#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/46/1514621.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_1514621
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            'C60 H82 Mg2 N4 O4'
_chemical_formula_weight         971.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5246(9)
_cell_length_b                   15.6210(9)
_cell_length_c                   25.9215(14)
_cell_measurement_temperature    123(2)
_cell_volume                     5881.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35432
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0466
_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)+(0.0424P)²+3.1446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                3987
_reflns_number_total             5177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52242c.txt
_cod_data_source_block           compound1S
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               1514621
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -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
Mg1 Mg 0.36005(4) 0.11933(4) 0.30770(2) 0.02664(17) Uani 1 1 d .
O1 O 0.37008(8) 0.24605(8) 0.30569(5) 0.0313(3) Uani 1 1 d .
O2 O 0.27446(9) 0.35911(8) 0.30336(5) 0.0315(3) Uani 1 1 d .
C30 C 0.29186(12) 0.28061(12) 0.30447(6) 0.0251(4) Uani 1 1 d .
N1 N 0.39588(11) 0.05033(10) 0.36966(5) 0.0322(4) Uani 1 1 d .
N2 N 0.43196(10) 0.05225(9) 0.25615(5) 0.0253(3) Uani 1 1 d .
C19 C 0.53899(13) 0.12595(12) 0.19757(7) 0.0313(4) Uani 1 1 d .
C4 C 0.46233(12) -0.02656(11) 0.26732(7) 0.0267(4) Uani 1 1 d .
C3 C 0.45824(12) -0.06279(12) 0.31664(7) 0.0297(4) Uani 1 1 d .
H3 H 0.4744 -0.1217 0.3181 0.036 Uiso 1 1 calc R
C23 C 0.38108(14) 0.09642(13) 0.16961(7) 0.0329(5) Uani 1 1 d .
C18 C 0.45165(13) 0.08967(11) 0.20651(7) 0.0271(4) Uani 1 1 d .
C24 C 0.61516(13) 0.12270(13) 0.23784(7) 0.0343(5) Uani 1 1 d .
H24 H 0.5993 0.0765 0.2630 0.041 Uiso 1 1 calc R
C6 C 0.37903(15) 0.08715(14) 0.41968(7) 0.0381(5) Uani 1 1 d .
C2 C 0.43408(14) -0.02643(13) 0.36452(7) 0.0342(5) Uani 1 1 d .
C22 C 0.40045(15) 0.13870(14) 0.12361(7) 0.0407(5) Uani 1 1 d .
H22 H 0.3539 0.1430 0.0980 0.049 Uiso 1 1 calc R
C27 C 0.28634(15) 0.05846(16) 0.17812(8) 0.0464(6) Uani 1 1 d .
H27 H 0.2823 0.0413 0.2152 0.056 Uiso 1 1 calc R
C20 C 0.55339(15) 0.16810(14) 0.15093(8) 0.0431(5) Uani 1 1 d .
H20 H 0.6118 0.1931 0.1442 0.052 Uiso 1 1 calc R
C5 C 0.50661(15) -0.07945(13) 0.22553(8) 0.0387(5) Uani 1 1 d .
H5A H 0.4686 -0.0772 0.1943 0.058 Uiso 1 1 calc R
H5B H 0.5121 -0.1389 0.2372 0.058 Uiso 1 1 calc R
H5C H 0.5679 -0.0566 0.2179 0.058 Uiso 1 1 calc R
C25 C 0.61872(15) 0.20730(14) 0.26745(8) 0.0422(5) Uani 1 1 d .
H25A H 0.6336 0.2539 0.2436 0.063 Uiso 1 1 calc R
H25B H 0.6661 0.2039 0.2943 0.063 Uiso 1 1 calc R
H25C H 0.5587 0.2183 0.2834 0.063 Uiso 1 1 calc R
C7 C 0.44344(16) 0.14630(15) 0.43937(7) 0.0422(5) Uani 1 1 d .
C11 C 0.29602(15) 0.07014(16) 0.44587(7) 0.0449(6) Uani 1 1 d .
C21 C 0.48510(16) 0.17437(15) 0.11434(8) 0.0468(6) Uani 1 1 d .
H21 H 0.4966 0.2033 0.0828 0.056 Uiso 1 1 calc R
C12 C 0.53386(16) 0.16620(15) 0.41282(8) 0.0457(6) Uani 1 1 d .
H12 H 0.5342 0.1355 0.3790 0.055 Uiso 1 1 calc R
C26 C 0.70952(14) 0.10159(14) 0.21498(8) 0.0419(5) Uani 1 1 d .
H26A H 0.7066 0.0463 0.1971 0.063 Uiso 1 1 calc R
H26B H 0.7552 0.0986 0.2427 0.063 Uiso 1 1 calc R
H26C H 0.7272 0.1463 0.1904 0.063 Uiso 1 1 calc R
C1 C 0.45594(18) -0.07906(16) 0.41175(8) 0.0545(7) Uani 1 1 d .
H1A H 0.4922 -0.0446 0.4359 0.082 Uiso 1 1 calc R
H1B H 0.4913 -0.1298 0.4016 0.082 Uiso 1 1 calc R
H1C H 0.3985 -0.0970 0.4284 0.082 Uiso 1 1 calc R
C10 C 0.28071(18) 0.11271(18) 0.49267(8) 0.0558(7) Uani 1 1 d .
H10 H 0.2256 0.1017 0.5113 0.067 Uiso 1 1 calc R
C8 C 0.42314(18) 0.18651(16) 0.48593(8) 0.0513(6) Uani 1 1 d .
H8 H 0.4658 0.2265 0.4998 0.062 Uiso 1 1 calc R
C9 C 0.34328(19) 0.17005(18) 0.51243(8) 0.0593(7) Uani 1 1 d .
H9 H 0.3313 0.1981 0.5442 0.071 Uiso 1 1 calc R
C13 C 0.54602(18) 0.26179(16) 0.40194(9) 0.0568(6) Uani 1 1 d .
H13A H 0.4951 0.2820 0.3803 0.085 Uiso 1 1 calc R
H13B H 0.6045 0.2711 0.3839 0.085 Uiso 1 1 calc R
H13C H 0.5462 0.2934 0.4346 0.085 Uiso 1 1 calc R
C15 C 0.22302(15) 0.00954(17) 0.42558(8) 0.0503(6) Uani 1 1 d .
H15 H 0.2461 -0.0146 0.3923 0.060 Uiso 1 1 calc R
C16 C 0.13233(17) 0.0557(2) 0.41431(10) 0.0643(8) Uani 1 1 d .
H16A H 0.1063 0.0776 0.4466 0.096 Uiso 1 1 calc R
H16B H 0.0889 0.0156 0.3984 0.096 Uiso 1 1 calc R
H16C H 0.1437 0.1035 0.3907 0.096 Uiso 1 1 calc R
C17 C 0.2043(2) -0.06593(19) 0.46212(10) 0.0715(8) Uani 1 1 d .
H17A H 0.2613 -0.0983 0.4674 0.107 Uiso 1 1 calc R
H17B H 0.1575 -0.1034 0.4469 0.107 Uiso 1 1 calc R
H17C H 0.1821 -0.0442 0.4953 0.107 Uiso 1 1 calc R
C14 C 0.61543(18) 0.13357(19) 0.44429(9) 0.0636(7) Uani 1 1 d .
H14A H 0.6168 0.1627 0.4778 0.095 Uiso 1 1 calc R
H14B H 0.6727 0.1453 0.4256 0.095 Uiso 1 1 calc R
H14C H 0.6092 0.0718 0.4497 0.095 Uiso 1 1 calc R
C29 C 0.2734(2) -0.0223(2) 0.14594(11) 0.1000(13) Uani 1 1 d .
H29A H 0.2816 -0.0085 0.1093 0.150 Uiso 1 1 calc R
H29B H 0.2113 -0.0450 0.1515 0.150 Uiso 1 1 calc R
H29C H 0.3190 -0.0652 0.1563 0.150 Uiso 1 1 calc R
C28 C 0.21002(17) 0.1232(3) 0.16820(12) 0.0946(13) Uani 1 1 d .
H28A H 0.2208 0.1745 0.1891 0.142 Uiso 1 1 calc R
H28B H 0.1505 0.0979 0.1776 0.142 Uiso 1 1 calc R
H28C H 0.2096 0.1387 0.1316 0.142 Uiso 1 1 calc R
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 O2 84.35(5) . 2
O1 Mg1 N2 117.90(6) . .
O2 Mg1 N2 124.52(6) 2 .
O1 Mg1 N1 122.58(7) . .
O2 Mg1 N1 113.10(7) 2 .
N2 Mg1 N1 96.80(7) . .
O1 Mg1 C30 58.87(5) . 2
O2 Mg1 C30 25.55(5) 2 2
N2 Mg1 C30 135.26(6) . 2
N1 Mg1 C30 123.21(6) . 2
O1 Mg1 C30 25.66(5) . .
O2 Mg1 C30 58.71(5) 2 .
N2 Mg1 C30 131.29(6) . .
N1 Mg1 C30 128.34(6) . .
C30 Mg1 C30 33.21(7) 2 .
C30 O1 Mg1 111.24(11) . .
C30 O2 Mg1 111.30(12) . 2
O2 C30 O1 127.08(17) . .
O2 C30 C30 116.54(19) . 2
O1 C30 C30 116.38(19) . 2
O2 C30 Mg1 43.15(8) . 2
O1 C30 Mg1 169.60(13) . 2
C30 C30 Mg1 73.51(13) 2 2
O2 C30 Mg1 170.17(13) . .
O1 C30 Mg1 43.10(9) . .
C30 C30 Mg1 73.28(13) 2 .
Mg1 C30 Mg1 146.59(7) 2 .
C2 N1 C6 121.49(15) . .
C2 N1 Mg1 120.93(12) . .
C6 N1 Mg1 117.58(12) . .
C4 N2 C18 120.01(15) . .
C4 N2 Mg1 120.72(12) . .
C18 N2 Mg1 119.27(11) . .
C20 C19 C18 117.93(18) . .
C20 C19 C24 120.13(17) . .
C18 C19 C24 121.91(16) . .
N2 C4 C3 123.72(16) . .
N2 C4 C5 119.28(16) . .
C3 C4 C5 116.96(17) . .
C4 C3 C2 130.71(18) . .
C4 C3 H3 114.6 . .
C2 C3 H3 114.6 . .
C22 C23 C18 118.11(18) . .
C22 C23 C27 119.62(18) . .
C18 C23 C27 122.27(17) . .
C23 C18 C19 120.97(16) . .
C23 C18 N2 119.54(16) . .
C19 C18 N2 119.23(16) . .
C19 C24 C25 109.87(16) . .
C19 C24 C26 113.13(16) . .
C25 C24 C26 110.52(17) . .
C19 C24 H24 107.7 . .
C25 C24 H24 107.7 . .
C26 C24 H24 107.7 . .
C11 C6 C7 121.11(19) . .
C11 C6 N1 120.3(2) . .
C7 C6 N1 118.36(18) . .
N1 C2 C3 123.80(17) . .
N1 C2 C1 119.91(17) . .
C3 C2 C1 116.27(18) . .
C21 C22 C23 121.61(19) . .
C21 C22 H22 119.2 . .
C23 C22 H22 119.2 . .
C23 C27 C28 112.2(2) . .
C23 C27 C29 110.9(2) . .
C28 C27 C29 111.5(3) . .
C23 C27 H27 107.3 . .
C28 C27 H27 107.3 . .
C29 C27 H27 107.3 . .
C21 C20 C19 121.6(2) . .
C21 C20 H20 119.2 . .
C19 C20 H20 119.2 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C8 C7 C6 118.0(2) . .
C8 C7 C12 119.0(2) . .
C6 C7 C12 123.02(18) . .
C10 C11 C6 117.6(2) . .
C10 C11 C15 119.1(2) . .
C6 C11 C15 123.31(19) . .
C22 C21 C20 119.78(19) . .
C22 C21 H21 120.1 . .
C20 C21 H21 120.1 . .
C7 C12 C14 111.20(19) . .
C7 C12 C13 112.59(19) . .
C14 C12 C13 109.6(2) . .
C7 C12 H12 107.8 . .
C14 C12 H12 107.8 . .
C13 C12 H12 107.8 . .
C24 C26 H26A 109.5 . .
C24 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C24 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C9 C10 C11 121.8(2) . .
C9 C10 H10 119.1 . .
C11 C10 H10 119.1 . .
C9 C8 C7 121.9(2) . .
C9 C8 H8 119.0 . .
C7 C8 H8 119.0 . .
C8 C9 C10 119.6(2) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C15 C16 112.0(2) . .
C11 C15 C17 112.90(19) . .
C16 C15 C17 109.1(2) . .
C11 C15 H15 107.5 . .
C16 C15 H15 107.5 . .
C17 C15 H15 107.5 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C27 C29 H29A 109.5 . .
C27 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C27 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 O1 1.9855(15) .
Mg1 O2 1.9858(14) 2
Mg1 N2 1.9936(15) .
Mg1 N1 2.0029(16) .
Mg1 C30 2.7052(19) 2
Mg1 C30 2.7084(19) .
O1 C30 1.258(2) .
O2 C30 1.252(2) .
O2 Mg1 1.9858(14) 2
C30 C30 1.547(4) 2
C30 Mg1 2.7052(19) 2
N1 C2 1.328(3) .
N1 C6 1.439(2) .
N2 C4 1.339(2) .
N2 C18 1.442(2) .
C19 C20 1.392(3) .
C19 C18 1.409(3) .
C19 C24 1.522(3) .
C4 C3 1.399(3) .
C4 C5 1.507(3) .
C3 C2 1.409(3) .
C3 H3 0.9500 .
C23 C22 1.392(3) .
C23 C18 1.406(3) .
C23 C27 1.515(3) .
C24 C25 1.529(3) .
C24 C26 1.529(3) .
C24 H24 1.0000 .
C6 C11 1.409(3) .
C6 C7 1.411(3) .
C2 C1 1.509(3) .
C22 C21 1.371(3) .
C22 H22 0.9500 .
C27 C28 1.522(4) .
C27 C29 1.523(4) .
C27 H27 1.0000 .
C20 C21 1.376(3) .
C20 H20 0.9500 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C7 C8 1.392(3) .
C7 C12 1.515(3) .
C11 C10 1.401(3) .
C11 C15 1.516(3) .
C21 H21 0.9500 .
C12 C14 1.526(3) .
C12 C13 1.530(3) .
C12 H12 1.0000 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C10 C9 1.375(4) .
C10 H10 0.9500 .
C8 C9 1.372(3) .
C8 H8 0.9500 .
C9 H9 0.9500 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C15 C16 1.530(3) .
C15 C17 1.536(4) .
C15 H15 1.0000 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
