(18)
_cell_length_c                   30.798(2)
_cell_measurement_reflns_used    1632
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.03
_cell_measurement_theta_min      2.61
_cell_volume                     11996.4(15)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1871
_diffrn_reflns_av_sigmaI/netI    0.1790
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            83795
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.07
_diffrn_source                   'rotating anode x-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_correction_T_min  0.9679
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       Block
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1346
_refine_ls_number_reflns         21313
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      2.484
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+0.1202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.2106
_reflns_number_gt                11517
_reflns_number_total             21313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300915p_si_002_3.cif
_cod_data_source_block           4b_hd295_0m
_cod_original_cell_volume        11996.4(16)
_cod_database_code               4330057