Transamination chemistry of sodium TMP-zincate: synthesis and crystal structure of a chiral amidozincate
Armstrong, David R.; Clegg, William; Dale, Sophie H.; García-Álvarez, Joaquín; Harrington, Ross W.; Hevia, Eva; Honeyman, Gordon W.; Kennedy, Alan R.; Mulvey, Robert E.; O'Hara, Charles T.; Chemical Communications (Cambridge, United Kingdom)  (2008) 187–189; doi:10.1039/b713987j

data_7102803
_publ_section_title
;
 Transamination chemistry of sodium TMP-zincate: synthesis and crystal
 structure of a chiral amidozincate
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   2
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              187
_journal_page_last               189
_journal_paper_doi               10.1039/b713987j
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H50 N3 Na Zn'
_chemical_formula_sum            'C29 H50 N3 Na Zn'
_chemical_formula_weight         529.08
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.524(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9412(2)
_cell_length_b                   17.3511(6)
_cell_length_c                   20.8700(7)
_cell_measurement_reflns_used    5854
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     3202.00(17)
_computing_cell_refinement       'DENZO & COLLECT'
_computing_data_collection       'DENZO & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXL97
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonious KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.075
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42285
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         11301
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0813
_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^)+(0.0149P)^2^+3.5949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                8844
_reflns_number_total             11301
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b713987j.txt
_cod_data_source_block           grem204_compound5
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7102803