#------------------------------------------------------------------------------
#$Date: 2019-11-25 12:07:51 +0100 (lun 25 de nov de 2019) $
#$Revision: 240926 $
#$URL: svn://www.crystallography.net/cod/cif/4/13/05/4130519.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_4130519
loop_
_publ_author_name
'Keyzer, Evan N.'
'Glass, Hugh F. J.'
'Liu, Zigeng'
'Bayley, Paul M.'
'Dutton, Siân E'
'Grey, Clare P.'
'Wright, Dominic S.'
_publ_section_title
;
 Mg(PF6)2-Based Electrolyte Systems: Understanding Electrolyte-Electrode
 Interactions for the Development of Mg-Ion Batteries.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8682
_journal_page_last               8685
_journal_paper_doi               10.1021/jacs.6b04319
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C12 H18 Mg N6 2+, 2(F6 P -)'
_chemical_formula_sum            'C12 H18 F12 Mg N6 P2'
_chemical_formula_weight         560.57
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.1793(2)
_cell_length_b                   11.1793(2)
_cell_length_c                   16.6946(8)
_cell_measurement_reflns_used    1661
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.52
_cell_measurement_theta_min      5.28
_cell_volume                     1806.91(10)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.910
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2227
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        66.511
_diffrn_reflns_theta_max         66.511
_diffrn_reflns_theta_min         5.281
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    2.901
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00058(13)
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         640
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0354
_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)+(0.0361P)²+2.5616P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                565
_reflns_number_total             640
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b04319_si_001.cif
_cod_data_source_block           DW_b2_0008
_cod_original_cell_volume        1806.91(11)
_cod_database_code               4130519
_cambridge_user_name             'Evan Keyzer'
_cambridge_user_crsid            ek406
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             EWK-1-65
_cambridge_data_id               DW_B2_0008
_ccdc_publ_extra_info
;
_cambridge_sample_id EWK-1-65
_cambridge_data_id DW_B2_0008
;
_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   0.595
_shelx_estimated_absorpt_t_max   0.869
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Mg1 Mg 0.0000 0.0000 0.5000 0.0261(4) Uani 1 6 d S T P
N1 N 0.15736(18) 0.16214(18) 0.42900(10) 0.0348(5) Uani 1 1 d . . .
C1 C 0.2484(2) 0.2514(2) 0.39736(11) 0.0327(5) Uani 1 1 d . . .
C2 C 0.3633(2) 0.3633(2) 0.35618(15) 0.0484(7) Uani 1 1 d . . .
H2A H 0.4493 0.3670 0.3724 0.073 Uiso 1 1 calc R U .
H2B H 0.3678 0.4508 0.3699 0.073 Uiso 1 1 calc R U .
H2C H 0.3508 0.3484 0.2982 0.073 Uiso 1 1 calc R U .
P1 P 0.6667 0.3333 0.16257(5) 0.0393(4) Uani 1 3 d DS T P
F1 F 0.6635(10) 0.4552(6) 0.1167(3) 0.0833(15) Uani 0.622 1 d D . P
F2 F 0.5423(8) 0.3306(12) 0.2062(3) 0.0813(17) Uani 0.622 1 d D . P
F1A F 0.6640(13) 0.4056(12) 0.0835(5) 0.099(6) Uani 0.263 1 d D . P
F2A F 0.6661(19) 0.2600(16) 0.2427(6) 0.123(8) Uani 0.263 1 d D . P
F1B F 0.584(5) 0.406(6) 0.168(3) 0.101(9) Uani 0.115 1 d . . P
F2B F 0.750(7) 0.500(2) 0.164(4) 0.119(12) Uani 0.115 1 d . . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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 180.0 11_556 2
N1 Mg1 N1 92.38(6) 11_556 12_556
N1 Mg1 N1 87.62(6) 2 12_556
N1 Mg1 N1 87.62(6) 11_556 3
N1 Mg1 N1 92.38(6) 2 3
N1 Mg1 N1 180.0 12_556 3
N1 Mg1 N1 92.38(6) 11_556 10_556
N1 Mg1 N1 87.62(6) 2 10_556
N1 Mg1 N1 92.38(6) 12_556 10_556
N1 Mg1 N1 87.62(6) 3 10_556
N1 Mg1 N1 87.62(6) 11_556 .
N1 Mg1 N1 92.38(6) 2 .
N1 Mg1 N1 87.62(6) 12_556 .
N1 Mg1 N1 92.38(6) 3 .
N1 Mg1 N1 180.00(7) 10_556 .
C1 N1 Mg1 173.73(16) . .
N1 C1 C2 179.1(2) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mg1 N1 2.1439(18) 11_556
Mg1 N1 2.1439(18) 2
Mg1 N1 2.1439(18) 12_556
Mg1 N1 2.1439(18) 3
Mg1 N1 2.1439(18) 10_556
Mg1 N1 2.1439(18) .
N1 C1 1.138(3) .
C1 C2 1.442(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
P1 F2 1.556(4) .
P1 F1A 1.556(8) .
P1 F2A 1.567(9) .
P1 F1B 1.509(17) .
