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_7102801
_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_formula_moiety         'C12 H32 N4 Na +, C14 H36 N Si2 Zn -'
_chemical_formula_sum            'C26 H68 N5 Na Si2 Zn'
_chemical_formula_weight         595.39
_space_group_IT_number           2
_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                81.740(10)
_cell_angle_beta                 78.079(10)
_cell_angle_gamma                83.872(12)
_cell_formula_units_Z            2
_cell_length_a                   9.3269(12)
_cell_length_b                   10.649(2)
_cell_length_c                   19.8598(12)
_cell_measurement_reflns_used    324
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     1904.0(5)
_computing_cell_refinement       DIRAX
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29550
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SHELXTL'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8621
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+1.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                6320
_reflns_number_total             8621
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b713987j.txt
_cod_data_source_block           rem335_compound3
_cod_database_code               7102801