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_4330060
_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_formula_sum            'C92 H116 N4 O14 Zn2'
_chemical_formula_weight         1632.63
_space_group_IT_number           1
_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                106.635(2)
_cell_angle_beta                 97.083(2)
_cell_angle_gamma                100.6200(10)
_cell_formula_units_Z            1
_cell_length_a                   11.8706(7)
_cell_length_b                   12.7734(9)
_cell_length_c                   14.4742(10)
_cell_measurement_reflns_used    6980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.53
_cell_volume                     2030.4(2)
_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
_computing_data_collection       'Bruker APEX2 v2011.4-0'
_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    Sir2011
_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 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support whith MicroMount'
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24647
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.69
_diffrn_reflns_theta_min         1.49
_diffrn_source                   'Micorfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.9869
_exptl_absorpt_correction_T_min  0.9492
_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    1.335
_exptl_crystal_description       Needle
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.882
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1041
_refine_ls_number_reflns         19965
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0481
_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^)+(0.1068P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                17008
_reflns_number_total             19965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300915p_si_002_6.cif
_cod_data_source_block           5c_ent_mo_hd324-b_0m
_cod_database_code               4330060