NMR-Spectroscopic and Solid-State Investigations of Cometal-Free Asymmetric Conjugate Addition: A Dinuclear Paracyclophaneimine Zinc Methyl Complex
Sefer Ay; R. E. Ziegert; H. Zhang; Martin Nieger; Kari Rissanen; K. Fink; A. Kubas; Ruth M. Gschwind; Stefan Bräse; Journal of the American Chemical Society 132 (2010) 12899–12905; doi:10.1021/ja1032502

data_4103049
_publ_contact_author
;
        Martin Nieger
        Laboratory of Inorganic Chemistry
        Department of Chemistry
        Universitity of Helsinki
        P.O. Box 55
        FIN-00014 University of Helsinki
        Finland
;
_publ_contact_author_email       martin.nieger@helsinki.fi
_publ_contact_author_fax         '++358 9 191 50198'
_publ_contact_author_phone       '++358 9 191 50223'
_publ_section_title
;
 NMR-Spectroscopic and Solid-State Investigations of Cometal-Free
 Asymmetric Conjugate Addition: A Dinuclear Paracyclophaneimine Zinc
 Methyl Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12899
_journal_page_last               12905
_journal_paper_doi               10.1021/ja1032502
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C54 H58 N2 O2 Zn2, (C7 H8)0.5'
_chemical_formula_sum            'C57.5 H62 N2 O2 Zn2'
_chemical_formula_weight         943.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.2807(4)
_cell_length_b                   13.2807(4)
_cell_length_c                   52.5695(17)
_cell_measurement_reflns_used    221797
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     8029.8(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'rotation in phi and omega, 0.5 deg.'
_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  0.0694
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            88125
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.87994
_exptl_absorpt_correction_T_min  0.75154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (PLaton, cf. Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2982
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.030(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         12234
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0692P)^2^+2.2561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                11103
_reflns_number_total             12234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1032502_si_001.cif
_cod_data_source_block           sb061_m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C57.50 H62 N2 O2 Zn2'
_cod_database_code               4103049