 
data_r-3
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C5.56 H Mg O4.56' 
_chemical_formula_weight          165.10

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'  -0.0020   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'
 'O'  'O'  -0.0041   0.0059
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mg'  'Mg'   0.0432   0.0356
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            148
_space_group_name_H-M_alt         'R -3 :H'
_space_group_name_Hall            '-R 3'
 
_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.
;
 
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'
 
_cell_length_a                    25.822(4)
_cell_length_b                    25.822(4)
_cell_length_c                    6.9350(14)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      4004.6(14)
_cell_formula_units_Z             18
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     66308
_cell_measurement_theta_min       0.71
_cell_measurement_theta_max       50.00
 
_exptl_crystal_description       'hexagonal column'
_exptl_crystal_colour             Yellow
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.232          
_exptl_crystal_F_000              1492
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.170
_exptl_crystal_size_mid           0.140
_exptl_crystal_size_min           0.040
_exptl_absorpt_coefficient_mu     0.161
_shelx_estimated_absorpt_T_min    0.973
_shelx_estimated_absorpt_T_max    0.994
_exptl_absorpt_correction_type    'empirical'
_exptl_absorpt_correction_T_min   0.8750
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    'HKL3000sm Scalepack (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.700
_diffrn_radiation_type            synchrotron
_diffrn_source                    'PLSII 2D bending magnet'
_diffrn_measurement_device_type   'ADSC Q210 CCD area detector' 
_diffrn_measurement_method        'omega scan' 
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             2507
_diffrn_reflns_av_unetI/netI      0.0129
_diffrn_reflns_av_R_equivalents   ?
_diffrn_reflns_limit_h_min        -36
_diffrn_reflns_limit_h_max        34
_diffrn_reflns_limit_k_min        -36
_diffrn_reflns_limit_k_max        36
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          3.029
_diffrn_reflns_theta_max          29.561
_diffrn_reflns_theta_full         24.835
_diffrn_measured_fraction_theta_max   0.960
_diffrn_measured_fraction_theta_full  0.965
_diffrn_reflns_Laue_measured_fraction_max    0.960
_diffrn_reflns_Laue_measured_fraction_full   0.965
_diffrn_reflns_point_group_measured_fraction_max   0.960
_diffrn_reflns_point_group_measured_fraction_full  0.965
_reflns_number_total              2507
_reflns_number_gt                 2363
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
 
_computing_data_collection        'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction         'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-2018/3 (Sheldrick, 2018)' 
_computing_molecular_graphics     'DIAMOND 4 (Putz & Brandenburg, 2014)'
_computing_publication_material    'enCifer 1.5.1'
_refine_special_details
;
 Refined as a 3-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1318P)²+3.3315P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.046(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2507
_refine_ls_number_parameters      114
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0499
_refine_ls_R_factor_gt            0.0482
_refine_ls_wR_factor_ref          0.1472
_refine_ls_wR_factor_gt           0.1431
_refine_ls_goodness_of_fit_ref    0.838
_refine_ls_restrained_S_all       0.838
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Mg1 Mg 0.36214(2) 0.04833(2) 0.02439(7) 0.0222(2) Uani 1 1 d . . . . .
O1 O 0.29677(4) -0.02934(4) 0.14333(14) 0.0235(2) Uani 1 1 d . . . . .
O2 O 0.23144(4) -0.07318(4) -0.09394(14) 0.0248(3) Uani 1 1 d . . . . .
O3 O 0.05860(4) -0.25193(4) 0.17252(14) 0.0234(2) Uani 1 1 d . . . . .
C1 C 0.24750(6) -0.07184(6) 0.07826(19) 0.0230(3) Uani 1 1 d . . . . .
C2 C 0.20794(6) -0.12037(6) 0.21435(19) 0.0233(3) Uani 1 1 d . . . . .
C3 C 0.15313(6) -0.16498(6) 0.14236(19) 0.0243(3) Uani 1 1 d . . . . .
H3 H 0.144414 -0.163551 0.010036 0.029 Uiso 1 1 calc R U . . .
C4 C 0.11038(6) -0.21172(6) 0.25566(19) 0.0231(3) Uani 1 1 d . . . . .
O1C O 0.48665(14) 0.18762(13) -0.1235(5) 0.1023(13) Uani 0.825(5) 1 d . . P . .
C1C C 0.44791(11) 0.13919(12) -0.0911(3) 0.0462(6) Uani 0.825(5) 1 d . . P . .
O2C O 0.5051(3) 0.1379(3) -0.5312(12) 0.153(3) Uani 0.737(6) 1 d . . P . .
C2C C 0.5201(4) 0.1563(3) -0.6687(11) 0.112(3) Uani 0.737(6) 1 d . . P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Mg1 O3 2.0160(11) 12 ?
Mg1 O3 2.0174(11) 14 ?
Mg1 O2 2.0346(11) 6 ?
Mg1 O1 2.0412(11) . ?
Mg1 O1 2.0710(11) 8_544 ?
Mg1 C1C 2.420(2) . ?
Mg1 Mg1 2.9818(6) 6 ?
Mg1 Mg1 2.9818(6) 8_544 ?
O1 C1 1.2769(16) . ?
O2 C1 1.2590(16) . ?
O3 C4 1.3453(15) . ?
C1 C2 1.4915(19) . ?
C2 C3 1.3960(18) . ?
C2 C4 1.4226(19) 16_545 ?
C3 C4 1.4001(18) . ?
O1C C1C 1.168(3) . ?
O2C C2C 1.049(9) . ?
 
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
 _geom_angle_publ_flag
O3 Mg1 O3 163.33(5) 12 14 ?
O3 Mg1 O2 100.45(4) 12 6 ?
O3 Mg1 O2 96.21(4) 14 6 ?
O3 Mg1 O1 97.28(4) 12 . ?
O3 Mg1 O1 81.40(4) 14 . ?
O2 Mg1 O1 95.18(4) 6 . ?
O3 Mg1 O1 80.71(4) 12 8_544 ?
O3 Mg1 O1 82.62(4) 14 8_544 ?
O2 Mg1 O1 178.73(5) 6 8_544 ?
O1 Mg1 O1 84.15(2) . 8_544 ?
O3 Mg1 C1C 89.60(7) 12 . ?
O3 Mg1 C1C 91.87(7) 14 . ?
O2 Mg1 C1C 83.98(7) 6 . ?
O1 Mg1 C1C 173.10(7) . . ?
O1 Mg1 C1C 96.55(7) 8_544 . ?
O3 Mg1 Mg1 140.84(4) 12 6 ?
O3 Mg1 Mg1 42.31(3) 14 6 ?
O2 Mg1 Mg1 81.89(3) 6 6 ?
O1 Mg1 Mg1 43.91(3) . 6 ?
O1 Mg1 Mg1 96.89(4) 8_544 6 ?
C1C Mg1 Mg1 129.29(6) . 6 ?
O3 Mg1 Mg1 42.35(3) 12 8_544 ?
O3 Mg1 Mg1 122.18(4) 14 8_544 ?
O2 Mg1 Mg1 137.75(4) 6 8_544 ?
O1 Mg1 Mg1 75.80(3) . 8_544 ?
O1 Mg1 Mg1 43.13(3) 8_544 8_544 ?
C1C Mg1 Mg1 109.38(6) . 8_544 ?
Mg1 Mg1 Mg1 113.67(2) 6 8_544 ?
C1 O1 Mg1 132.90(9) . . ?
C1 O1 Mg1 130.72(9) . 6 ?
Mg1 O1 Mg1 92.96(4) . 6 ?
C1 O2 Mg1 125.04(9) . 8_544 ?
C4 O3 Mg1 126.02(8) . 11 ?
C4 O3 Mg1 126.30(8) . 15_445 ?
Mg1 O3 Mg1 95.34(4) 11 15_445 ?
O2 C1 O1 122.12(12) . . ?
O2 C1 C2 119.96(12) . . ?
O1 C1 C2 117.91(12) . . ?
C3 C2 C4 119.97(12) . 16_545 ?
C3 C2 C1 116.93(12) . . ?
C4 C2 C1 123.07(12) 16_545 . ?
C2 C3 C4 123.21(12) . . ?
O3 C4 C3 118.41(12) . . ?
O3 C4 C2 124.78(12) . 16_545 ?
C3 C4 C2 116.82(11) . 16_545 ?
O1C C1C Mg1 168.7(3) . . ?
 
_refine_diff_density_max    0.569
_refine_diff_density_min   -0.431
_refine_diff_density_rms    0.073



