#------------------------------------------------------------------------------
#$Date: 2017-03-05 07:13:20 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193815 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/16/7041670.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_7041670
loop_
_publ_author_name
'Schnitzler, S.'
'Cui, P.'
'Spaniol, T. P.'
'Okuda, J.'
_publ_section_title
;
 Molecular magnesium hydrides supported by an anionic
 triazacyclononane-type ligand.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1761
_journal_page_last               1765
_journal_paper_doi               10.1039/c6dt04654a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C30 H62 Mg2 N6'
_chemical_formula_sum            'C30 H62 Mg2 N6'
_chemical_formula_weight         555.47
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-11-10 deposited with the CCDC.
2017-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                106.2030(19)
_cell_angle_beta                 91.124(2)
_cell_angle_gamma                110.3937(19)
_cell_formula_units_Z            1
_cell_length_a                   8.0801(11)
_cell_length_b                   9.6293(13)
_cell_length_c                   11.6216(15)
_cell_measurement_reflns_used    3220
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.30
_cell_measurement_theta_min      2.37
_cell_volume                     807.00(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11557
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.036
_diffrn_reflns_theta_min         2.369
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_correction_T_min  0.9787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0459P)²+0.3114P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3692
_reflns_number_total             4281
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04654a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7041669--7041670.cif.'
_cod_database_code               7041670
_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.
;
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
Mg1 Mg 0.04834(5) 0.46783(5) 0.62251(3) 0.01374(11) Uani 1 1 d
N1 N -0.15174(13) 0.52648(11) 0.54571(9) 0.0147(2) Uani 1 1 d
N2 N -0.18746(13) 0.30413(11) 0.67569(9) 0.0147(2) Uani 1 1 d
N3 N 0.01028(13) 0.64864(12) 0.78988(9) 0.0159(2) Uani 1 1 d
C1 C 0.26442(16) 0.40323(15) 0.69307(11) 0.0174(2) Uani 1 1 d
H1A H 0.252(2) 0.315(2) 0.6344(15) 0.027(4) Uiso 1 1 d
H1B H 0.356(3) 0.483(2) 0.6784(17) 0.041(5) Uiso 1 1 d
C2 C 0.30646(17) 0.39300(17) 0.81070(12) 0.0234(3) Uani 1 1 d
H2 H 0.359(2) 0.495(2) 0.8795(15) 0.029(4) Uiso 1 1 d
C3 C 0.2813(2) 0.2651(2) 0.84375(15) 0.0324(3) Uani 1 1 d
H3A H 0.233(3) 0.158(2) 0.7804(19) 0.050(6) Uiso 1 1 d
H3B H 0.311(3) 0.275(2) 0.9283(18) 0.043(5) Uiso 1 1 d
C4 C -0.30490(15) 0.37903(14) 0.51175(11) 0.0159(2) Uani 1 1 d
H4A H -0.2789(19) 0.3045(17) 0.4469(13) 0.014(3) Uiso 1 1 d
H4B H -0.414(2) 0.3867(17) 0.4800(13) 0.018(4) Uiso 1 1 d
C5 C -0.35052(15) 0.30515(14) 0.61420(11) 0.0159(2) Uani 1 1 d
H5A H -0.4078(19) 0.3618(17) 0.6727(13) 0.015(3) Uiso 1 1 d
H5B H -0.437(2) 0.2005(17) 0.5827(13) 0.016(3) Uiso 1 1 d
C6 C -0.16054(16) 0.38200(14) 0.80795(11) 0.0174(2) Uani 1 1 d
H6A H -0.052(2) 0.3753(18) 0.8419(14) 0.021(4) Uiso 1 1 d
H6B H -0.261(2) 0.3310(17) 0.8455(13) 0.019(4) Uiso 1 1 d
C7 C -0.13864(16) 0.55293(14) 0.84173(11) 0.0174(2) Uani 1 1 d
H7A H -0.250(2) 0.5639(17) 0.8160(13) 0.017(4) Uiso 1 1 d
H7B H -0.118(2) 0.5931(18) 0.9290(14) 0.020(4) Uiso 1 1 d
C8 C -0.04861(17) 0.74836(14) 0.73470(11) 0.0181(2) Uani 1 1 d
H8A H 0.055(2) 0.8132(18) 0.7076(13) 0.019(4) Uiso 1 1 d
H8B H -0.090(2) 0.8206(18) 0.7939(14) 0.024(4) Uiso 1 1 d
C9 C -0.19473(16) 0.65154(14) 0.62689(11) 0.0165(2) Uani 1 1 d
H9A H -0.3108(19) 0.6118(16) 0.6577(12) 0.012(3) Uiso 1 1 d
H9B H -0.2104(19) 0.7239(17) 0.5860(13) 0.015(3) Uiso 1 1 d
C10 C -0.18228(16) 0.14499(14) 0.65102(11) 0.0171(2) Uani 1 1 d
H10 H -0.071(2) 0.1613(17) 0.6980(13) 0.019(4) Uiso 1 1 d
C11 C -0.33764(18) 0.03123(16) 0.69115(13) 0.0218(3) Uani 1 1 d
H11A H -0.360(2) 0.076(2) 0.7734(17) 0.036(5) Uiso 1 1 d
H11B H -0.313(2) -0.059(2) 0.6907(16) 0.035(5) Uiso 1 1 d
H11C H -0.447(2) -0.005(2) 0.6371(15) 0.031(4) Uiso 1 1 d
C12 C -0.17102(18) 0.07775(15) 0.51744(12) 0.0206(3) Uani 1 1 d
H12A H -0.274(2) 0.0662(18) 0.4670(14) 0.024(4) Uiso 1 1 d
H12B H -0.163(2) -0.0226(19) 0.5023(14) 0.020(4) Uiso 1 1 d
H12C H -0.066(2) 0.1435(19) 0.4918(14) 0.026(4) Uiso 1 1 d
C13 C 0.16709(17) 0.74198(15) 0.88602(11) 0.0194(2) Uani 1 1 d
H13 H 0.182(2) 0.6655(18) 0.9231(14) 0.021(4) Uiso 1 1 d
C14 C 0.1400(2) 0.87346(17) 0.98383(12) 0.0259(3) Uani 1 1 d
H14A H 0.139(2) 0.958(2) 0.9533(16) 0.033(5) Uiso 1 1 d
H14B H 0.237(2) 0.920(2) 1.0469(17) 0.036(5) Uiso 1 1 d
H14C H 0.032(2) 0.837(2) 1.0209(16) 0.033(5) Uiso 1 1 d
C15 C 0.33759(18) 0.80786(18) 0.83275(13) 0.0256(3) Uani 1 1 d
H15A H 0.358(2) 0.729(2) 0.7720(16) 0.032(4) Uiso 1 1 d
H15B H 0.437(2) 0.854(2) 0.8989(16) 0.034(5) Uiso 1 1 d
H15C H 0.338(2) 0.893(2) 0.7996(16) 0.033(5) Uiso 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'
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
N1 Mg1 N1 82.94(4) . 2_566
N1 Mg1 N2 82.54(4) . .
N1 Mg1 N2 134.15(4) 2_566 .
N1 Mg1 C1 176.77(5) . .
N1 Mg1 C1 93.90(4) 2_566 .
N2 Mg1 C1 99.31(4) . .
N1 Mg1 N3 78.79(4) . .
N1 Mg1 N3 135.88(4) 2_566 .
N2 Mg1 N3 82.68(4) . .
C1 Mg1 N3 104.03(4) . .
N1 Mg1 C4 30.25(4) . .
N1 Mg1 C4 91.38(4) 2_566 .
N2 Mg1 C4 57.38(4) . .
C1 Mg1 C4 149.81(5) . .
N3 Mg1 C4 92.46(4) . .
N1 Mg1 C4 90.97(4) . 2_566
N1 Mg1 C4 29.92(4) 2_566 2_566
N2 Mg1 C4 163.95(4) . 2_566
C1 Mg1 C4 86.57(4) . 2_566
N3 Mg1 C4 110.53(4) . 2_566
C4 Mg1 C4 111.37(3) . 2_566
N1 Mg1 Mg1 41.54(3) . 2_566
N1 Mg1 Mg1 41.40(3) 2_566 2_566
N2 Mg1 Mg1 112.26(3) . 2_566
C1 Mg1 Mg1 135.29(4) . 2_566
N3 Mg1 Mg1 110.49(3) . 2_566
C4 Mg1 Mg1 55.97(3) . 2_566
C4 Mg1 Mg1 55.40(3) 2_566 2_566
C9 N1 C4 111.34(9) . .
C9 N1 Mg1 114.99(7) . .
C4 N1 Mg1 102.31(7) . .
C9 N1 Mg1 125.00(8) . 2_566
C4 N1 Mg1 103.09(7) . 2_566
Mg1 N1 Mg1 97.06(4) . 2_566
C6 N2 C5 112.48(9) . .
C6 N2 C10 110.00(9) . .
C5 N2 C10 113.29(9) . .
C6 N2 Mg1 99.94(7) . .
C5 N2 Mg1 107.63(7) . .
C10 N2 Mg1 112.75(7) . .
C8 N3 C7 110.73(9) . .
C8 N3 C13 112.22(10) . .
C7 N3 C13 109.53(9) . .
C8 N3 Mg1 102.81(7) . .
C7 N3 Mg1 103.76(7) . .
C13 N3 Mg1 117.34(7) . .
C2 C1 Mg1 130.63(9) . .
C2 C1 H1A 111.3(11) . .
Mg1 C1 H1A 101.1(11) . .
C2 C1 H1B 109.4(12) . .
Mg1 C1 H1B 94.1(12) . .
H1A C1 H1B 107.6(15) . .
C3 C2 C1 128.39(14) . .
C3 C2 H2 114.4(10) . .
C1 C2 H2 117.1(10) . .
C2 C3 H3A 119.9(12) . .
C2 C3 H3B 119.8(12) . .
H3A C3 H3B 120.3(16) . .
N1 C4 C5 114.27(10) . .
N1 C4 Mg1 47.44(5) . .
C5 C4 Mg1 82.06(6) . .
N1 C4 Mg1 46.99(5) . 2_566
C5 C4 Mg1 150.39(8) . 2_566
Mg1 C4 Mg1 68.63(3) . 2_566
N1 C4 H4A 108.8(9) . .
C5 C4 H4A 106.6(8) . .
Mg1 C4 H4A 87.0(8) . .
Mg1 C4 H4A 68.8(8) 2_566 .
N1 C4 H4B 113.4(9) . .
C5 C4 H4B 107.6(9) . .
Mg1 C4 H4B 160.5(9) . .
Mg1 C4 H4B 101.6(9) 2_566 .
H4A C4 H4B 105.6(12) . .
N2 C5 C4 110.87(9) . .
N2 C5 H5A 110.0(9) . .
C4 C5 H5A 110.1(9) . .
N2 C5 H5B 110.1(9) . .
C4 C5 H5B 110.2(9) . .
H5A C5 H5B 105.3(12) . .
N2 C6 C7 113.70(10) . .
N2 C6 H6A 107.6(9) . .
C7 C6 H6A 108.5(9) . .
N2 C6 H6B 111.0(9) . .
C7 C6 H6B 106.7(9) . .
H6A C6 H6B 109.2(12) . .
N3 C7 C6 113.69(10) . .
N3 C7 H7A 108.5(9) . .
C6 C7 H7A 110.9(9) . .
N3 C7 H7B 109.7(9) . .
C6 C7 H7B 107.0(9) . .
H7A C7 H7B 106.8(12) . .
N3 C8 C9 111.95(10) . .
N3 C8 H8A 107.2(9) . .
C9 C8 H8A 109.5(9) . .
N3 C8 H8B 112.2(9) . .
C9 C8 H8B 109.8(9) . .
H8A C8 H8B 106.0(13) . .
N1 C9 C8 111.80(9) . .
N1 C9 H9A 112.2(8) . .
C8 C9 H9A 109.0(8) . .
N1 C9 H9B 112.4(8) . .
C8 C9 H9B 107.2(9) . .
H9A C9 H9B 103.9(11) . .
N2 C10 C12 110.17(10) . .
N2 C10 C11 114.34(10) . .
C12 C10 C11 110.23(11) . .
N2 C10 H10 104.6(9) . .
C12 C10 H10 108.4(9) . .
C11 C10 H10 108.8(9) . .
C10 C11 H11A 112.6(11) . .
C10 C11 H11B 110.4(11) . .
H11A C11 H11B 106.8(15) . .
C10 C11 H11C 111.9(10) . .
H11A C11 H11C 108.2(14) . .
H11B C11 H11C 106.6(15) . .
C10 C12 H12A 111.8(9) . .
C10 C12 H12B 110.1(9) . .
H12A C12 H12B 108.1(13) . .
C10 C12 H12C 111.6(10) . .
H12A C12 H12C 107.8(13) . .
H12B C12 H12C 107.2(13) . .
N3 C13 C15 111.93(10) . .
N3 C13 C14 114.07(11) . .
C15 C13 C14 109.45(11) . .
N3 C13 H13 104.4(9) . .
C15 C13 H13 107.5(9) . .
C14 C13 H13 109.2(9) . .
C13 C14 H14A 112.0(10) . .
C13 C14 H14B 110.0(11) . .
H14A C14 H14B 104.9(15) . .
C13 C14 H14C 112.6(10) . .
H14A C14 H14C 109.8(14) . .
H14B C14 H14C 107.2(15) . .
C13 C15 H15A 111.3(11) . .
C13 C15 H15B 107.6(10) . .
H15A C15 H15B 108.9(15) . .
C13 C15 H15C 112.9(10) . .
H15A C15 H15C 109.6(14) . .
H15B C15 H15C 106.4(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 N1 2.1425(10) .
Mg1 N1 2.1482(11) 2_566
Mg1 N2 2.2347(11) .
Mg1 C1 2.2568(12) .
Mg1 N3 2.3273(11) .
Mg1 C4 2.8418(13) .
Mg1 C4 2.8613(13) 2_566
Mg1 Mg1 3.2152(8) 2_566
N1 C9 1.4599(15) .
N1 C4 1.4652(15) .
N1 Mg1 2.1482(11) 2_566
N2 C6 1.4839(15) .
N2 C5 1.4908(15) .
N2 C10 1.4940(15) .
N3 C8 1.4866(16) .
N3 C7 1.4919(15) .
N3 C13 1.5007(16) .
C1 C2 1.4402(18) .
C1 H1A 0.902(17) .
C1 H1B 0.92(2) .
C2 C3 1.341(2) .
C2 H2 1.020(17) .
C3 H3A 1.02(2) .
C3 H3B 0.98(2) .
C4 C5 1.5384(17) .
C4 Mg1 2.8613(13) 2_566
C4 H4A 0.968(15) .
C4 H4B 0.981(15) .
C5 H5A 0.978(15) .
C5 H5B 0.966(15) .
C6 C7 1.5259(17) .
C6 H6A 0.987(16) .
C6 H6B 0.973(16) .
C7 H7A 0.993(15) .
C7 H7B 0.967(16) .
C8 C9 1.5349(17) .
C8 H8A 0.975(16) .
C8 H8B 0.984(16) .
C9 H9A 0.997(14) .
C9 H9B 0.986(15) .
C10 C12 1.5242(18) .
C10 C11 1.5307(17) .
C10 H10 0.986(15) .
C11 H11A 0.981(18) .
C11 H11B 0.952(18) .
C11 H11C 0.970(18) .
C12 H12A 0.962(16) .
C12 H12B 0.959(16) .
C12 H12C 0.976(17) .
C13 C15 1.5256(18) .
C13 C14 1.5306(18) .
C13 H13 0.990(16) .
C14 H14A 0.976(18) .
C14 H14B 0.952(19) .
C14 H14C 0.980(18) .
C15 H15A 0.950(18) .
C15 H15B 0.985(19) .
C15 H15C 0.996(18) .
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
_geom_torsion_site_symmetry_4
Mg1 C1 C2 C3 107.65(16) . .
C9 N1 C4 C5 -71.63(12) . .
Mg1 N1 C4 C5 51.71(10) . .
Mg1 N1 C4 C5 152.07(8) 2_566 .
C9 N1 C4 Mg1 -123.34(10) . .
Mg1 N1 C4 Mg1 100.37(6) 2_566 .
C9 N1 C4 Mg1 136.30(10) . 2_566
Mg1 N1 C4 Mg1 -100.37(6) . 2_566
C6 N2 C5 C4 124.54(10) . .
C10 N2 C5 C4 -109.93(11) . .
Mg1 N2 C5 C4 15.42(11) . .
N1 C4 C5 N2 -47.32(13) . .
Mg1 C4 C5 N2 -11.61(8) . .
Mg1 C4 C5 N2 -3.4(2) 2_566 .
C5 N2 C6 C7 -60.53(13) . .
C10 N2 C6 C7 172.17(9) . .
Mg1 N2 C6 C7 53.39(10) . .
C8 N3 C7 C6 133.24(11) . .
C13 N3 C7 C6 -102.48(11) . .
Mg1 N3 C7 C6 23.57(11) . .
N2 C6 C7 N3 -56.74(13) . .
C7 N3 C8 C9 -63.81(12) . .
C13 N3 C8 C9 173.46(9) . .
Mg1 N3 C8 C9 46.48(10) . .
C4 N1 C9 C8 133.98(10) . .
Mg1 N1 C9 C8 18.22(12) . .
Mg1 N1 C9 C8 -101.25(10) 2_566 .
N3 C8 C9 N1 -45.88(13) . .
C6 N2 C10 C12 -168.27(10) . .
C5 N2 C10 C12 64.88(12) . .
Mg1 N2 C10 C12 -57.68(11) . .
C6 N2 C10 C11 66.95(13) . .
C5 N2 C10 C11 -59.90(13) . .
Mg1 N2 C10 C11 177.54(8) . .
C8 N3 C13 C15 -71.86(13) . .
C7 N3 C13 C15 164.74(11) . .
Mg1 N3 C13 C15 46.87(13) . .
C8 N3 C13 C14 53.10(14) . .
C7 N3 C13 C14 -70.30(13) . .
Mg1 N3 C13 C14 171.83(9) . .
