#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/21/4302124.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_4302124
loop_
_publ_author_name
'Anthony G. M. Barrett'
'Ian J. Casely'
'Mark R. Crimmin'
'Michael S. Hill'
'Jennifer R. Lachs'
'Mary F. Mahon'
'Panayiotis A. Procopiou'
_publ_section_title
;
β-Diketiminato Calcium and Magnesium Amides; Model Complexes for
Hydroamination Catalysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4445
_journal_page_last               4453
_journal_paper_doi               10.1021/ic900091x
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C36 H49 Mg N3'
_chemical_formula_weight         548.09
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.145(1)
_cell_angle_beta                 110.902(1)
_cell_angle_gamma                111.107(1)
_cell_formula_units_Z            2
_cell_length_a                   11.6669(2)
_cell_length_b                   12.9052(2)
_cell_length_c                   13.0838(2)
_cell_measurement_reflns_used    29413
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1620.79(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  '95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       CCD
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33768
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         7400
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0532
_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/[σ²(Fo²)+(0.0674P)²+0.9153P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                5772
_reflns_number_total             7400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900091x_si_001_1.cif
_cod_data_source_block           k08msh27
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' 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 
;
_cod_original_cell_volume        1620.79(4)
_cod_database_code               4302124
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_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
Mg1 Mg -0.07309(5) 0.49225(5) 0.37559(4) 0.02225(14) Uani 1 1 d . . .
N1 N -0.02205(14) 0.60027(11) 0.27798(12) 0.0234(3) Uani 1 1 d . . .
N2 N -0.25767(14) 0.36839(12) 0.23316(12) 0.0232(3) Uani 1 1 d . . .
N3 N 0.05553(16) 0.42108(13) 0.46356(13) 0.0306(3) Uani 1 1 d D . .
C1 C 0.1614(2) 0.40742(18) 0.43685(18) 0.0401(5) Uani 1 1 d . . .
H1A H 0.2174 0.3865 0.4991 0.048 Uiso 1 1 calc R . .
H1B H 0.2230 0.4841 0.4371 0.048 Uiso 1 1 calc R . .
C2 C 0.10666(19) 0.31455(17) 0.32078(17) 0.0340(4) Uani 1 1 d . . .
C3 C 0.1200(2) 0.21223(19) 0.31416(19) 0.0420(5) Uani 1 1 d . . .
H3A H 0.1686 0.2004 0.3833 0.050 Uiso 1 1 calc R . .
C4 C 0.0633(2) 0.1257(2) 0.2076(2) 0.0469(5) Uani 1 1 d . . .
H4 H 0.0731 0.0555 0.2045 0.056 Uiso 1 1 calc R . .
C5 C -0.0071(3) 0.1421(2) 0.1066(2) 0.0490(5) Uani 1 1 d . . .
H5 H -0.0466 0.0831 0.0338 0.059 Uiso 1 1 calc R . .
C6 C -0.0193(2) 0.2451(2) 0.11266(19) 0.0461(5) Uani 1 1 d . . .
H6 H -0.0673 0.2572 0.0435 0.055 Uiso 1 1 calc R . .
C7 C 0.0379(2) 0.33130(18) 0.21892(18) 0.0404(5) Uani 1 1 d . . .
H7 H 0.0299 0.4023 0.2218 0.048 Uiso 1 1 calc R . .
C8 C -0.07716(18) 0.55495(15) 0.16286(14) 0.0263(3) Uani 1 1 d . . .
C9 C -0.18411(18) 0.44183(15) 0.09623(14) 0.0286(4) Uani 1 1 d . . .
H9 H -0.1988 0.4160 0.0185 0.034 Uiso 1 1 calc R . .
C10 C -0.27338(17) 0.36031(14) 0.12607(14) 0.0264(3) Uani 1 1 d . . .
C11 C -0.0264(2) 0.62679(17) 0.09318(16) 0.0369(4) Uani 1 1 d . . .
H11A H -0.0237 0.7041 0.1160 0.055 Uiso 1 1 calc R . .
H11B H -0.0888 0.5858 0.0104 0.055 Uiso 1 1 calc R . .
H11C H 0.0662 0.6370 0.1081 0.055 Uiso 1 1 calc R . .
C12 C -0.3964(2) 0.25787(17) 0.02285(15) 0.0372(4) Uani 1 1 d . . .
H12A H -0.4788 0.2400 0.0348 0.056 Uiso 1 1 calc R . .
H12B H -0.3795 0.1886 0.0151 0.056 Uiso 1 1 calc R . .
H12C H -0.4103 0.2790 -0.0478 0.056 Uiso 1 1 calc R . .
C13 C 0.06214(17) 0.72610(14) 0.32537(14) 0.0249(3) Uani 1 1 d . . .
C14 C 0.20372(18) 0.77718(15) 0.35712(15) 0.0290(4) Uani 1 1 d . . .
C15 C 0.2776(2) 0.89987(16) 0.39814(17) 0.0358(4) Uani 1 1 d . . .
H15 H 0.3734 0.9354 0.4198 0.043 Uiso 1 1 calc R . .
C16 C 0.2145(2) 0.97027(16) 0.40775(18) 0.0381(4) Uani 1 1 d . . .
H16 H 0.2666 1.0535 0.4355 0.046 Uiso 1 1 calc R . .
C17 C 0.0758(2) 0.91991(15) 0.37699(17) 0.0355(4) Uani 1 1 d . . .
H17 H 0.0330 0.9691 0.3843 0.043 Uiso 1 1 calc R . .
C18 C -0.00330(18) 0.79755(15) 0.33510(15) 0.0300(4) Uani 1 1 d . . .
C19 C 0.27918(19) 0.70468(16) 0.34632(16) 0.0329(4) Uani 1 1 d . . .
H19 H 0.2101 0.6199 0.3079 0.039 Uiso 1 1 calc R . .
C20 C 0.3820(2) 0.71917(19) 0.46593(18) 0.0424(5) Uani 1 1 d . . .
H20A H 0.4298 0.6720 0.4575 0.064 Uiso 1 1 calc R . .
H20B H 0.3332 0.6927 0.5113 0.064 Uiso 1 1 calc R . .
H20C H 0.4492 0.8022 0.5058 0.064 Uiso 1 1 calc R . .
C21 C 0.3560(3) 0.7383(2) 0.2729(2) 0.0518(6) Uani 1 1 d . . .
H21A H 0.4033 0.6898 0.2688 0.078 Uiso 1 1 calc R . .
H21B H 0.4235 0.8215 0.3087 0.078 Uiso 1 1 calc R . .
H21C H 0.2899 0.7251 0.1945 0.078 Uiso 1 1 calc R . .
C22 C -0.1566(2) 0.74542(17) 0.2979(2) 0.0438(5) Uani 1 1 d . . .
H22 H -0.1893 0.6612 0.2942 0.053 Uiso 1 1 calc R . .
C23 C -0.2334(3) 0.7474(4) 0.1784(3) 0.0991(14) Uani 1 1 d . . .
H23A H -0.3320 0.7138 0.1568 0.149 Uiso 1 1 calc R . .
H23B H -0.2180 0.7009 0.1225 0.149 Uiso 1 1 calc R . .
H23C H -0.2001 0.8288 0.1784 0.149 Uiso 1 1 calc R . .
C24 C -0.1931(3) 0.8056(2) 0.3818(2) 0.0546(6) Uani 1 1 d . . .
H24A H -0.2931 0.7684 0.3531 0.082 Uiso 1 1 calc R . .
H24B H -0.1601 0.8890 0.3888 0.082 Uiso 1 1 calc R . .
H24C H -0.1496 0.7984 0.4579 0.082 Uiso 1 1 calc R . .
C25 C -0.37197(17) 0.28275(15) 0.24156(14) 0.0266(3) Uani 1 1 d . . .
C26 C -0.38330(17) 0.17007(15) 0.23937(15) 0.0286(4) Uani 1 1 d . . .
C27 C -0.5024(2) 0.08680(17) 0.23601(18) 0.0385(4) Uani 1 1 d . . .
H27 H -0.5118 0.0102 0.2340 0.046 Uiso 1 1 calc R . .
C28 C -0.6063(2) 0.11402(19) 0.23556(19) 0.0439(5) Uani 1 1 d . . .
H28 H -0.6880 0.0555 0.2304 0.053 Uiso 1 1 calc R . .
C29 C -0.5918(2) 0.22635(19) 0.24256(18) 0.0402(5) Uani 1 1 d . . .
H29 H -0.6629 0.2449 0.2444 0.048 Uiso 1 1 calc R . .
C30 C -0.47472(18) 0.31290(16) 0.24692(15) 0.0309(4) Uani 1 1 d . . .
C31 C -0.27114(18) 0.13588(15) 0.23993(15) 0.0300(4) Uani 1 1 d . . .
H31 H -0.1971 0.2036 0.2371 0.036 Uiso 1 1 calc R . .
C32 C -0.2088(2) 0.11059(19) 0.35110(19) 0.0420(5) Uani 1 1 d . . .
H32A H -0.1367 0.0888 0.3507 0.063 Uiso 1 1 calc R . .
H32B H -0.2806 0.0457 0.3562 0.063 Uiso 1 1 calc R . .
H32C H -0.1690 0.1810 0.4180 0.063 Uiso 1 1 calc R . .
C33 C -0.3233(2) 0.02742(19) 0.1367(2) 0.0479(5) Uani 1 1 d . . .
H33A H -0.2471 0.0095 0.1415 0.072 Uiso 1 1 calc R . .
H33B H -0.3605 0.0434 0.0643 0.072 Uiso 1 1 calc R . .
H33C H -0.3958 -0.0399 0.1384 0.072 Uiso 1 1 calc R . .
C34 C -0.4623(2) 0.43556(17) 0.25414(17) 0.0355(4) Uani 1 1 d . . .
H34 H -0.3624 0.4907 0.2866 0.043 Uiso 1 1 calc R . .
C35 C -0.5348(3) 0.4431(3) 0.1348(2) 0.0667(8) Uani 1 1 d . . .
H35A H -0.5240 0.5233 0.1428 0.100 Uiso 1 1 calc R . .
H35B H -0.6328 0.3879 0.0993 0.100 Uiso 1 1 calc R . .
H35C H -0.4942 0.4230 0.0856 0.100 Uiso 1 1 calc R . .
C36 C -0.5157(2) 0.4785(2) 0.3347(2) 0.0489(5) Uani 1 1 d . . .
H36A H -0.5053 0.5576 0.3361 0.073 Uiso 1 1 calc R . .
H36B H -0.4630 0.4806 0.4131 0.073 Uiso 1 1 calc R . .
H36C H -0.6131 0.4247 0.3065 0.073 Uiso 1 1 calc R . .
H3 H 0.001(2) 0.3463(9) 0.454(2) 0.057(7) Uiso 1 1 d D . .
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'
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
N2 Mg1 N1 92.65(6) . . ?
N2 Mg1 N3 125.02(6) . 2_566 ?
N1 Mg1 N3 115.75(6) . 2_566 ?
N2 Mg1 N3 114.66(6) . . ?
N1 Mg1 N3 122.65(6) . . ?
N3 Mg1 N3 89.27(6) 2_566 . ?
C8 N1 C13 115.06(13) . . ?
C8 N1 Mg1 120.21(11) . . ?
C13 N1 Mg1 124.53(10) . . ?
C10 N2 C25 115.29(13) . . ?
C10 N2 Mg1 120.28(11) . . ?
C25 N2 Mg1 124.33(10) . . ?
C1 N3 Mg1 128.98(12) . 2_566 ?
C1 N3 Mg1 125.04(12) . . ?
Mg1 N3 Mg1 90.73(6) 2_566 . ?
N3 C1 C2 114.60(16) . . ?
C3 C2 C7 118.68(19) . . ?
C3 C2 C1 121.79(18) . . ?
C7 C2 C1 119.50(18) . . ?
C2 C3 C4 121.0(2) . . ?
C5 C4 C3 120.0(2) . . ?
C4 C5 C6 119.2(2) . . ?
C5 C6 C7 120.6(2) . . ?
C2 C7 C6 120.5(2) . . ?
N1 C8 C9 124.87(15) . . ?
N1 C8 C11 120.77(15) . . ?
C9 C8 C11 114.36(15) . . ?
C8 C9 C10 130.23(16) . . ?
N2 C10 C9 125.27(15) . . ?
N2 C10 C12 120.62(15) . . ?
C9 C10 C12 114.11(15) . . ?
C14 C13 C18 120.44(15) . . ?
C14 C13 N1 121.79(15) . . ?
C18 C13 N1 117.73(15) . . ?
C15 C14 C13 118.56(17) . . ?
C15 C14 C19 118.67(16) . . ?
C13 C14 C19 122.76(15) . . ?
C16 C15 C14 121.39(18) . . ?
C15 C16 C17 119.91(17) . . ?
C16 C17 C18 121.12(18) . . ?
C17 C18 C13 118.58(17) . . ?
C17 C18 C22 119.59(16) . . ?
C13 C18 C22 121.79(15) . . ?
C14 C19 C20 110.47(16) . . ?
C14 C19 C21 112.46(16) . . ?
C20 C19 C21 108.91(17) . . ?
C23 C22 C24 109.4(2) . . ?
C23 C22 C18 111.2(2) . . ?
C24 C22 C18 113.24(18) . . ?
C26 C25 C30 120.66(16) . . ?
C26 C25 N2 120.77(15) . . ?
C30 C25 N2 118.51(15) . . ?
C27 C26 C25 118.48(17) . . ?
C27 C26 C31 119.15(16) . . ?
C25 C26 C31 122.36(15) . . ?
C28 C27 C26 121.09(19) . . ?
C27 C28 C29 120.00(18) . . ?
C28 C29 C30 121.18(19) . . ?
C29 C30 C25 118.44(17) . . ?
C29 C30 C34 119.81(17) . . ?
C25 C30 C34 121.73(16) . . ?
C26 C31 C32 110.10(16) . . ?
C26 C31 C33 113.01(15) . . ?
C32 C31 C33 108.37(17) . . ?
C30 C34 C35 111.79(18) . . ?
C30 C34 C36 112.93(17) . . ?
C35 C34 C36 109.60(18) . . ?
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
Mg1 N2 2.0918(14) . ?
Mg1 N1 2.1071(14) . ?
Mg1 N3 2.1216(16) 2_566 ?
Mg1 N3 2.1251(16) . ?
N1 C8 1.335(2) . ?
N1 C13 1.443(2) . ?
N2 C10 1.328(2) . ?
N2 C25 1.447(2) . ?
N3 C1 1.458(3) . ?
N3 Mg1 2.1216(16) 2_566 ?
C1 C2 1.526(3) . ?
C2 C3 1.377(3) . ?
C2 C7 1.386(3) . ?
C3 C4 1.394(3) . ?
C4 C5 1.380(3) . ?
C5 C6 1.381(3) . ?
C6 C7 1.388(3) . ?
C8 C9 1.398(2) . ?
C8 C11 1.517(2) . ?
C9 C10 1.405(2) . ?
C10 C12 1.521(2) . ?
C13 C14 1.405(2) . ?
C13 C18 1.410(2) . ?
C14 C15 1.398(2) . ?
C14 C19 1.520(3) . ?
C15 C16 1.376(3) . ?
C16 C17 1.378(3) . ?
C17 C18 1.400(2) . ?
C18 C22 1.516(3) . ?
C19 C20 1.526(3) . ?
C19 C21 1.543(3) . ?
C22 C23 1.509(4) . ?
C22 C24 1.514(3) . ?
C25 C26 1.407(2) . ?
C25 C30 1.407(3) . ?
C26 C27 1.398(2) . ?
C26 C31 1.522(3) . ?
C27 C28 1.377(3) . ?
C28 C29 1.381(3) . ?
C29 C30 1.394(3) . ?
C30 C34 1.521(3) . ?
C31 C32 1.523(3) . ?
C31 C33 1.534(3) . ?
C34 C35 1.526(3) . ?
C34 C36 1.528(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168336753
