#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/27/4322707.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_4322707
loop_
_publ_author_name
'Jennifer L. Sebestl'
'T. Timothy Nadasdi'
'Mary Jane Heeg'
'Charles H. Winter'
_publ_section_title
;
 Monomeric Three- and Four-Coordinate Magnesium Amides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1289
_journal_page_last               1294
_journal_paper_doi               10.1021/ic970905m
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C24 H50 Mg N4 Si4'
_chemical_formula_weight         531.35
_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   observed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                99.3180(10)
_cell_angle_beta                 98.4180(10)
_cell_angle_gamma                111.5320(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4914(6)
_cell_length_b                   11.8504(6)
_cell_length_c                   15.4546(9)
_cell_measurement_reflns_used    4981
_cell_measurement_temperature    295(2)
_cell_volume                     1718.85(17)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'SMART 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  0.022
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16479
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.37
_diffrn_standards_interval_time  21600
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_description       'cut fragment'
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0000(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.905
_refine_ls_goodness_of_fit_obs   0.988
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         6740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_restrained_S_obs      0.988
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_obs          0.0446
_refine_ls_shift/esd_max         -0.489
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0870P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1332
_refine_ls_wR_factor_obs         0.1157
_reflns_number_observed          4690
_reflns_number_total             6742
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970905m_2.cif
_cod_data_source_block           mgin(3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+0.0000P] 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^)+(0.0870P)^2^+0.0000P] 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        1718.8(2)
_cod_database_code               4322707
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mg1 Mg 0.23040(7) 0.22877(6) 0.76147(4) 0.0425(2) Uani 1 d . .
Si1 Si 0.20029(7) 0.38303(6) 0.61669(4) 0.0563(2) Uani 1 d . .
Si2 Si 0.48546(6) 0.47421(6) 0.73308(4) 0.0536(2) Uani 1 d . .
Si3 Si 0.02783(6) 0.29830(6) 0.87050(4) 0.0523(2) Uani 1 d . .
Si4 Si -0.08305(7) 0.03208(6) 0.77203(4) 0.0564(2) Uani 1 d . .
N1 N 0.3127(2) 0.37299(14) 0.70337(11) 0.0456(4) Uani 1 d . .
N2 N 0.0449(2) 0.1801(2) 0.80082(11) 0.0459(4) Uani 1 d . .
C1 C 0.0357(3) 0.2371(3) 0.5778(2) 0.0784(8) Uani 1 d . .
C2 C 0.2726(5) 0.4019(4) 0.5129(2) 0.0902(10) Uani 1 d . .
C3 C 0.1412(5) 0.5137(4) 0.6467(3) 0.0933(11) Uani 1 d . .
C4 C 0.5604(4) 0.5179(4) 0.8574(2) 0.0836(9) Uani 1 d . .
C5 C 0.5976(4) 0.4085(4) 0.6771(3) 0.0799(8) Uani 1 d . .
C6 C 0.5229(4) 0.6300(3) 0.7048(3) 0.0869(9) Uani 1 d . .
C7 C 0.1966(3) 0.4404(3) 0.9062(2) 0.0707(7) Uani 1 d . .
C8 C -0.1079(4) 0.3505(4) 0.8188(3) 0.0833(9) Uani 1 d . .
C9 C -0.0170(4) 0.2615(4) 0.9786(2) 0.0753(8) Uani 1 d . .
C10 C -0.0941(4) -0.0589(3) 0.6586(2) 0.0803(9) Uani 1 d . .
C11 C -0.2678(3) 0.0227(4) 0.7663(3) 0.0976(11) Uani 1 d . .
C12 C -0.0577(5) -0.0648(3) 0.8527(3) 0.0918(10) Uani 1 d . .
N3 N 0.2678(2) 0.0793(2) 0.67838(11) 0.0520(4) Uani 1 d . .
C13 C 0.2995(3) 0.0876(2) 0.5988(2) 0.0548(5) Uani 1 d . .
C14 C 0.3245(3) -0.0028(2) 0.5460(2) 0.0637(6) Uani 1 d . .
C15 C 0.3201(3) -0.1082(2) 0.5737(2) 0.0620(6) Uani 1 d . .
C16 C 0.2884(3) -0.1166(3) 0.6557(2) 0.0738(7) Uani 1 d . .
C17 C 0.2624(3) -0.0238(2) 0.7048(2) 0.0687(7) Uani 1 d . .
C18 C 0.3456(6) -0.2103(4) 0.5168(4) 0.0978(11) Uani 1 d . .
N4 N 0.3650(2) 0.2083(2) 0.87672(11) 0.0501(4) Uani 1 d . .
C19 C 0.3172(3) 0.1819(2) 0.94964(14) 0.0529(5) Uani 1 d . .
C20 C 0.3957(3) 0.1668(2) 1.0226(2) 0.0614(6) Uani 1 d . .
C21 C 0.5320(3) 0.1794(2) 1.02400(15) 0.0588(6) Uani 1 d . .
C22 C 0.5813(3) 0.2047(3) 0.9487(2) 0.0687(7) Uani 1 d . .
C23 C 0.4963(3) 0.2170(3) 0.8776(2) 0.0633(6) Uani 1 d . .
C24 C 0.6224(5) 0.1671(5) 1.1038(3) 0.0911(10) Uani 1 d . .
H1A H -0.0219(31) 0.2253(28) 0.6205(21) 0.088(10) Uiso 1 d . .
H1B H 0.0613(34) 0.1651(33) 0.5577(21) 0.107(11) Uiso 1 d . .
H1C H -0.0262(39) 0.2611(34) 0.5375(25) 0.122(12) Uiso 1 d . .
H2A H 0.1955(44) 0.3995(37) 0.4703(28) 0.135(14) Uiso 1 d . .
H2B H 0.3551(47) 0.4793(44) 0.5203(27) 0.142(15) Uiso 1 d . .
H2C H 0.3028(44) 0.3333(44) 0.4892(29) 0.145(16) Uiso 1 d . .
H3A H 0.2162(42) 0.5801(38) 0.6612(26) 0.118(15) Uiso 1 d . .
H3B H 0.0791(44) 0.5100(37) 0.6009(29) 0.130(15) Uiso 1 d . .
H3C H 0.0783(45) 0.5004(39) 0.6911(29) 0.147(16) Uiso 1 d . .
H4A H 0.5622(51) 0.4530(50) 0.8837(32) 0.171(21) Uiso 1 d . .
H4B H 0.6472(43) 0.5708(37) 0.8650(24) 0.114(12) Uiso 1 d . .
H4C H 0.5169(46) 0.5590(41) 0.8810(29) 0.136(17) Uiso 1 d . .
H5A H 0.5922(33) 0.3339(33) 0.6913(21) 0.097(11) Uiso 1 d . .
H5B H 0.5747(42) 0.3975(39) 0.6166(29) 0.139(16) Uiso 1 d . .
H5C H 0.6883(35) 0.4650(28) 0.6886(19) 0.083(9) Uiso 1 d . .
H6A H 0.6237(47) 0.6748(41) 0.7218(27) 0.145(15) Uiso 1 d . .
H6B H 0.4642(42) 0.6665(35) 0.7252(25) 0.121(14) Uiso 1 d . .
H6C H 0.4977(34) 0.6174(30) 0.6402(24) 0.097(11) Uiso 1 d . .
H7A H 0.1775(34) 0.4958(31) 0.9438(22) 0.104(10) Uiso 1 d . .
H7B H 0.2261(31) 0.4707(28) 0.8615(21) 0.085(10) Uiso 1 d . .
H7C H 0.2781(37) 0.4177(31) 0.9406(21) 0.109(11) Uiso 1 d . .
H8A H -0.0839(33) 0.3829(30) 0.7677(24) 0.100(11) Uiso 1 d . .
H8B H -0.1106(41) 0.4127(39) 0.8582(26) 0.129(15) Uiso 1 d . .
H8C H -0.2016(45) 0.2917(37) 0.8099(25) 0.127(14) Uiso 1 d . .
H9A H 0.0625(37) 0.2495(31) 1.0147(21) 0.108(11) Uiso 1 d . .
H9B H -0.0318(39) 0.3229(35) 1.0160(25) 0.126(13) Uiso 1 d . .
H9C H -0.0933(33) 0.1828(29) 0.9721(19) 0.086(10) Uiso 1 d . .
H10A H -0.1094(44) -0.0119(41) 0.6169(29) 0.148(16) Uiso 1 d . .
H10B H -0.0109(60) -0.0761(48) 0.6526(34) 0.183(22) Uiso 1 d . .
H10C H -0.1689(49) -0.1352(45) 0.6465(28) 0.154(16) Uiso 1 d . .
H11A H -0.2801(37) 0.0836(36) 0.7296(24) 0.118(13) Uiso 1 d . .
H11B H -0.2754(35) 0.0535(34) 0.8251(26) 0.108(13) Uiso 1 d . .
H11C H -0.3333(58) -0.0566(54) 0.7436(34) 0.185(20) Uiso 1 d . .
H12A H 0.0430(39) -0.0544(32) 0.8606(22) 0.104(11) Uiso 1 d . .
H12B H -0.1176(48) -0.1495(46) 0.8368(28) 0.155(16) Uiso 1 d . .
H12C H -0.0608(43) -0.0300(39) 0.9119(30) 0.138(15) Uiso 1 d . .
H13 H 0.3066(24) 0.1571(23) 0.5812(15) 0.057(6) Uiso 1 d . .
H14 H 0.3415(25) 0.0032(22) 0.4929(17) 0.062(7) Uiso 1 d . .
H16 H 0.2705(29) -0.1908(27) 0.6773(18) 0.081(8) Uiso 1 d . .
H17 H 0.2358(30) -0.0309(27) 0.7654(21) 0.095(9) Uiso 1 d . .
H18A H 0.3616(44) -0.1977(37) 0.4652(28) 0.126(16) Uiso 1 d . .
H18B H 0.2844(49) -0.2912(48) 0.5153(30) 0.156(18) Uiso 1 d . .
H18C H 0.4333(54) -0.2106(44) 0.5432(31) 0.166(20) Uiso 1 d . .
H19 H 0.2278(24) 0.1747(20) 0.9510(14) 0.053(6) Uiso 1 d . .
H20 H 0.3522(27) 0.1529(24) 1.0699(18) 0.074(8) Uiso 1 d . .
H22 H 0.6713(30) 0.2155(25) 0.9445(17) 0.081(8) Uiso 1 d . .
H23 H 0.5292(27) 0.2372(24) 0.8294(17) 0.072(8) Uiso 1 d . .
H24A H 0.6833(44) 0.1363(40) 1.0830(27) 0.138(16) Uiso 1 d . .
H24B H 0.6705(53) 0.2459(52) 1.1353(35) 0.175(22) Uiso 1 d . .
H24C H 0.5657(35) 0.1278(32) 1.1395(23) 0.096(12) Uiso 1 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'
Si Si 0.0817 0.0704 '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 Mg1 N2 125.52(8) . . ?
N1 Mg1 N3 101.73(7) . . ?
N2 Mg1 N3 117.24(7) . . ?
N1 Mg1 N4 119.00(8) . . ?
N2 Mg1 N4 100.62(7) . . ?
N3 Mg1 N4 86.80(7) . . ?
N1 Si1 C1 111.31(12) . . ?
N1 Si1 C2 113.9(2) . . ?
C1 Si1 C2 104.4(2) . . ?
N1 Si1 C3 113.5(2) . . ?
C1 Si1 C3 105.7(2) . . ?
C2 Si1 C3 107.4(2) . . ?
N1 Si2 C5 111.66(14) . . ?
N1 Si2 C4 113.24(14) . . ?
C5 Si2 C4 107.6(2) . . ?
N1 Si2 C6 115.09(14) . . ?
C5 Si2 C6 105.8(2) . . ?
C4 Si2 C6 102.8(2) . . ?
N2 Si3 C7 111.20(12) . . ?
N2 Si3 C9 113.97(13) . . ?
C7 Si3 C9 104.6(2) . . ?
N2 Si3 C8 114.20(15) . . ?
C7 Si3 C8 105.8(2) . . ?
C9 Si3 C8 106.3(2) . . ?
N2 Si4 C10 113.90(13) . . ?
N2 Si4 C12 112.73(14) . . ?
C10 Si4 C12 105.6(2) . . ?
N2 Si4 C11 114.9(2) . . ?
C10 Si4 C11 103.4(2) . . ?
C12 Si4 C11 105.3(2) . . ?
Si1 N1 Si2 120.72(10) . . ?
Si1 N1 Mg1 115.65(9) . . ?
Si2 N1 Mg1 123.52(9) . . ?
Si3 N2 Si4 121.33(10) . . ?
Si3 N2 Mg1 114.62(9) . . ?
Si4 N2 Mg1 123.99(9) . . ?
C13 N3 C17 115.7(2) . . ?
C13 N3 Mg1 121.67(14) . . ?
C17 N3 Mg1 122.6(2) . . ?
N3 C13 C14 123.2(2) . . ?
C13 C14 C15 121.0(2) . . ?
C16 C15 C14 116.0(2) . . ?
C16 C15 C18 121.6(3) . . ?
C14 C15 C18 122.3(3) . . ?
C15 C16 C17 120.3(2) . . ?
N3 C17 C16 123.8(3) . . ?
C19 N4 C23 115.6(2) . . ?
C19 N4 Mg1 121.13(15) . . ?
C23 N4 Mg1 123.2(2) . . ?
N4 C19 C20 123.5(2) . . ?
C19 C20 C21 120.5(2) . . ?
C22 C21 C20 116.4(2) . . ?
C22 C21 C24 121.7(3) . . ?
C20 C21 C24 121.9(3) . . ?
C23 C22 C21 120.0(2) . . ?
N4 C23 C22 123.9(2) . . ?
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 N1 2.028(2) . ?
Mg1 N2 2.032(2) . ?
Mg1 N3 2.205(2) . ?
Mg1 N4 2.209(2) . ?
Si1 N1 1.700(2) . ?
Si1 C1 1.871(3) . ?
Si1 C2 1.883(3) . ?
Si1 C3 1.885(4) . ?
Si2 N1 1.708(2) . ?
Si2 C5 1.869(3) . ?
Si2 C4 1.875(3) . ?
Si2 C6 1.880(3) . ?
Si3 N2 1.705(2) . ?
Si3 C7 1.871(3) . ?
Si3 C9 1.875(3) . ?
Si3 C8 1.877(3) . ?
Si4 N2 1.709(2) . ?
Si4 C10 1.867(3) . ?
Si4 C12 1.880(3) . ?
Si4 C11 1.888(4) . ?
N3 C13 1.330(3) . ?
N3 C17 1.334(3) . ?
C13 C14 1.367(3) . ?
C14 C15 1.372(4) . ?
C15 C16 1.365(4) . ?
C15 C18 1.508(4) . ?
C16 C17 1.368(3) . ?
N4 C19 1.336(3) . ?
N4 C23 1.341(3) . ?
C19 C20 1.372(3) . ?
C20 C21 1.379(3) . ?
C21 C22 1.373(4) . ?
C21 C24 1.502(4) . ?
C22 C23 1.373(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168337494
