Homo- and heteroanionic alkali metal aza-enolate aggregates derived from o-methylvalerolactim ether
Andrews, Philip C.; Bull, Steven D.; Koutsaplis, Magdaline; New Journal of Chemistry 34 (2010) 1678–; doi:10.1039/c0nj00088d

data_7053492
_publ_section_title
;
 Homo- and heteroanionic alkali metal aza-enolate aggregates derived from
 o-methylvalerolactim ether
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1678
_journal_paper_doi               10.1039/c0nj00088d
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C38 H78 Li6 N8 O6, C6 H14'
_chemical_formula_sum            'C44 H92 Li6 N8 O6'
_chemical_formula_weight         870.90
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.41(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.235(4)
_cell_length_b                   15.067(3)
_cell_length_c                   18.853(4)
_cell_measurement_reflns_used    23100
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.26
_cell_volume                     5421(2)
_computing_cell_refinement       'DENZO-SMN (Otwinoski & Minor, 1997)'
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'DENZO-SMN (Otwinoski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'CIFTAB (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega 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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23100
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4767
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+3.2270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1460
_reflns_number_gt                3354
_reflns_number_total             4767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00088d.txt
_cod_data_source_block           mag
_cod_original_cell_volume        5421.2(22)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7053492