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#$Date: 2025-08-18 17:20:24 +0300 (Mon, 18 Aug 2025) $
#$Revision: 301776 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/51/46/1514624.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_1514624
loop_
_publ_author_name
'Lalrempuia, Ralte'
'Stasch, Andreas'
'Jones, Cameron'
_publ_section_title
;
 The reductive disproportionation of CO2 using a magnesium(i) complex:
 analogies with low valent f-block chemistry
;
_journal_issue                   12
_journal_name_full               'Chemical Science'
_journal_page_first              4383
_journal_paper_doi               10.1039/c3sc52242c
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C73 H106 Mg2 N4 O4'
_chemical_formula_weight         1152.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.03(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.749(3)
_cell_length_b                   14.372(3)
_cell_length_c                   18.802(4)
_cell_measurement_temperature    123(2)
_cell_volume                     3431.8(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Apex'
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12479
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.244
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6667
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0786
_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)+(0.1144P)²+3.7969P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2112
_refine_ls_wR_factor_ref         0.2273
_reflns_number_gt                5153
_reflns_number_total             6667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52242c.txt
_cod_data_source_block           compound3S
_cod_original_cell_volume        3431.7(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1514624
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.11975(6) 0.93799(6) 0.02429(5) 0.0246(2) Uani 1 1 d . . .
O1 O -0.01889(15) 0.99019(15) 0.03844(10) 0.0354(5) Uani 1 1 d . . .
O2 O 0.21401(15) 1.04569(14) 0.06573(13) 0.0397(5) Uani 1 1 d . . .
N1 N 0.22273(18) 0.87134(18) -0.04061(12) 0.0332(6) Uani 1 1 d . . .
N2 N 0.15238(16) 0.83572(15) 0.10262(11) 0.0246(5) Uani 1 1 d . . .
C1 C 0.4035(3) 0.8132(3) -0.05252(19) 0.0563(11) Uani 1 1 d . . .
H1A H 0.3879 0.7590 -0.0833 0.084 Uiso 1 1 calc R . .
H1B H 0.4659 0.8003 -0.0198 0.084 Uiso 1 1 calc R . .
H1C H 0.4170 0.8674 -0.0820 0.084 Uiso 1 1 calc R . .
C2 C 0.3105(2) 0.8331(2) -0.00995(16) 0.0355(7) Uani 1 1 d . . .
C3 C 0.3242(2) 0.8075(2) 0.06221(15) 0.0318(6) Uani 1 1 d . . .
H3 H 0.3943 0.7922 0.0796 0.038 Uiso 1 1 calc R . .
C4 C 0.2491(2) 0.80118(19) 0.11255(14) 0.0273(6) Uani 1 1 d . . .
C5 C 0.2857(2) 0.7499(2) 0.18081(15) 0.0370(7) Uani 1 1 d . . .
H5A H 0.2891 0.7934 0.2211 0.056 Uiso 1 1 calc R . .
H5B H 0.3557 0.7234 0.1765 0.056 Uiso 1 1 calc R . .
H5C H 0.2360 0.6998 0.1889 0.056 Uiso 1 1 calc R . .
C6 C 0.2125(2) 0.8776(3) -0.11777(16) 0.0447(9) Uani 1 1 d . . .
C7 C 0.2504(2) 0.9555(3) -0.15156(19) 0.0587(12) Uani 1 1 d . . .
C8 C 0.2390(3) 0.9561(5) -0.2278(2) 0.0833(19) Uani 1 1 d . . .
H8 H 0.2650 1.0077 -0.2525 0.100 Uiso 1 1 calc R . .
C9 C 0.1914(4) 0.8838(5) -0.2664(2) 0.0791(15) Uani 1 1 d U . .
H9 H 0.1849 0.8855 -0.3171 0.095 Uiso 1 1 calc R . .
C10 C 0.1540(4) 0.8108(4) -0.2316(2) 0.0755(15) Uani 1 1 d . . .
H10 H 0.1213 0.7612 -0.2587 0.091 Uiso 1 1 calc R . .
C11 C 0.1616(3) 0.8053(3) -0.15719(17) 0.0548(10) Uani 1 1 d . . .
C12 C 0.3014(3) 1.0362(4) -0.1111(2) 0.0714(14) Uani 1 1 d . . .
H12 H 0.3099 1.0191 -0.0594 0.086 Uiso 1 1 calc R . .
C13 C 0.2326(3) 1.1227(4) -0.1190(3) 0.0775(14) Uani 1 1 d . . .
H13A H 0.2249 1.1419 -0.1692 0.116 Uiso 1 1 calc R . .
H13B H 0.2656 1.1730 -0.0898 0.116 Uiso 1 1 calc R . .
H13C H 0.1631 1.1088 -0.1031 0.116 Uiso 1 1 calc R . .
C14 C 0.4116(4) 1.0572(4) -0.1350(3) 0.0978(17) Uani 1 1 d U . .
H14A H 0.4537 1.0000 -0.1329 0.147 Uiso 1 1 calc R . .
H14B H 0.4465 1.1039 -0.1031 0.147 Uiso 1 1 calc R . .
H14C H 0.4047 1.0810 -0.1840 0.147 Uiso 1 1 calc R . .
C15 C 0.1168(4) 0.7221(3) -0.1212(2) 0.0712(13) Uani 1 1 d . . .
H15 H 0.1020 0.7421 -0.0721 0.085 Uiso 1 1 calc R . .
C16 C 0.1963(5) 0.6427(4) -0.1127(4) 0.111(2) Uani 1 1 d U . .
H16A H 0.2235 0.6297 -0.1589 0.167 Uiso 1 1 calc R . .
H16B H 0.1619 0.5869 -0.0959 0.167 Uiso 1 1 calc R . .
H16C H 0.2547 0.6604 -0.0780 0.167 Uiso 1 1 calc R . .
C17 C 0.0134(4) 0.6859(4) -0.1586(3) 0.0847(15) Uani 1 1 d . . .
H17A H -0.0368 0.7373 -0.1660 0.127 Uiso 1 1 calc R . .
H17B H -0.0160 0.6381 -0.1288 0.127 Uiso 1 1 calc R . .
H17C H 0.0266 0.6589 -0.2048 0.127 Uiso 1 1 calc R . .
C18 C 0.0798(2) 0.80993(19) 0.15380(14) 0.0279(6) Uani 1 1 d . . .
C19 C 0.0709(2) 0.8629(2) 0.21522(15) 0.0338(6) Uani 1 1 d . . .
C20 C -0.0003(3) 0.8324(3) 0.26342(17) 0.0484(9) Uani 1 1 d . . .
H20 H -0.0076 0.8677 0.3054 0.058 Uiso 1 1 calc R . .
C21 C -0.0591(3) 0.7538(3) 0.25163(19) 0.0522(9) Uani 1 1 d . . .
H21 H -0.1049 0.7337 0.2858 0.063 Uiso 1 1 calc R . .
C22 C -0.0516(3) 0.7040(3) 0.1901(2) 0.0486(9) Uani 1 1 d . . .
H22 H -0.0937 0.6499 0.1817 0.058 Uiso 1 1 calc R . .
C23 C 0.0163(2) 0.7307(2) 0.13944(18) 0.0390(7) Uani 1 1 d . . .
C24 C 0.1323(2) 0.9518(2) 0.22925(17) 0.0393(7) Uani 1 1 d . . .
H24 H 0.1802 0.9592 0.1903 0.047 Uiso 1 1 calc R . .
C25 C 0.0590(3) 1.0357(3) 0.2265(2) 0.0536(9) Uani 1 1 d . . .
H25A H 0.0137 1.0349 0.1816 0.080 Uiso 1 1 calc R . .
H25B H 0.1009 1.0929 0.2293 0.080 Uiso 1 1 calc R . .
H25C H 0.0153 1.0332 0.2668 0.080 Uiso 1 1 calc R . .
C26 C 0.2008(3) 0.9503(3) 0.3003(2) 0.0654(11) Uani 1 1 d . . .
H26A H 0.1561 0.9412 0.3395 0.098 Uiso 1 1 calc R . .
H26B H 0.2385 1.0095 0.3068 0.098 Uiso 1 1 calc R . .
H26C H 0.2517 0.8992 0.3000 0.098 Uiso 1 1 calc R . .
C27 C 0.0192(3) 0.6773(3) 0.0701(2) 0.0618(11) Uani 1 1 d . . .
H27 H 0.0437 0.7221 0.0343 0.074 Uiso 1 1 calc R . .
C28 C -0.0876(4) 0.6419(3) 0.0396(2) 0.0667(11) Uani 1 1 d . . .
H28A H -0.0824 0.6190 -0.0091 0.100 Uiso 1 1 calc R . .
H28B H -0.1390 0.6926 0.0386 0.100 Uiso 1 1 calc R . .
H28C H -0.1103 0.5911 0.0695 0.100 Uiso 1 1 calc R . .
C29 C 0.0964(4) 0.5992(4) 0.0750(4) 0.0987(18) Uani 1 1 d U . .
H29A H 0.1675 0.6239 0.0865 0.148 Uiso 1 1 calc R . .
H29B H 0.0933 0.5662 0.0293 0.148 Uiso 1 1 calc R . .
H29C H 0.0791 0.5560 0.1126 0.148 Uiso 1 1 calc R . .
C30 C 0.3214(2) 1.0457(2) 0.0986(2) 0.0454(8) Uani 1 1 d . . .
H30A H 0.3723 1.0461 0.0617 0.055 Uiso 1 1 calc R . .
H30B H 0.3347 0.9901 0.1291 0.055 Uiso 1 1 calc R . .
C31 C 0.3311(3) 1.1316(3) 0.1419(3) 0.0666(12) Uani 1 1 d . . .
H31A H 0.4048 1.1542 0.1471 0.080 Uiso 1 1 calc R . .
H31B H 0.3068 1.1214 0.1898 0.080 Uiso 1 1 calc R . .
C32 C 0.2599(4) 1.1994(3) 0.0987(3) 0.0707(12) Uani 1 1 d . . .
H32A H 0.2347 1.2491 0.1295 0.085 Uiso 1 1 calc R . .
H32B H 0.2968 1.2282 0.0601 0.085 Uiso 1 1 calc R . .
C33 C 0.1702(3) 1.1392(2) 0.0687(2) 0.0488(9) Uani 1 1 d . . .
H33A H 0.1116 1.1407 0.0999 0.059 Uiso 1 1 calc R . .
H33B H 0.1437 1.1606 0.0204 0.059 Uiso 1 1 calc R . .
C34 C -0.0762(7) 1.0194(7) 0.4970(6) 0.096(3) Uiso 0.50 1 d PD A -1
C35 C 0.0036(9) 1.0728(10) 0.4665(10) 0.146(6) Uiso 0.50 1 d PD A -1
H35 H -0.0123 1.1301 0.4427 0.175 Uiso 0.50 1 calc PR A -1
C36 C 0.1066(9) 1.0367(10) 0.4734(9) 0.143(6) Uiso 0.50 1 d PD A -1
H36 H 0.1608 1.0712 0.4539 0.171 Uiso 0.50 1 calc PR A -1
C37 C 0.1332(7) 0.9517(9) 0.5080(8) 0.107(4) Uiso 0.50 1 d PD A -1
H37 H 0.2032 0.9284 0.5100 0.128 Uiso 0.50 1 calc PR A -1
C38 C 0.0528(7) 0.9010(8) 0.5401(7) 0.105(4) Uiso 0.50 1 d PD A -1
H38 H 0.0682 0.8446 0.5651 0.126 Uiso 0.50 1 calc PR A -1
C39 C -0.0539(6) 0.9392(5) 0.5329(4) 0.0527(17) Uiso 0.50 1 d PD A -1
H39 H -0.1086 0.9072 0.5539 0.063 Uiso 0.50 1 calc PR A -1
C40 C -0.1844(10) 1.0609(18) 0.4873(19) 0.285(17) Uiso 0.50 1 d PD A -1
H40A H -0.2140 1.0513 0.4380 0.427 Uiso 0.50 1 calc PR A -1
H40B H -0.1804 1.1277 0.4976 0.427 Uiso 0.50 1 calc PR A -1
H40C H -0.2296 1.0307 0.5201 0.427 Uiso 0.50 1 calc PR A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 '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
O1 Mg1 O1 47.81(10) . 3_575
O1 Mg1 O2 99.41(10) . .
O1 Mg1 O2 99.28(10) 3_575 .
O1 Mg1 N2 107.38(9) . .
O1 Mg1 N2 150.57(9) 3_575 .
O2 Mg1 N2 100.78(9) . .
O1 Mg1 N1 150.54(10) . .
O1 Mg1 N1 107.52(9) 3_575 .
O2 Mg1 N1 100.83(10) . .
N2 Mg1 N1 89.59(9) . .
O1 O1 Mg1 66.13(13) 3_575 .
O1 O1 Mg1 66.07(13) 3_575 3_575
Mg1 O1 Mg1 132.19(10) . 3_575
C30 O2 C33 109.5(2) . .
C30 O2 Mg1 130.93(19) . .
C33 O2 Mg1 119.46(18) . .
C2 N1 C6 117.2(2) . .
C2 N1 Mg1 118.76(19) . .
C6 N1 Mg1 123.23(18) . .
C4 N2 C18 116.9(2) . .
C4 N2 Mg1 119.05(18) . .
C18 N2 Mg1 123.37(16) . .
N1 C2 C3 123.8(2) . .
N1 C2 C1 121.1(3) . .
C3 C2 C1 115.1(3) . .
C2 C3 C4 129.3(2) . .
N2 C4 C3 124.1(2) . .
N2 C4 C5 120.9(2) . .
C3 C4 C5 115.0(2) . .
C7 C6 C11 121.1(3) . .
C7 C6 N1 120.2(4) . .
C11 C6 N1 118.7(3) . .
C6 C7 C8 117.0(5) . .
C6 C7 C12 122.7(3) . .
C8 C7 C12 120.3(4) . .
C9 C8 C7 121.7(5) . .
C10 C9 C8 119.4(4) . .
C9 C10 C11 122.3(5) . .
C10 C11 C6 118.4(4) . .
C10 C11 C15 119.9(4) . .
C6 C11 C15 121.7(3) . .
C7 C12 C13 111.2(3) . .
C7 C12 C14 111.7(5) . .
C13 C12 C14 110.1(4) . .
C11 C15 C16 111.4(5) . .
C11 C15 C17 114.1(4) . .
C16 C15 C17 109.3(4) . .
C19 C18 C23 120.8(3) . .
C19 C18 N2 121.0(2) . .
C23 C18 N2 118.1(2) . .
C18 C19 C20 117.8(3) . .
C18 C19 C24 121.9(3) . .
C20 C19 C24 120.3(3) . .
C21 C20 C19 122.0(3) . .
C20 C21 C22 119.5(3) . .
C21 C22 C23 121.7(3) . .
C22 C23 C18 118.1(3) . .
C22 C23 C27 120.7(3) . .
C18 C23 C27 121.1(3) . .
C19 C24 C25 110.9(3) . .
C19 C24 C26 112.9(3) . .
C25 C24 C26 110.0(3) . .
C29 C27 C23 113.1(4) . .
C29 C27 C28 109.7(3) . .
C23 C27 C28 113.9(3) . .
O2 C30 C31 105.3(3) . .
C30 C31 C32 103.0(3) . .
C33 C32 C31 103.4(3) . .
O2 C33 C32 105.3(3) . .
C39 C34 C35 122.0(6) . .
C39 C34 C40 123.3(8) . .
C35 C34 C40 114.6(8) . .
C36 C35 C34 117.0(7) . .
C35 C36 C37 123.2(7) . .
C36 C37 C38 118.8(7) . .
C37 C38 C39 117.7(6) . .
C34 C39 C38 121.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 O1 1.960(2) .
Mg1 O1 1.961(2) 3_575
Mg1 O2 2.069(2) .
Mg1 N2 2.096(2) .
Mg1 N1 2.100(3) .
O1 O1 1.588(4) 3_575
O1 Mg1 1.961(2) 3_575
O2 C30 1.452(3) .
O2 C33 1.458(4) .
N1 C2 1.332(4) .
N1 C6 1.448(4) .
N2 C4 1.328(3) .
N2 C18 1.441(3) .
C1 C2 1.515(4) .
C2 C3 1.402(4) .
C3 C4 1.407(4) .
C4 C5 1.518(4) .
C6 C7 1.394(5) .
C6 C11 1.403(6) .
C7 C8 1.428(6) .
C7 C12 1.502(7) .
C8 C9 1.378(8) .
C9 C10 1.346(8) .
C10 C11 1.397(5) .
C11 C15 1.510(6) .
C12 C13 1.521(7) .
C12 C14 1.542(6) .
C15 C16 1.526(7) .
C15 C17 1.531(7) .
C18 C19 1.396(4) .
C18 C23 1.409(4) .
C19 C20 1.408(4) .
C19 C24 1.508(5) .
C20 C21 1.364(6) .
C21 C22 1.370(6) .
C22 C23 1.396(4) .
C23 C27 1.517(5) .
C24 C25 1.524(5) .
C24 C26 1.531(5) .
C27 C29 1.490(7) .
C27 C28 1.518(6) .
C30 C31 1.478(5) .
C31 C32 1.517(6) .
C32 C33 1.504(5) .
C34 C39 1.353(7) .
C34 C35 1.434(8) .
C34 C40 1.499(8) .
C35 C36 1.408(9) .
C36 C37 1.412(9) .
C37 C38 1.434(8) .
C38 C39 1.462(8) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139042484
