Syntheses and Structures of Alkaline Earth Metal Bis(diphenylamides)
Martin Gärtner; Reinald Fischer; Jens Langer; Helmar Görls; Dirk Walther; Matthias Westerhausen; Inorganic Chemistry 46 (2007) 5118–5124; doi:10.1021/ic700459d

data_4308296
_publ_contact_author
;
      Matthias Westerhausen
      Institut f\"ur anorganische und analytische Chemie
      Friedrich-Schiller-Universit\"at Jena
      August-Bebel-Str. 2
      07743 Jena
      Germany
;
_publ_contact_author_email       m.we@uni-jena.de
_publ_contact_author_fax         '03641 948 102'
_publ_contact_author_phone       '03641 948 110'
_publ_section_title
;
Syntheses and Structures of Alkaline Earth Metal Bis(diphenylamides)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5118
_journal_page_last               5124
_journal_paper_doi               10.1021/ic700459d
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C36 H44 Mg N2 O3'
_chemical_formula_weight         577.04
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 106.111(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1143(4)
_cell_length_b                   14.4644(5)
_cell_length_c                   19.8690(4)
_cell_measurement_temperature    183(2)
_cell_volume                     3620.94(19)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24242
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.0119
_exptl_absorpt_correction_T_min  0.9573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.423
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1911P)^2^+3.5971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2771
_refine_ls_wR_factor_ref         0.3199
_reflns_number_gt                5307
_reflns_number_total             8274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700459d-file001_2.cif
_cod_data_source_block           FO3051
_cod_original_cell_volume        3620.94(18)
_cod_database_code               4308296