#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:38:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179120 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/82/4308296.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4308296
loop_
_publ_author_name
'Martin Gärtner'
'Reinald Fischer'
'Jens Langer'
'Helmar Görls'
'Dirk Walther'
'Matthias Westerhausen'
_publ_contact_author
;
      Matthias Westerhausen
      Institut für anorganische und analytische Chemie
      Friedrich-Schiller-Universität 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
_chemical_name_systematic
; 
 ? 
;
_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/[σ²(Fo²)+(0.1911P)²+3.5971P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
MgA Mg 0.7500 0.68451(10) 0.7500 0.0298(4) Uani 1 2 d S . .
O1A O 0.64810(18) 0.59103(16) 0.69333(12) 0.0364(5) Uani 1 1 d . . .
N1A N 0.8336(2) 0.7467(2) 0.69182(14) 0.0346(6) Uani 1 1 d . . .
C1A C 0.8205(3) 0.7047(2) 0.62544(16) 0.0343(7) Uani 1 1 d . . .
C2A C 0.7232(3) 0.7141(3) 0.57465(18) 0.0418(8) Uani 1 1 d . . .
H2AA H 0.6703 0.7532 0.5836 0.050 Uiso 1 1 calc R . .
C3A C 0.7023(4) 0.6673(3) 0.51137(19) 0.0536(10) Uani 1 1 d . . .
H3AA H 0.6350 0.6734 0.4780 0.064 Uiso 1 1 calc R . .
C4A C 0.7790(4) 0.6117(3) 0.4965(2) 0.0556(11) Uani 1 1 d . . .
H4AA H 0.7653 0.5809 0.4527 0.067 Uiso 1 1 calc R . .
C5A C 0.8757(4) 0.6015(3) 0.5460(2) 0.0536(10) Uani 1 1 d . . .
H5AA H 0.9280 0.5623 0.5362 0.064 Uiso 1 1 calc R . .
C6A C 0.8982(3) 0.6475(3) 0.61011(19) 0.0431(8) Uani 1 1 d . . .
H6AA H 0.9656 0.6404 0.6433 0.052 Uiso 1 1 calc R . .
C7A C 0.9204(3) 0.8043(2) 0.71881(17) 0.0329(7) Uani 1 1 d . . .
C8A C 0.9924(3) 0.8332(3) 0.6822(2) 0.0420(8) Uani 1 1 d . . .
H8AA H 0.9841 0.8121 0.6357 0.050 Uiso 1 1 calc R . .
C9A C 1.0761(3) 0.8928(3) 0.7135(2) 0.0493(9) Uani 1 1 d . . .
H9AA H 1.1236 0.9113 0.6876 0.059 Uiso 1 1 calc R . .
C10A C 1.0914(3) 0.9252(3) 0.7802(2) 0.0500(10) Uani 1 1 d . . .
H10A H 1.1491 0.9653 0.8008 0.060 Uiso 1 1 calc R . .
C11A C 1.0217(3) 0.8985(3) 0.8169(2) 0.0465(9) Uani 1 1 d . . .
H11A H 1.0315 0.9205 0.8633 0.056 Uiso 1 1 calc R . .
C12A C 0.9363(3) 0.8393(2) 0.78705(18) 0.0394(8) Uani 1 1 d . . .
H12A H 0.8885 0.8226 0.8133 0.047 Uiso 1 1 calc R . .
C13A C 0.5346(3) 0.5889(3) 0.6816(2) 0.0433(8) Uani 1 1 d . . .
H13A H 0.5072 0.6507 0.6889 0.052 Uiso 1 1 calc R . .
H13B H 0.5144 0.5441 0.7133 0.052 Uiso 1 1 calc R . .
C14A C 0.4927(3) 0.5592(3) 0.6062(2) 0.0536(10) Uani 1 1 d . . .
H14A H 0.4855 0.6127 0.5742 0.064 Uiso 1 1 calc R . .
H14B H 0.4229 0.5284 0.5979 0.064 Uiso 1 1 calc R . .
C15A C 0.5767(3) 0.4918(3) 0.5960(2) 0.0495(9) Uani 1 1 d . . .
H15A H 0.5926 0.5033 0.5509 0.059 Uiso 1 1 calc R . .
H15B H 0.5523 0.4271 0.5967 0.059 Uiso 1 1 calc R . .
C16A C 0.6742(3) 0.5100(3) 0.65738(19) 0.0428(8) Uani 1 1 d . . .
H16A H 0.6895 0.4560 0.6893 0.051 Uiso 1 1 calc R . .
H16B H 0.7371 0.5223 0.6404 0.051 Uiso 1 1 calc R . .
MgB Mg 0.7500 0.19632(10) 0.7500 0.0302(4) Uani 1 2 d S . .
O1B O 0.70672(19) 0.10212(17) 0.81129(13) 0.0414(6) Uani 1 1 d . . .
N1B N 0.6138(2) 0.25951(19) 0.69743(14) 0.0329(6) Uani 1 1 d . . .
C1B C 0.5529(2) 0.3116(2) 0.72983(16) 0.0313(7) Uani 1 1 d . . .
C2B C 0.5999(3) 0.3455(2) 0.79762(18) 0.0392(8) Uani 1 1 d . . .
H2BA H 0.6721 0.3312 0.8199 0.047 Uiso 1 1 calc R . .
C3B C 0.5437(4) 0.3993(3) 0.8330(2) 0.0491(9) Uani 1 1 d . . .
H3BA H 0.5777 0.4202 0.8791 0.059 Uiso 1 1 calc R . .
C4B C 0.4383(3) 0.4228(3) 0.8017(2) 0.0508(10) Uani 1 1 d . . .
H4BA H 0.3998 0.4596 0.8259 0.061 Uiso 1 1 calc R . .
C5B C 0.3918(3) 0.3918(3) 0.7357(2) 0.0465(9) Uani 1 1 d . . .
H5BA H 0.3200 0.4077 0.7138 0.056 Uiso 1 1 calc R . .
C6B C 0.4463(3) 0.3374(2) 0.69919(18) 0.0374(7) Uani 1 1 d . . .
H6BA H 0.4112 0.3175 0.6530 0.045 Uiso 1 1 calc R . .
C7B C 0.5636(2) 0.2175(2) 0.63262(16) 0.0322(7) Uani 1 1 d . . .
C8B C 0.6037(3) 0.2318(3) 0.57494(18) 0.0402(8) Uani 1 1 d . . .
H8BA H 0.6604 0.2742 0.5789 0.048 Uiso 1 1 calc R . .
C9B C 0.5624(3) 0.1856(3) 0.51245(19) 0.0465(9) Uani 1 1 d . . .
H9BA H 0.5912 0.1961 0.4742 0.056 Uiso 1 1 calc R . .
C10B C 0.4793(3) 0.1241(3) 0.5053(2) 0.0477(9) Uani 1 1 d . . .
H10B H 0.4511 0.0922 0.4624 0.057 Uiso 1 1 calc R . .
C11B C 0.4376(3) 0.1094(3) 0.5610(2) 0.0457(9) Uani 1 1 d . . .
H11B H 0.3802 0.0675 0.5561 0.055 Uiso 1 1 calc R . .
C12B C 0.4788(3) 0.1552(2) 0.62397(18) 0.0402(8) Uani 1 1 d . . .
H12B H 0.4492 0.1443 0.6618 0.048 Uiso 1 1 calc R . .
C13B C 0.7647(3) 0.0190(3) 0.8409(3) 0.0566(11) Uani 1 1 d . . .
H13C H 0.8422 0.0297 0.8525 0.068 Uiso 1 1 calc R . .
H13D H 0.7462 -0.0330 0.8072 0.068 Uiso 1 1 calc R . .
C14B C 0.7321(3) -0.0021(3) 0.9056(2) 0.0554(10) Uani 1 1 d . . .
H14C H 0.7890 0.0151 0.9480 0.067 Uiso 1 1 calc R . .
H14D H 0.7162 -0.0687 0.9079 0.067 Uiso 1 1 calc R . .
C15B C 0.6329(4) 0.0561(3) 0.8995(2) 0.0557(10) Uani 1 1 d . . .
H15C H 0.5738 0.0171 0.9052 0.067 Uiso 1 1 calc R . .
H15D H 0.6470 0.1054 0.9354 0.067 Uiso 1 1 calc R . .
C16B C 0.6072(3) 0.0963(3) 0.8278(2) 0.0539(11) Uani 1 1 d . . .
H16C H 0.5571 0.0560 0.7938 0.065 Uiso 1 1 calc R . .
H16D H 0.5749 0.1583 0.8269 0.065 Uiso 1 1 calc R . .
O1TB O 1.1843(7) 0.5878(5) 0.5967(4) 0.080(2) Uani 0.50 1 d P . .
C1TB C 1.1782(8) 0.6449(6) 0.5399(4) 0.058(2) Uani 0.50 1 d P . .
H1TA H 1.1096 0.6369 0.5038 0.069 Uiso 0.50 1 calc PR . .
H1TB H 1.2367 0.6319 0.5188 0.069 Uiso 0.50 1 calc PR . .
C2TB C 1.1887(7) 0.7507(9) 0.5735(5) 0.074(3) Uani 0.50 1 d P . .
H2TA H 1.2250 0.7941 0.5492 0.089 Uiso 0.50 1 calc PR . .
H2TB H 1.1195 0.7766 0.5750 0.089 Uiso 0.50 1 calc PR . .
C3TB C 1.2567(6) 0.7232(4) 0.6442(4) 0.0400(15) Uani 0.50 1 d P . .
H3TA H 1.3325 0.7259 0.6451 0.048 Uiso 0.50 1 calc PR . .
H3TB H 1.2453 0.7663 0.6802 0.048 Uiso 0.50 1 calc PR . .
C4TB C 1.2292(7) 0.6297(6) 0.6594(5) 0.054(2) Uani 0.50 1 d P . .
H4TA H 1.2934 0.5956 0.6855 0.065 Uiso 0.50 1 calc PR . .
H4TB H 1.1784 0.6310 0.6881 0.065 Uiso 0.50 1 calc PR . .
O1TA O 0.3458(5) 0.0611(4) 0.9156(4) 0.070(2) Uani 0.50 1 d P . .
C1TA C 0.3920(7) 0.1368(6) 0.9649(3) 0.052(2) Uani 0.50 1 d P . .
H1TC H 0.3407 0.1585 0.9897 0.062 Uiso 0.50 1 calc PR . .
H1TD H 0.4574 0.1158 1.0000 0.062 Uiso 0.50 1 calc PR . .
C2TA C 0.4159(7) 0.2098(5) 0.9213(4) 0.0474(19) Uani 0.50 1 d P . .
H2TC H 0.4883 0.2025 0.9159 0.057 Uiso 0.50 1 calc PR . .
H2TD H 0.4100 0.2715 0.9415 0.057 Uiso 0.50 1 calc PR . .
C3TA C 0.3363(8) 0.1980(8) 0.8548(6) 0.083(4) Uani 0.50 1 d P . .
H3TC H 0.2708 0.2321 0.8545 0.100 Uiso 0.50 1 calc PR . .
H3TD H 0.3629 0.2211 0.8159 0.100 Uiso 0.50 1 calc PR . .
C4TA C 0.3161(7) 0.1029(7) 0.8476(4) 0.063(3) Uani 0.50 1 d P . .
H4TC H 0.3574 0.0751 0.8179 0.075 Uiso 0.50 1 calc PR . .
H4TD H 0.2398 0.0921 0.8248 0.075 Uiso 0.50 1 calc PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1A MgA O1A 95.54(15) . 2_656 ?
O1A MgA N1A 111.24(10) . . ?
O1A MgA N1A 103.81(10) 2_656 . ?
O1A MgA N1A 103.81(10) . 2_656 ?
O1A MgA N1A 111.23(10) 2_656 2_656 ?
N1A MgA N1A 126.89(18) . 2_656 ?
C13A O1A C16A 106.0(3) . . ?
C13A O1A MgA 126.9(2) . . ?
C16A O1A MgA 127.1(2) . . ?
C7A N1A C1A 119.3(3) . . ?
C7A N1A MgA 124.3(2) . . ?
C1A N1A MgA 113.4(2) . . ?
C2A C1A C6A 118.1(3) . . ?
C2A C1A N1A 118.7(3) . . ?
C6A C1A N1A 123.0(3) . . ?
C3A C2A C1A 121.2(4) . . ?
C4A C3A C2A 120.4(4) . . ?
C5A C4A C3A 119.4(4) . . ?
C4A C5A C6A 121.2(4) . . ?
C5A C6A C1A 119.7(4) . . ?
N1A C7A C8A 125.0(3) . . ?
N1A C7A C12A 118.2(3) . . ?
C8A C7A C12A 116.8(3) . . ?
C9A C8A C7A 120.6(4) . . ?
C10A C9A C8A 121.9(4) . . ?
C9A C10A C11A 118.5(4) . . ?
C10A C11A C12A 121.2(4) . . ?
C11A C12A C7A 120.9(3) . . ?
O1A C13A C14A 104.0(3) . . ?
C13A C14A C15A 103.7(3) . . ?
C14A C15A C16A 105.1(3) . . ?
O1A C16A C15A 105.7(3) . . ?
O1B MgB O1B 94.71(16) 2_656 . ?
O1B MgB N1B 105.19(10) 2_656 2_656 ?
O1B MgB N1B 110.54(11) . 2_656 ?
O1B MgB N1B 110.55(11) 2_656 . ?
O1B MgB N1B 105.19(10) . . ?
N1B MgB N1B 126.20(17) 2_656 . ?
C16B O1B C13B 105.4(3) . . ?
C16B O1B MgB 127.3(2) . . ?
C13B O1B MgB 126.9(2) . . ?
C1B N1B C7B 118.5(3) . . ?
C1B N1B MgB 123.3(2) . . ?
C7B N1B MgB 113.5(2) . . ?
N1B C1B C2B 118.7(3) . . ?
N1B C1B C6B 125.1(3) . . ?
C2B C1B C6B 116.1(3) . . ?
C3B C2B C1B 121.8(3) . . ?
C2B C3B C4B 120.7(4) . . ?
C5B C4B C3B 118.3(4) . . ?
C4B C5B C6B 122.0(4) . . ?
C5B C6B C1B 121.0(3) . . ?
C8B C7B C12B 117.3(3) . . ?
C8B C7B N1B 119.7(3) . . ?
C12B C7B N1B 122.8(3) . . ?
C9B C8B C7B 121.4(3) . . ?
C10B C9B C8B 120.3(4) . . ?
C11B C10B C9B 119.5(3) . . ?
C10B C11B C12B 120.6(4) . . ?
C11B C12B C7B 120.9(3) . . ?
O1B C13B C14B 105.9(3) . . ?
C13B C14B C15B 105.1(3) . . ?
C16B C15B C14B 104.7(3) . . ?
O1B C16B C15B 105.2(3) . . ?
C4TB O1TB C1TB 113.2(7) . . ?
O1TB C1TB C2TB 104.1(6) . . ?
C3TB C2TB C1TB 95.3(7) . . ?
C4TB C3TB C2TB 109.0(7) . . ?
O1TB C4TB C3TB 107.0(8) . . ?
C4TA O1TA C1TA 105.4(6) . . ?
C2TA C1TA O1TA 105.0(5) . . ?
C1TA C2TA C3TA 103.7(7) . . ?
C4TA C3TA C2TA 106.1(6) . . ?
C3TA C4TA O1TA 108.9(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
MgA O1A 2.012(2) . ?
MgA O1A 2.012(2) 2_656 ?
MgA N1A 2.013(3) . ?
MgA N1A 2.013(3) 2_656 ?
O1A C13A 1.442(4) . ?
O1A C16A 1.462(4) . ?
N1A C7A 1.392(4) . ?
N1A C1A 1.419(4) . ?
C1A C2A 1.397(5) . ?
C1A C6A 1.410(5) . ?
C2A C3A 1.387(5) . ?
C3A C4A 1.381(7) . ?
C4A C5A 1.380(7) . ?
C5A C6A 1.395(5) . ?
C7A C8A 1.406(5) . ?
C7A C12A 1.408(5) . ?
C8A C9A 1.398(5) . ?
C9A C10A 1.369(6) . ?
C10A C11A 1.373(6) . ?
C11A C12A 1.405(5) . ?
C13A C14A 1.508(5) . ?
C14A C15A 1.526(6) . ?
C15A C16A 1.526(5) . ?
MgB O1B 2.011(3) 2_656 ?
MgB O1B 2.011(3) . ?
MgB N1B 2.020(3) 2_656 ?
MgB N1B 2.020(3) . ?
O1B C16B 1.434(4) . ?
O1B C13B 1.457(4) . ?
N1B C1B 1.381(4) . ?
N1B C7B 1.411(4) . ?
C1B C2B 1.405(5) . ?
C1B C6B 1.411(5) . ?
C2B C3B 1.390(5) . ?
C3B C4B 1.391(6) . ?
C4B C5B 1.360(6) . ?
C5B C6B 1.394(5) . ?
C7B C8B 1.403(5) . ?
C7B C12B 1.404(5) . ?
C8B C9B 1.382(5) . ?
C9B C10B 1.383(6) . ?
C10B C11B 1.380(6) . ?
C11B C12B 1.386(5) . ?
C13B C14B 1.494(6) . ?
C14B C15B 1.526(6) . ?
C15B C16B 1.489(6) . ?
O1TB C4TB 1.363(11) . ?
O1TB C1TB 1.382(12) . ?
C1TB C2TB 1.660(15) . ?
C2TB C3TB 1.495(11) . ?
C3TB C4TB 1.453(11) . ?
O1TA C4TA 1.433(12) . ?
O1TA C1TA 1.482(11) . ?
C1TA C2TA 1.455(11) . ?
C2TA C3TA 1.450(14) . ?
C3TA C4TA 1.400(15) . ?
