#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:43:29 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180274 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/60/7116096.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_7116096
loop_
_publ_author_name
'T. Kruczynski'
'P. Henke'
'T. Augenstein'
'N. Arleth'
'F. Breher'
'H. Schnockel'
_publ_section_title
;
 From MgBr via single-electron transfer (SET) to a paramagnetic Mg(II)
 compound and back to Mg(I): [MgBr(L¹)^.^]2 and [K(thf)3]2[Mg2(L¹)2],
 L¹ == RN[double bond, length as m-dash]C(Me)C(Me)[double bond, length
 as m-dash]NR, R == 2,6-diisopropylphenyl
;
_journal_name_full               Chem.Commun.
_journal_page_first              15677
_journal_paper_doi               10.1039/C4cc07680J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C56 H80 Cl2 Mg2 N4'
_chemical_formula_sum            'C56 H80 Cl2 Mg2 N4'
_chemical_formula_weight         928.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 123.10(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.096(4)
_cell_length_b                   18.733(4)
_cell_length_c                   11.813(2)
_cell_measurement_reflns_used    19799
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      1.56
_cell_volume                     3354.7(16)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
 200 frames, detector distance = 120 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14206
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.703
_diffrn_reflns_theta_min         1.728
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.919
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.086
_platon_squeeze_details
;
;
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0963P)²+0.8414P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3230
_reflns_number_total             3630
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc07680j2.cif
_cod_data_source_block           c2m
_cod_original_cell_volume        3354.7(15)
_cod_database_code               7116096
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2013-2
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C9(H9A,H9B,
 H9C), C8(H8A,H8B,H8C)
;
_olex2_submission_special_instructions 'No special instructions were received'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C12 C 0.59689(14) 0.87716(15) 0.1871(2) 0.0859(7) Uani 1 1 d . . .
H12A H 0.5790 0.8308 0.2029 0.129 Uiso 1 1 calc GR . .
H12B H 0.5857 0.8781 0.0960 0.129 Uiso 1 1 calc GR . .
H12C H 0.5629 0.9152 0.1954 0.129 Uiso 1 1 calc GR . .
C3 C 0.74616(12) 0.76216(8) 0.30191(18) 0.0558(4) Uani 1 1 d . . .
H3 H 0.7055 0.7477 0.3247 0.067 Uiso 1 1 calc R . .
C11 C 0.71446(14) 0.88900(13) 0.4336(2) 0.0757(6) Uani 1 1 d . . .
H11A H 0.7775 0.8979 0.4985 0.114 Uiso 1 1 calc GR . .
H11B H 0.6985 0.8426 0.4527 0.114 Uiso 1 1 calc GR . .
H11C H 0.6799 0.9267 0.4415 0.114 Uiso 1 1 calc GR . .
C13 C 0.76233(8) 0.96186(7) 0.10639(12) 0.0346(3) Uani 1 1 d . . .
C1 C 0.81168(8) 0.85437(6) 0.24150(12) 0.0359(3) Uani 1 1 d . . .
C5 C 0.85864(12) 0.73188(7) 0.26315(16) 0.0516(4) Uani 1 1 d . . .
H5 H 0.8952 0.6968 0.2594 0.062 Uiso 1 1 calc R . .
C6 C 0.86663(9) 0.80363(7) 0.23648(14) 0.0417(3) Uani 1 1 d . . .
C14 C 0.69844(11) 0.92064(8) -0.01960(14) 0.0491(4) Uani 1 1 d . . .
H14A H 0.7067 0.8694 0.0000 0.074 Uiso 1 1 calc GR . .
H14B H 0.7091 0.9317 -0.0906 0.074 Uiso 1 1 calc GR . .
H14C H 0.6379 0.9340 -0.0502 0.074 Uiso 1 1 calc GR . .
C2 C 0.75145(10) 0.83429(8) 0.27648(15) 0.0450(3) Uani 1 1 d . . .
C9 C 1.02811(12) 0.80674(11) 0.3215(2) 0.0702(5) Uani 1 1 d . . .
H9A H 1.0354 0.7549 0.3334 0.105 Uiso 1 1 calc GR . .
H9B H 1.0388 0.8286 0.4046 0.105 Uiso 1 1 calc GR . .
H9C H 1.0703 0.8258 0.3017 0.105 Uiso 1 1 calc GR . .
C7 C 0.93376(11) 0.82387(8) 0.20384(17) 0.0502(4) Uani 1 1 d . . .
H7 H 0.9298 0.8766 0.1888 0.060 Uiso 1 1 calc R . .
C4 C 0.79909(13) 0.71157(8) 0.29447(18) 0.0573(4) Uani 1 1 d . . .
H4 H 0.7941 0.6627 0.3111 0.069 Uiso 1 1 calc R . .
C10 C 0.69500(11) 0.88877(9) 0.29109(19) 0.0540(4) Uani 1 1 d . . .
H10 H 0.7107 0.9370 0.2741 0.065 Uiso 1 1 calc R . .
C8 C 0.91324(15) 0.78768(12) 0.0735(2) 0.0711(5) Uani 1 1 d . . .
H8A H 0.8534 0.8005 -0.0007 0.107 Uiso 1 1 calc GR . .
H8B H 0.9174 0.7358 0.0858 0.107 Uiso 1 1 calc GR . .
H8C H 0.9557 0.8036 0.0518 0.107 Uiso 1 1 calc GR . .
Cl1 Cl 0.94632(3) 1.0000 0.58524(4) 0.04301(17) Uani 1 2 d S T P
Mg1 Mg 0.90630(4) 1.0000 0.35927(6) 0.03388(19) Uani 1 2 d S T P
N1 N 0.82091(7) 0.92858(5) 0.22304(10) 0.0332(2) Uani 1 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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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
H12A C12 H12B 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
C2 C3 H3 119.4 . .
C4 C3 H3 119.4 . .
C4 C3 C2 121.13(15) . .
H11A C11 H11B 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
C13 C13 C14 120.84(8) 6_575 .
C13 C13 Mg1 75.10(3) 6_575 .
C14 C13 Mg1 163.18(10) . .
N1 C13 C13 117.55(7) . 6_575
N1 C13 C14 121.61(12) . .
C6 C1 C2 120.75(12) . .
C6 C1 N1 120.56(12) . .
C2 C1 N1 118.46(12) . .
C6 C5 H5 119.4 . .
C4 C5 H5 119.4 . .
C4 C5 C6 121.21(15) . .
C1 C6 C5 118.51(14) . .
C1 C6 C7 121.96(12) . .
C5 C6 C7 119.53(13) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C3 C2 C1 118.34(14) . .
C3 C2 C10 119.70(14) . .
C1 C2 C10 121.93(12) . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
C6 C7 C9 111.60(14) . .
C6 C7 H7 107.7 . .
C6 C7 C8 111.02(14) . .
C9 C7 H7 107.7 . .
C8 C7 C9 110.92(15) . .
C8 C7 H7 107.7 . .
C3 C4 H4 120.0 . .
C5 C4 C3 120.03(14) . .
C5 C4 H4 120.0 . .
C12 C10 H10 107.5 . .
C11 C10 C12 110.87(16) . .
C11 C10 H10 107.5 . .
C2 C10 C12 111.83(16) . .
C2 C10 C11 111.36(15) . .
C2 C10 H10 107.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
Mg1 Cl1 Mg1 85.22(4) . 5_776
C13 Mg1 C13 29.80(5) 6_575 .
C13 Mg1 Mg1 163.03(3) . 5_776
C13 Mg1 Mg1 163.03(3) 6_575 5_776
Cl1 Mg1 C13 138.28(4) . .
Cl1 Mg1 C13 138.28(4) . 6_575
Cl1 Mg1 C13 123.32(4) 5_776 .
Cl1 Mg1 C13 123.32(4) 5_776 6_575
Cl1 Mg1 Cl1 94.79(4) . 5_776
Cl1 Mg1 Mg1 47.65(3) . 5_776
Cl1 Mg1 Mg1 47.13(3) 5_776 5_776
N1 Mg1 C13 27.11(4) 6_575 6_575
N1 Mg1 C13 56.75(5) . 6_575
N1 Mg1 C13 56.75(5) 6_575 .
N1 Mg1 C13 27.11(4) . .
N1 Mg1 Cl1 122.22(4) . .
N1 Mg1 Cl1 118.49(4) . 5_776
N1 Mg1 Cl1 118.50(4) 6_575 5_776
N1 Mg1 Cl1 122.22(4) 6_575 .
N1 Mg1 Mg1 138.25(3) . 5_776
N1 Mg1 Mg1 138.25(3) 6_575 5_776
N1 Mg1 N1 83.31(7) . 6_575
C13 N1 C1 120.87(10) . .
C13 N1 Mg1 110.00(8) . .
C1 N1 Mg1 128.78(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C12 C10 1.525(3) .
C3 H3 0.9500 .
C3 C2 1.399(2) .
C3 C4 1.384(3) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C11 C10 1.520(3) .
C13 C13 1.429(2) 6_575
C13 C14 1.5061(18) .
C13 Mg1 2.7789(18) .
C13 N1 1.3475(17) .
C1 C6 1.4000(19) .
C1 C2 1.4115(19) .
C1 N1 1.4310(15) .
C5 H5 0.9500 .
C5 C6 1.4058(19) .
C5 C4 1.371(3) .
C6 C7 1.510(2) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C2 C10 1.519(2) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C9 C7 1.536(3) .
C7 H7 1.0000 .
C7 C8 1.531(2) .
C4 H4 0.9500 .
C10 H10 1.0000 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
Cl1 Mg1 2.3536(10) .
Cl1 Mg1 2.3733(10) 5_776
Mg1 C13 2.7789(18) 6_575
Mg1 Cl1 2.3734(10) 5_776
Mg1 Mg1 3.200(2) 5_776
Mg1 N1 2.0128(12) 6_575
Mg1 N1 2.0128(12) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C3 C2 C10 C12 -65.4(2) .
C3 C2 C10 C11 59.2(2) .
C13 C13 N1 C1 164.73(8) 6_575
C13 C13 N1 Mg1 -9.03(9) 6_575
C1 C6 C7 C9 118.21(15) .
C1 C6 C7 C8 -117.49(16) .
C1 C2 C10 C12 116.44(18) .
C1 C2 C10 C11 -118.90(17) .
C5 C6 C7 C9 -61.62(18) .
C5 C6 C7 C8 62.68(19) .
C6 C1 C2 C3 -1.9(2) .
C6 C1 C2 C10 176.21(14) .
C6 C1 N1 C13 104.92(15) .
C6 C1 N1 Mg1 -82.62(15) .
C6 C5 C4 C3 -0.8(3) .
C14 C13 N1 C1 -14.80(19) .
C14 C13 N1 Mg1 171.45(11) .
C2 C3 C4 C5 0.7(3) .
C2 C1 C6 C5 1.9(2) .
C2 C1 C6 C7 -177.98(13) .
C2 C1 N1 C13 -80.55(16) .
C2 C1 N1 Mg1 91.92(14) .
C4 C3 C2 C1 0.6(2) .
C4 C3 C2 C10 -177.54(16) .
C4 C5 C6 C1 -0.5(2) .
C4 C5 C6 C7 179.34(15) .
Mg1 C13 N1 C1 173.76(15) .
N1 C1 C6 C5 176.27(12) .
N1 C1 C6 C7 -3.6(2) .
N1 C1 C2 C3 -176.46(13) .
N1 C1 C2 C10 1.7(2) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.034 0.000 -0.034 400.7 -1.5
2 0.000 0.500 0.000 14.9 -0.7
3 0.304 0.500 -0.196 400.7 -1.5
4 0.500 0.000 0.000 14.9 -0.7
