#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/30/7013011.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_7013011
loop_
_publ_author_name
'Dove, Andrew P.'
'Gibson, Vernon C.'
'Hormnirun, Pimpa'
'Marshall, Edward L.'
'Segal, John A.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Low coordinate magnesium chemistry supported by a bulky ?-diketiminate
 ligand
;
_journal_issue                   15
_journal_name_full               'Dalton Transactions'
_journal_page_first              3088
_journal_paper_doi               10.1039/b303550f
_journal_year                    2003
_chemical_formula_sum            'C39 H56 Mg N2 O'
_chemical_formula_weight         593.17
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 112.124(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3526(6)
_cell_length_b                   19.746(2)
_cell_length_c                   10.4848(6)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      11.12
_cell_volume                     1793.7(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2946
_diffrn_reflns_theta_max         59.98
_diffrn_reflns_theta_min         4.48
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       plates
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0015(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_obs          0.0567
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0876P)²+0.4171P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1604
_refine_ls_wR_factor_obs         0.1421
_reflns_number_observed          2139
_reflns_number_total             2752
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b303550f.txt
_cod_data_source_block           Compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+0.4171P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+0.4171P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_original_formula_sum        'C39 H56 N2 O Mg'
_cod_database_code               7013011
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mg Mg 0.48312(11) 0.7500 0.30348(10) 0.0315(3) Uani 1 d S .
N1 N 0.4770(2) 0.67338(10) 0.1678(2) 0.0333(4) Uani 1 d . .
C1 C 0.5129(2) 0.68537(12) 0.0584(2) 0.0338(5) Uani 1 d . .
C2 C 0.5389(4) 0.7500 0.0162(3) 0.0362(7) Uani 1 d S .
H2A H 0.5811(4) 0.7500 -0.0522(3) 0.043 Uiso 1 calc SR .
C3 C 0.5249(3) 0.62773(14) -0.0324(3) 0.0472(6) Uani 1 d . .
H3A H 0.6284(3) 0.60902(14) 0.0048(3) 0.071 Uiso 1 d R .
H3B H 0.5032(3) 0.64452(14) -0.1247(3) 0.071 Uiso 1 d R .
H3C H 0.4509(3) 0.59275(14) -0.0353(3) 0.071 Uiso 1 d R .
C4 C 0.4259(3) 0.60692(13) 0.1870(2) 0.0387(6) Uani 1 d . .
C5 C 0.5301(3) 0.55543(14) 0.2553(3) 0.0488(6) Uani 1 d . .
C6 C 0.4722(4) 0.4931(2) 0.2755(4) 0.0635(8) Uani 1 d . .
H6A H 0.5412(4) 0.4586(2) 0.3222(4) 0.076 Uiso 1 calc R .
C7 C 0.3155(5) 0.4811(2) 0.2283(4) 0.0712(10) Uani 1 d . .
H7A H 0.2784(5) 0.4383(2) 0.2406(4) 0.085 Uiso 1 calc R .
C8 C 0.2143(4) 0.5318(2) 0.1634(4) 0.0661(9) Uani 1 d . .
H8A H 0.1077(4) 0.5234(2) 0.1333(4) 0.079 Uiso 1 calc R .
C9 C 0.2647(3) 0.59533(14) 0.1406(3) 0.0498(7) Uani 1 d . .
C10 C 0.7037(4) 0.5655(2) 0.3076(4) 0.0618(8) Uani 1 d . .
H10A H 0.7234(4) 0.6114(2) 0.2798(4) 0.074 Uiso 1 calc R .
C11 C 0.7751(6) 0.5618(3) 0.4640(5) 0.117(2) Uani 1 d . .
H11A H 0.8858(6) 0.5683(3) 0.4948(5) 0.176 Uiso 1 calc R .
H11B H 0.7541(6) 0.5178(3) 0.4941(5) 0.176 Uiso 1 calc R .
H11C H 0.7311(6) 0.5969(3) 0.5028(5) 0.176 Uiso 1 calc R .
C12 C 0.7824(4) 0.5145(2) 0.2459(5) 0.0757(10) Uani 1 d . .
H12A H 0.8927(4) 0.5228(2) 0.2822(5) 0.113 Uiso 1 calc R .
H12B H 0.7417(4) 0.5193(2) 0.1465(5) 0.113 Uiso 1 calc R .
H12C H 0.7627(4) 0.4689(2) 0.2698(5) 0.113 Uiso 1 calc R .
C13 C 0.1499(3) 0.6495(2) 0.0665(4) 0.0614(8) Uani 1 d . .
H13A H 0.1996(3) 0.6940(2) 0.0982(4) 0.074 Uiso 1 calc R .
C14 C 0.0027(4) 0.6471(2) 0.0977(5) 0.0839(12) Uani 1 d . .
H14A H -0.0667(4) 0.6829(2) 0.0475(5) 0.126 Uiso 1 calc R .
H14B H 0.0289(4) 0.6532(2) 0.1957(5) 0.126 Uiso 1 calc R .
H14C H -0.0473(4) 0.6035(2) 0.0696(5) 0.126 Uiso 1 calc R .
C15 C 0.1087(5) 0.6456(3) -0.0875(4) 0.0886(13) Uani 1 d . .
H15A H 0.0349(5) 0.6809(3) -0.1328(4) 0.133 Uiso 1 calc R .
H15B H 0.0637(5) 0.6017(3) -0.1210(4) 0.133 Uiso 1 calc R .
H15C H 0.2011(5) 0.6517(3) -0.1073(4) 0.133 Uiso 1 calc R .
C16 C 0.3381(3) 0.7500 0.4199(3) 0.0380(8) Uani 1 d S .
C17 C 0.3052(3) 0.69050(15) 0.4763(3) 0.0443(6) Uani 1 d . .
H17A H 0.3195(3) 0.64874(15) 0.4397(3) 0.053 Uiso 1 calc R .
C18 C 0.2526(3) 0.6902(2) 0.5837(3) 0.0553(8) Uani 1 d . .
H18A H 0.2324(3) 0.6488(2) 0.6180(3) 0.066 Uiso 1 calc R .
C19 C 0.2300(4) 0.7500 0.6402(4) 0.0558(11) Uani 1 d S .
H19A H 0.1995(4) 0.7500 0.7160(4) 0.067 Uiso 1 calc SR .
O20 O 0.6960(3) 0.7334(2) 0.4697(3) 0.046(2) Uani 0.50 d P -1
C21 C 0.8528(5) 0.7385(10) 0.4767(5) 0.052(5) Uani 0.50 d P -1
H21A H 0.9099(5) 0.6979(10) 0.5218(5) 0.062 Uiso 0.50 calc PR -1
H21B H 0.9025(5) 0.7777(10) 0.5335(5) 0.062 Uiso 0.50 calc PR -1
C22 C 0.8619(5) 0.7457(27) 0.3406(5) 0.052(4) Uani 0.50 d P -1
H22A H 0.9692(5) 0.7488(27) 0.3510(5) 0.077 Uiso 1 calc SR -1
H22B H 0.8076(5) 0.7863(27) 0.2963(5) 0.077 Uiso 0.50 calc PR -1
H22C H 0.8149(5) 0.7065(27) 0.2845(5) 0.077 Uiso 0.50 calc PR -1
C23 C 0.6963(6) 0.7174(4) 0.6043(6) 0.057(2) Uani 0.50 d P -1
H23A H 0.7826(6) 0.6867(4) 0.6512(6) 0.069 Uiso 0.50 calc PR -1
H23B H 0.6006(6) 0.6935(4) 0.5932(6) 0.069 Uiso 0.50 calc PR -1
C24 C 0.7101(7) 0.7778(4) 0.6918(8) 0.073(2) Uani 0.50 d P -1
H24A H 0.7097(7) 0.7639(4) 0.7803(8) 0.110 Uiso 0.50 calc PR -1
H24B H 0.6237(7) 0.8080(4) 0.6471(8) 0.110 Uiso 0.50 calc PR -1
H24C H 0.8058(7) 0.8012(4) 0.7051(8) 0.110 Uiso 0.50 calc PR -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 '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
N1 Mg N1 94.36(12) . 4_575 ?
N1 Mg O20 103.13(12) . . ?
N1 Mg O20 116.97(12) 4_575 . ?
N1 Mg O20 116.97(12) . 4_575 ?
N1 Mg O20 103.13(12) 4_575 4_575 ?
O20 Mg O20 17.8(2) . 4_575 ?
N1 Mg C16 122.32(7) . . ?
N1 Mg C16 122.32(7) 4_575 . ?
O20 Mg C16 97.59(12) . . ?
O20 Mg C16 97.59(12) 4_575 . ?
C1 N1 C4 119.2(2) . . ?
C1 N1 Mg 120.9(2) . . ?
C4 N1 Mg 119.82(14) . . ?
N1 C1 C2 124.3(2) . . ?
N1 C1 C3 120.6(2) . . ?
C2 C1 C3 115.0(2) . . ?
C1 C2 C1 131.2(3) 4_575 . ?
C5 C4 C9 120.2(2) . . ?
C5 C4 N1 122.0(2) . . ?
C9 C4 N1 117.8(2) . . ?
C6 C5 C4 118.8(3) . . ?
C6 C5 C10 119.0(3) . . ?
C4 C5 C10 122.2(2) . . ?
C7 C6 C5 121.3(3) . . ?
C8 C7 C6 119.6(3) . . ?
C7 C8 C9 121.9(3) . . ?
C8 C9 C4 118.1(3) . . ?
C8 C9 C13 120.4(3) . . ?
C4 C9 C13 121.4(2) . . ?
C5 C10 C11 111.0(4) . . ?
C5 C10 C12 112.4(3) . . ?
C11 C10 C12 109.8(3) . . ?
C9 C13 C15 111.0(3) . . ?
C9 C13 C14 113.0(3) . . ?
C15 C13 C14 109.8(3) . . ?
C17 C16 C17 114.0(3) . 4_575 ?
C17 C16 Mg 121.9(2) . . ?
C17 C16 Mg 121.9(2) 4_575 . ?
C18 C17 C16 123.2(3) . . ?
C19 C18 C17 120.4(3) . . ?
C18 C19 C18 118.7(3) 4_575 . ?
C21 O20 C23 109.7(4) . . ?
C21 O20 Mg 130.8(4) . . ?
C23 O20 Mg 119.5(3) . . ?
O20 C21 C22 112.7(4) . . ?
O20 C23 C24 113.3(5) . . ?
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
Mg N1 2.063(2) . ?
Mg N1 2.063(2) 4_575 ?
Mg O20 2.120(3) . ?
Mg O20 2.120(3) 4_575 ?
Mg C16 2.139(3) . ?
N1 C1 1.332(3) . ?
N1 C4 1.437(3) . ?
C1 C2 1.401(3) . ?
C1 C3 1.515(3) . ?
C2 C1 1.401(3) 4_575 ?
C4 C5 1.404(4) . ?
C4 C9 1.418(4) . ?
C5 C6 1.393(4) . ?
C5 C10 1.518(4) . ?
C6 C7 1.379(5) . ?
C7 C8 1.370(5) . ?
C8 C9 1.392(4) . ?
C9 C13 1.508(5) . ?
C10 C11 1.522(5) . ?
C10 C12 1.527(5) . ?
C13 C15 1.514(5) . ?
C13 C14 1.531(4) . ?
C16 C17 1.401(3) . ?
C16 C17 1.401(3) 4_575 ?
C17 C18 1.389(4) . ?
C18 C19 1.372(4) . ?
C19 C18 1.372(4) 4_575 ?
O20 C21 1.444(5) . ?
O20 C23 1.445(7) . ?
C21 C22 1.469(9) . ?
C23 C24 1.481(9) . ?
