A μ~4~-oxide-containing a dimeric variant of a sodium dialkyl(amido)zincate reagent
Balloch, Liam; Kennedy, Alan R.; Mulvey, Robert E.; Robertson, Stuart D.; Acta Crystallographica Section C 67 (2011) m252–m254; doi:10.1107/S0108270111022645

data_2018164
_publ_section_title
;
 A \m~4~-oxide-containing a dimeric variant of a sodium
 dialkyl(amido)zincate reagent
;
_journal_coeditor_code           WQ3004
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m252
_journal_page_last               m254
_journal_paper_doi               10.1107/S0108270111022645
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Na2 Zn4 (C4 H9)4 (C9 H18 N)2 O2 (C6 H16 N2)2] , 0.59C6 H14'
_chemical_formula_moiety         'C46 H104 N6 Na2 O2 Zn4, 0.59(C6 H14)'
_chemical_formula_sum            'C49.54 H112.26 N6 Na2 O2 Zn4'
_chemical_formula_weight         1131.65
_chemical_name_systematic
;
tetra-<i>tert</i>-butyldi-\m~4~-oxido-bis(tetramethylethylenediamine-
\k^2^<i>N</i>,<i>N</i>')bis(\m~2~-2,2,6,6-tetramethylpiperidin-1-ido-
\k^2^<i>N</i>:<i>N</i>)disodiumtetrazinc hexane 0.59-solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.565(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.3191(12)
_cell_length_b                   18.7841(7)
_cell_length_c                   12.7375(6)
_cell_measurement_reflns_used    13556
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.69
_cell_volume                     6479.5(5)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Oxford Gemini S'
_diffrn_measurement_method       \w
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42490
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.512
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2438
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         7387
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                5153
_reflns_number_total             7387
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wq3004.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2018164
_cod_database_fobs_code          2018164