#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/30/7013012.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_7013012
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            'C35 H46 Mg N2'
_chemical_formula_weight         519.05
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8417(9)
_cell_length_b                   20.974(3)
_cell_length_c                   9.1888(4)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      10.58
_cell_volume                     3245.8(5)
_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      183(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2776
_diffrn_reflns_theta_max         64.00
_diffrn_reflns_theta_min         4.22
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.47
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_restrained_S_obs      1.049
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_obs          0.0445
_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)+(0.0582P)²+1.2396P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1284
_refine_ls_wR_factor_obs         0.1117
_reflns_number_observed          2331
_reflns_number_total             2776
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b303550f.txt
_cod_data_source_block           Compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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^)+(0.0582P)^2^+1.2396P] 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^)+(0.0582P)^2^+1.2396P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3245.9(6)
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C35 H46 N2 Mg'
_cod_database_code               7013012
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mg Mg 0.11499(5) 0.2500 0.11299(9) 0.0346(2) Uani 1 d S .
N1 N 0.17578(8) 0.31971(6) 0.2110(2) 0.0308(3) Uani 1 d . .
C1 C 0.23713(10) 0.31040(7) 0.2996(2) 0.0317(4) Uani 1 d . .
C2 C 0.26741(14) 0.2500 0.3352(3) 0.0354(6) Uani 1 d S .
H2A H 0.31492(14) 0.2500 0.3909(3) 0.043 Uiso 1 calc SR .
C3 C 0.27620(11) 0.36688(8) 0.3716(2) 0.0430(5) Uani 1 d . .
H3A H 0.32501(11) 0.35303(8) 0.4203(2) 0.064 Uiso 1 d R .
H3B H 0.23987(11) 0.38534(8) 0.4435(2) 0.064 Uiso 1 d R .
H3C H 0.28912(11) 0.39899(8) 0.2978(2) 0.064 Uiso 1 d R .
C4 C 0.14341(10) 0.38286(7) 0.1910(2) 0.0325(4) Uani 1 d . .
C5 C 0.17268(10) 0.42195(8) 0.0794(2) 0.0389(4) Uani 1 d . .
C6 C 0.13416(13) 0.48005(9) 0.0543(3) 0.0515(5) Uani 1 d . .
H6A H 0.15298(13) 0.50735(9) -0.0206(3) 0.062 Uiso 1 calc R .
C7 C 0.06980(13) 0.49839(8) 0.1356(3) 0.0551(6) Uani 1 d . .
H7A H 0.04449(13) 0.53802(8) 0.1167(3) 0.066 Uiso 1 calc R .
C8 C 0.04194(12) 0.45936(9) 0.2445(3) 0.0509(5) Uani 1 d . .
H8A H -0.00273(12) 0.47246(9) 0.3001(3) 0.061 Uiso 1 calc R .
C9 C 0.07786(11) 0.40097(8) 0.2750(2) 0.0406(4) Uani 1 d . .
C10 C 0.24101(12) 0.40137(9) -0.0170(2) 0.0469(5) Uani 1 d . .
H10A H 0.26814(12) 0.36492(9) 0.0325(2) 0.056 Uiso 1 calc R .
C11 C 0.2099(2) 0.3770(2) -0.1624(3) 0.0864(9) Uani 1 d . .
H11A H 0.2547(2) 0.3638(2) -0.2236(3) 0.130 Uiso 1 calc R .
H11B H 0.1803(2) 0.4110(2) -0.2113(3) 0.130 Uiso 1 calc R .
H11C H 0.1748(2) 0.3404(2) -0.1458(3) 0.130 Uiso 1 calc R .
C12 C 0.30273(14) 0.45370(11) -0.0391(3) 0.0776(8) Uani 1 d . .
H12A H 0.34536(14) 0.43784(11) -0.1020(3) 0.116 Uiso 1 calc R .
H12B H 0.32491(14) 0.46612(11) 0.0553(3) 0.116 Uiso 1 calc R .
H12C H 0.27757(14) 0.49077(11) -0.0848(3) 0.116 Uiso 1 calc R .
C13 C 0.04547(13) 0.35970(10) 0.3965(3) 0.0558(5) Uani 1 d . .
H13A H 0.07907(13) 0.32049(10) 0.4030(3) 0.067 Uiso 1 calc R .
C14 C -0.0396(2) 0.33915(13) 0.3685(3) 0.0778(8) Uani 1 d . .
H14A H -0.0581(2) 0.31264(13) 0.4495(3) 0.117 Uiso 1 calc R .
H14B H -0.0421(2) 0.31460(13) 0.2779(3) 0.117 Uiso 1 calc R .
H14C H -0.0735(2) 0.37695(13) 0.3601(3) 0.117 Uiso 1 calc R .
C15 C 0.0500(2) 0.3945(2) 0.5426(3) 0.0905(10) Uani 1 d . .
H15A H 0.0288(2) 0.3670(2) 0.6195(3) 0.136 Uiso 1 calc R .
H15B H 0.0187(2) 0.4338(2) 0.5376(3) 0.136 Uiso 1 calc R .
H15C H 0.1055(2) 0.4050(2) 0.5642(3) 0.136 Uiso 1 calc R .
C16 C 0.01778(14) 0.2500 -0.0292(3) 0.0368(6) Uani 1 d S .
C17 C -0.01702(11) 0.30627(9) -0.0802(2) 0.0448(5) Uani 1 d . .
H17A H 0.00404(11) 0.34588(9) -0.0483(2) 0.054 Uiso 1 calc R .
C18 C -0.08071(12) 0.30683(10) -0.1752(2) 0.0523(5) Uani 1 d . .
H18A H -0.10229(12) 0.34624(10) -0.2073(2) 0.063 Uiso 1 calc R .
C19 C -0.1130(2) 0.2500 -0.2233(3) 0.0543(8) Uani 1 d S .
H19A H -0.1567(2) 0.2500 -0.2886(3) 0.065 Uiso 1 calc SR .
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'
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 93.99(8) . 7_565 ?
N1 Mg C16 132.94(4) . . ?
N1 Mg C16 132.94(4) 7_565 . ?
C1 N1 C4 120.38(13) . . ?
C1 N1 Mg 124.49(10) . . ?
C4 N1 Mg 114.85(10) . . ?
N1 C1 C2 123.8(2) . . ?
N1 C1 C3 119.49(14) . . ?
C2 C1 C3 116.6(2) . . ?
C1 C2 C1 128.9(2) 7_565 . ?
C9 C4 C5 121.46(15) . . ?
C9 C4 N1 118.5(2) . . ?
C5 C4 N1 119.8(2) . . ?
C6 C5 C4 117.8(2) . . ?
C6 C5 C10 120.3(2) . . ?
C4 C5 C10 121.87(15) . . ?
C7 C6 C5 121.4(2) . . ?
C6 C7 C8 119.9(2) . . ?
C7 C8 C9 121.4(2) . . ?
C8 C9 C4 118.0(2) . . ?
C8 C9 C13 119.6(2) . . ?
C4 C9 C13 122.4(2) . . ?
C5 C10 C11 110.3(2) . . ?
C5 C10 C12 113.0(2) . . ?
C11 C10 C12 111.1(2) . . ?
C9 C13 C14 112.2(2) . . ?
C9 C13 C15 110.8(2) . . ?
C14 C13 C15 109.4(2) . . ?
C17 C16 C17 115.1(2) 7_565 . ?
C17 C16 Mg 122.46(12) 7_565 . ?
C17 C16 Mg 122.46(12) . . ?
C18 C17 C16 122.9(2) . . ?
C17 C18 C19 120.0(2) . . ?
C18 C19 C18 119.1(3) . 7_565 ?
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 1.9992(14) . ?
Mg N1 1.9992(14) 7_565 ?
Mg C16 2.095(3) . ?
N1 C1 1.330(2) . ?
N1 C4 1.444(2) . ?
C1 C2 1.404(2) . ?
C1 C3 1.508(2) . ?
C2 C1 1.404(2) 7_565 ?
C4 C9 1.399(3) . ?
C4 C5 1.403(2) . ?
C5 C6 1.400(2) . ?
C5 C10 1.515(3) . ?
C6 C7 1.371(3) . ?
C7 C8 1.375(3) . ?
C8 C9 1.394(3) . ?
C9 C13 1.514(3) . ?
C10 C11 1.523(3) . ?
C10 C12 1.525(3) . ?
C13 C14 1.518(3) . ?
C13 C15 1.530(3) . ?
C16 C17 1.399(2) 7_565 ?
C16 C17 1.399(2) . ?
C17 C18 1.383(3) . ?
C18 C19 1.383(3) . ?
C19 C18 1.383(3) 7_565 ?
