#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/21/4302125.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_4302125
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            'C35.5 H53 Mg N3'
_chemical_formula_weight         546.12
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 114.064(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.1971(3)
_cell_length_b                   21.1259(4)
_cell_length_c                   17.7461(3)
_cell_measurement_reflns_used    45040
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     6571.5(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0859
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72227
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         7534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0740
_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)+(0.1105P)²+14.2044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1984
_refine_ls_wR_factor_ref         0.2312
_reflns_number_gt                5075
_reflns_number_total             7534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900091x_si_001_2.cif
_cod_data_source_block           k08msh25
_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.

'_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_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C35.50 H53 Mg N3'
_cod_database_code               4302125
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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_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 0.92489(4) 0.23574(4) 0.25818(5) 0.0215(2) Uani 1 1 d . . .
N1 N 0.85010(12) 0.16294(10) 0.26023(13) 0.0237(4) Uani 1 1 d . . .
N2 N 0.85404(12) 0.31102(10) 0.26473(13) 0.0246(5) Uani 1 1 d . . .
N3 N 0.96037(12) 0.23297(10) 0.15985(13) 0.0249(5) Uani 1 1 d . . .
C1 C 0.93282(18) 0.17376(17) 0.1146(2) 0.0521(9) Uani 1 1 d . . .
H1A H 0.9302 0.1401 0.1522 0.063 Uiso 1 1 calc R . .
H1B H 0.9674 0.1596 0.0890 0.063 Uiso 1 1 calc R . .
C2 C 0.93185(19) 0.27928(19) 0.0943(3) 0.0613(11) Uani 1 1 d . . .
H2A H 0.9631 0.2792 0.0616 0.074 Uiso 1 1 calc R . .
H2B H 0.9334 0.3222 0.1173 0.074 Uiso 1 1 calc R . .
C3 C 0.85005(19) 0.2602(2) 0.0407(2) 0.0600(11) Uani 1 1 d . . .
H3A H 0.8350 0.2739 -0.0172 0.072 Uiso 1 1 calc R . .
H3B H 0.8140 0.2784 0.0620 0.072 Uiso 1 1 calc R . .
C4 C 0.8529(2) 0.1880(2) 0.0478(2) 0.0609(11) Uani 1 1 d . . .
H4A H 0.8459 0.1682 -0.0053 0.073 Uiso 1 1 calc R . .
H4B H 0.8128 0.1721 0.0646 0.073 Uiso 1 1 calc R . .
C5 C 0.77978(14) 0.29850(12) 0.23236(16) 0.0267(5) Uani 1 1 d . . .
C6 C 0.74625(14) 0.23884(13) 0.20538(16) 0.0278(6) Uani 1 1 d . . .
H6 H 0.6943 0.2405 0.1675 0.033 Uiso 1 1 calc R . .
C7 C 0.77582(14) 0.17721(12) 0.22435(16) 0.0264(5) Uani 1 1 d . . .
C8 C 0.72072(16) 0.34951(14) 0.2242(2) 0.0400(7) Uani 1 1 d . . .
H8A H 0.7466 0.3901 0.2437 0.060 Uiso 1 1 calc R . .
H8B H 0.6927 0.3377 0.2575 0.060 Uiso 1 1 calc R . .
H8C H 0.6850 0.3534 0.1662 0.060 Uiso 1 1 calc R . .
C9 C 0.71557(16) 0.12592(14) 0.2021(2) 0.0375(7) Uani 1 1 d . . .
H9A H 0.7331 0.0921 0.2434 0.056 Uiso 1 1 calc R . .
H9B H 0.7066 0.1086 0.1477 0.056 Uiso 1 1 calc R . .
H9C H 0.6680 0.1439 0.2007 0.056 Uiso 1 1 calc R . .
C10 C 0.87711(14) 0.37478(12) 0.29554(17) 0.0274(5) Uani 1 1 d . . .
C11 C 0.90383(15) 0.38658(13) 0.38101(17) 0.0315(6) Uani 1 1 d . . .
C12 C 0.92321(17) 0.44831(14) 0.4098(2) 0.0388(7) Uani 1 1 d . . .
H12 H 0.9410 0.4565 0.4673 0.047 Uiso 1 1 calc R . .
C13 C 0.91706(17) 0.49783(14) 0.3567(2) 0.0418(7) Uani 1 1 d . . .
H13 H 0.9300 0.5396 0.3774 0.050 Uiso 1 1 calc R . .
C14 C 0.89189(16) 0.48612(14) 0.2732(2) 0.0387(7) Uani 1 1 d . . .
H14 H 0.8880 0.5203 0.2368 0.046 Uiso 1 1 calc R . .
C15 C 0.87195(15) 0.42498(13) 0.24084(18) 0.0316(6) Uani 1 1 d . . .
C16 C 0.84302(18) 0.41775(16) 0.1480(2) 0.0430(7) Uani 1 1 d . . .
H16 H 0.8334 0.3718 0.1340 0.052 Uiso 1 1 calc R . .
C17 C 0.9017(2) 0.44158(17) 0.1165(2) 0.0516(9) Uani 1 1 d . . .
H17A H 0.8815 0.4361 0.0565 0.077 Uiso 1 1 calc R . .
H17B H 0.9491 0.4173 0.1427 0.077 Uiso 1 1 calc R . .
H17C H 0.9121 0.4865 0.1302 0.077 Uiso 1 1 calc R . .
C18 C 0.7677(2) 0.4544(3) 0.1021(3) 0.0741(13) Uani 1 1 d . . .
H18A H 0.7507 0.4485 0.0425 0.111 Uiso 1 1 calc R . .
H18B H 0.7761 0.4995 0.1154 0.111 Uiso 1 1 calc R . .
H18C H 0.7285 0.4383 0.1193 0.111 Uiso 1 1 calc R . .
C19 C 0.90717(17) 0.33503(15) 0.44210(18) 0.0364(7) Uani 1 1 d . . .
H19 H 0.9158 0.2938 0.4196 0.044 Uiso 1 1 calc R . .
C20 C 0.8314(2) 0.33034(19) 0.4511(2) 0.0565(9) Uani 1 1 d . . .
H20A H 0.8347 0.2967 0.4904 0.085 Uiso 1 1 calc R . .
H20B H 0.7903 0.3206 0.3974 0.085 Uiso 1 1 calc R . .
H20C H 0.8206 0.3707 0.4714 0.085 Uiso 1 1 calc R . .
C21 C 0.9728(2) 0.34470(17) 0.52691(19) 0.0484(8) Uani 1 1 d . . .
H21A H 0.9727 0.3103 0.5639 0.073 Uiso 1 1 calc R . .
H21B H 0.9663 0.3853 0.5500 0.073 Uiso 1 1 calc R . .
H21C H 1.0214 0.3448 0.5211 0.073 Uiso 1 1 calc R . .
C22 C 0.87078(14) 0.10145(12) 0.29932(16) 0.0248(5) Uani 1 1 d . . .
C23 C 0.89001(15) 0.09885(13) 0.38516(16) 0.0291(6) Uani 1 1 d . . .
C24 C 0.91346(17) 0.04111(14) 0.42661(18) 0.0361(6) Uani 1 1 d . . .
H24 H 0.9270 0.0394 0.4844 0.043 Uiso 1 1 calc R . .
C25 C 0.91727(17) -0.01319(14) 0.38553(19) 0.0370(7) Uani 1 1 d . . .
H25 H 0.9347 -0.0517 0.4149 0.044 Uiso 1 1 calc R . .
C26 C 0.89565(15) -0.01115(13) 0.30153(18) 0.0320(6) Uani 1 1 d . . .
H26 H 0.8969 -0.0490 0.2732 0.038 Uiso 1 1 calc R . .
C27 C 0.87187(14) 0.04519(12) 0.25654(16) 0.0276(6) Uani 1 1 d . . .
C28 C 0.87883(18) 0.15549(14) 0.43196(18) 0.0384(7) Uani 1 1 d . . .
H28 H 0.8822 0.1945 0.4017 0.046 Uiso 1 1 calc R . .
C29 C 0.7991(2) 0.1535(2) 0.4313(3) 0.0618(10) Uani 1 1 d . . .
H29A H 0.7922 0.1901 0.4615 0.093 Uiso 1 1 calc R . .
H29B H 0.7931 0.1144 0.4579 0.093 Uiso 1 1 calc R . .
H29C H 0.7608 0.1546 0.3742 0.093 Uiso 1 1 calc R . .
C30 C 0.9394(2) 0.16068(18) 0.5202(2) 0.0584(10) Uani 1 1 d . . .
H30A H 0.9291 0.1980 0.5468 0.088 Uiso 1 1 calc R . .
H30B H 0.9899 0.1648 0.5192 0.088 Uiso 1 1 calc R . .
H30C H 0.9381 0.1226 0.5511 0.088 Uiso 1 1 calc R . .
C31 C 0.84512(16) 0.04033(13) 0.16354(17) 0.0323(6) Uani 1 1 d . . .
H31 H 0.8274 0.0831 0.1389 0.039 Uiso 1 1 calc R . .
C32 C 0.9089(2) 0.01826(16) 0.1387(2) 0.0461(8) Uani 1 1 d . . .
H32A H 0.8893 0.0160 0.0784 0.069 Uiso 1 1 calc R . .
H32B H 0.9267 -0.0237 0.1623 0.069 Uiso 1 1 calc R . .
H32C H 0.9513 0.0484 0.1595 0.069 Uiso 1 1 calc R . .
C33 C 0.77773(19) -0.00660(15) 0.1268(2) 0.0434(7) Uani 1 1 d . . .
H33A H 0.7613 -0.0089 0.0668 0.065 Uiso 1 1 calc R . .
H33B H 0.7352 0.0080 0.1393 0.065 Uiso 1 1 calc R . .
H33C H 0.7940 -0.0486 0.1509 0.065 Uiso 1 1 calc R . .
C34 C 0.5000 0.1323(3) 0.2500 0.0605(14) Uani 1 2 d S . .
H34 H 0.5000 0.0873 0.2500 0.073 Uiso 1 2 calc SR . .
C35 C 0.4332(2) 0.1639(2) 0.2127(3) 0.0190(9) Uani 0.50 1 d P . .
H35 H 0.3868 0.1412 0.1867 0.023 Uiso 1 1 calc R . .
C36 C 0.4326(3) 0.2286(2) 0.2125(3) 0.0212(10) Uani 0.50 1 d P . .
H36 H 0.3857 0.2507 0.1866 0.025 Uiso 1 1 calc R . .
C37 C 0.5000 0.2619(3) 0.2500 0.088(3) Uani 1 2 d S . .
C38 C 0.5000 0.3333(3) 0.2500 0.113(3) Uani 1 2 d S . .
H38A H 0.5524 0.3488 0.2791 0.170 Uiso 0.50 1 calc PR . .
H38B H 0.4685 0.3488 0.2779 0.170 Uiso 0.50 1 calc PR . .
H38C H 0.4791 0.3488 0.1930 0.170 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'
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
N3 Mg1 N1 119.90(9) 2_755 . ?
N3 Mg1 N3 88.33(9) 2_755 . ?
N1 Mg1 N3 116.30(9) . . ?
N3 Mg1 N2 119.97(9) 2_755 . ?
N1 Mg1 N2 95.12(8) . . ?
N3 Mg1 N2 119.58(9) . . ?
N3 Mg1 Mg1 44.60(6) 2_755 2_755 ?
N1 Mg1 Mg1 133.22(6) . 2_755 ?
N3 Mg1 Mg1 43.82(6) . 2_755 ?
N2 Mg1 Mg1 131.58(6) . 2_755 ?
C7 N1 C22 117.4(2) . . ?
C7 N1 Mg1 115.30(17) . . ?
C22 N1 Mg1 127.21(15) . . ?
C5 N2 C10 117.1(2) . . ?
C5 N2 Mg1 115.15(17) . . ?
C10 N2 Mg1 127.61(16) . . ?
C2 N3 C1 101.7(3) . . ?
C2 N3 Mg1 119.17(18) . 2_755 ?
C1 N3 Mg1 116.66(18) . 2_755 ?
C2 N3 Mg1 120.1(2) . . ?
C1 N3 Mg1 108.1(2) . . ?
Mg1 N3 Mg1 91.58(9) 2_755 . ?
N3 C1 C4 106.2(3) . . ?
N3 C2 C3 106.2(3) . . ?
C2 C3 C4 102.7(3) . . ?
C3 C4 C1 104.4(3) . . ?
N2 C5 C6 125.9(2) . . ?
N2 C5 C8 121.6(2) . . ?
C6 C5 C8 112.4(2) . . ?
C7 C6 C5 131.6(2) . . ?
N1 C7 C6 124.8(2) . . ?
N1 C7 C9 121.0(2) . . ?
C6 C7 C9 114.2(2) . . ?
C11 C10 C15 119.9(2) . . ?
C11 C10 N2 119.3(2) . . ?
C15 C10 N2 120.8(2) . . ?
C12 C11 C10 119.0(3) . . ?
C12 C11 C19 118.8(3) . . ?
C10 C11 C19 122.1(2) . . ?
C13 C12 C11 121.5(3) . . ?
C14 C13 C12 119.5(3) . . ?
C13 C14 C15 121.5(3) . . ?
C14 C15 C10 118.6(3) . . ?
C14 C15 C16 117.1(3) . . ?
C10 C15 C16 124.2(3) . . ?
C15 C16 C17 111.4(3) . . ?
C15 C16 C18 111.8(3) . . ?
C17 C16 C18 108.2(3) . . ?
C11 C19 C20 110.8(3) . . ?
C11 C19 C21 112.6(3) . . ?
C20 C19 C21 110.0(3) . . ?
C23 C22 C27 119.4(2) . . ?
C23 C22 N1 116.8(2) . . ?
C27 C22 N1 123.8(2) . . ?
C24 C23 C22 119.1(2) . . ?
C24 C23 C28 119.0(2) . . ?
C22 C23 C28 121.6(2) . . ?
C25 C24 C23 121.5(3) . . ?
C26 C25 C24 119.3(3) . . ?
C25 C26 C27 121.9(3) . . ?
C26 C27 C22 118.7(2) . . ?
C26 C27 C31 116.7(2) . . ?
C22 C27 C31 124.6(2) . . ?
C23 C28 C29 109.8(3) . . ?
C23 C28 C30 113.5(3) . . ?
C29 C28 C30 110.6(3) . . ?
C27 C31 C32 112.1(2) . . ?
C27 C31 C33 110.8(2) . . ?
C32 C31 C33 108.2(2) . . ?
C35 C34 C35 120.8(6) 2_655 . ?
C34 C35 C36 120.0(5) . . ?
C35 C36 C37 120.2(5) . . ?
C36 C37 C36 118.8(6) . 2_655 ?
C36 C37 C38 120.6(3) . . ?
C36 C37 C38 120.6(3) 2_655 . ?
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 N3 2.088(2) 2_755 ?
Mg1 N1 2.114(2) . ?
Mg1 N3 2.117(2) . ?
Mg1 N2 2.126(2) . ?
Mg1 Mg1 3.0140(16) 2_755 ?
N1 C7 1.338(3) . ?
N1 C22 1.450(3) . ?
N2 C5 1.328(3) . ?
N2 C10 1.453(3) . ?
N3 C2 1.446(4) . ?
N3 C1 1.464(4) . ?
N3 Mg1 2.088(2) 2_755 ?
C1 C4 1.538(5) . ?
C2 C3 1.521(5) . ?
C3 C4 1.531(6) . ?
C5 C6 1.407(4) . ?
C5 C8 1.528(4) . ?
C6 C7 1.405(4) . ?
C7 C9 1.515(4) . ?
C10 C11 1.411(4) . ?
C10 C15 1.413(4) . ?
C11 C12 1.395(4) . ?
C11 C19 1.519(4) . ?
C12 C13 1.381(5) . ?
C13 C14 1.381(5) . ?
C14 C15 1.402(4) . ?
C15 C16 1.516(4) . ?
C16 C17 1.532(4) . ?
C16 C18 1.547(5) . ?
C19 C20 1.531(4) . ?
C19 C21 1.532(4) . ?
C22 C23 1.415(4) . ?
C22 C27 1.415(4) . ?
C23 C24 1.401(4) . ?
C23 C28 1.521(4) . ?
C24 C25 1.377(4) . ?
C25 C26 1.375(4) . ?
C26 C27 1.402(4) . ?
C27 C31 1.519(4) . ?
C28 C29 1.526(5) . ?
C28 C30 1.527(5) . ?
C31 C32 1.533(4) . ?
C31 C33 1.547(4) . ?
C34 C35 1.356(5) 2_655 ?
C34 C35 1.356(5) . ?
C35 C36 1.365(7) . ?
C36 C37 1.382(6) . ?
C37 C36 1.382(6) 2_655 ?
C37 C38 1.510(9) . ?
