 
data_Mg-p-Nitrophenolate
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C12 H24 Mg N2 O14' 
_chemical_formula_weight          444.64

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'H'  'H'   0.0000   0.0000
 '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'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_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'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    12.3698(15)
_cell_length_b                    6.6167(8)
_cell_length_c                    11.7758(14)
_cell_angle_alpha                 90
_cell_angle_beta                  93.553(3)
_cell_angle_gamma                 90
_cell_volume                      962.0(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9741
_cell_measurement_theta_min       3.58
_cell_measurement_theta_max       68.41
 
_exptl_crystal_description        'Needle-shaped'
_exptl_crystal_colour             'Yellow'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.535          
_exptl_crystal_F_000              468
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.13
_exptl_crystal_size_min           0.10
_exptl_absorpt_coefficient_mu     1.519
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.6078
_exptl_absorpt_correction_T_max   0.7531
_exptl_absorpt_process_details    'multi-scan absorption correction'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    'Micro-focus X-ray source'
_diffrn_measurement_device_type   'Bruker APEX3 Photon 100 CMOS chip'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             22584
_diffrn_reflns_av_unetI/netI      0.0168
_diffrn_reflns_av_R_equivalents   0.0415
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          3.580
_diffrn_reflns_theta_max          68.402
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   0.990
_diffrn_measured_fraction_theta_full  0.991
_diffrn_reflns_Laue_measured_fraction_max    0.990
_diffrn_reflns_Laue_measured_fraction_full   0.991
_diffrn_reflns_point_group_measured_fraction_max   0.990
_diffrn_reflns_point_group_measured_fraction_full  0.991
_reflns_number_total              1744
_reflns_number_gt                 1720
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
 
_computing_data_collection        'Bruker APEX3'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0633P)²+1.6939P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.041(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          1744
_refine_ls_number_parameters      142
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0418
_refine_ls_R_factor_gt            0.0414
_refine_ls_wR_factor_ref          0.1128
_refine_ls_wR_factor_gt           0.1124
_refine_ls_goodness_of_fit_ref    0.965
_refine_ls_restrained_S_all       0.965
_refine_ls_shift/su_max           0.000
_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
Mg Mg 1.000000 0.500000 0.500000 0.0074(3) Uani 1 2 d S . P . .
O4 O 0.95583(10) 0.40651(19) 0.65997(10) 0.0098(3) Uani 1 1 d . . . . .
H4B H 0.905019 0.483114 0.699302 0.012 Uiso 1 1 calc R U . . .
H4A H 0.986528 0.287368 0.693433 0.012 Uiso 1 1 calc R U . . .
O6 O 0.90203(10) 0.74544(19) 0.49907(10) 0.0115(3) Uani 1 1 d . . . . .
H6B H 0.898585 0.834647 0.435738 0.014 Uiso 1 1 calc R U . . .
H6A H 0.859535 0.771323 0.561970 0.014 Uiso 1 1 calc R U . . .
O5 O 1.12996(10) 0.6694(2) 0.57587(11) 0.0119(3) Uani 1 1 d . . . . .
H5B H 1.120229 0.808205 0.593036 0.014 Uiso 1 1 calc R U . . .
H5A H 1.198153 0.606677 0.592822 0.014 Uiso 1 1 calc R U . . .
O3 O 0.83520(10) 0.5468(2) 0.81491(11) 0.0114(3) Uani 1 1 d . . . . .
O1 O 0.35821(11) 0.5800(2) 0.60865(13) 0.0213(4) Uani 1 1 d . . . . .
O2 O 0.33220(11) 0.5856(2) 0.78933(13) 0.0225(4) Uani 1 1 d . . . . .
N1 N 0.39318(13) 0.5842(2) 0.70989(15) 0.0154(4) Uani 1 1 d . . . . .
C4 C 0.50782(15) 0.5865(3) 0.73632(17) 0.0127(4) Uani 1 1 d . . . . .
C1 C 0.73064(15) 0.5651(3) 0.78973(16) 0.0101(4) Uani 1 1 d . . . . .
C2 C 0.68828(16) 0.5754(3) 0.67515(16) 0.0132(4) Uani 1 1 d . . . . .
H2A H 0.736606 0.575686 0.615516 0.016 Uiso 1 1 calc R U . . .
C5 C 0.54630(16) 0.5841(3) 0.85039(17) 0.0140(4) Uani 1 1 d . . . . .
H5 H 0.497166 0.589299 0.909208 0.017 Uiso 1 1 calc R U . . .
C3 C 0.57868(16) 0.5849(3) 0.64887(17) 0.0143(4) Uani 1 1 d . . . . .
H3 H 0.551415 0.590266 0.571711 0.017 Uiso 1 1 calc R U . . .
C6 C 0.65617(16) 0.5742(3) 0.87663(16) 0.0137(4) Uani 1 1 d . . . . .
H6 H 0.682593 0.573386 0.954114 0.016 Uiso 1 1 calc R U . . .
O7 O 0.88462(12) 0.0074(2) 0.67400(12) 0.0116(3) Uani 1 1 d . . . . .
H8 H 0.923(3) -0.028(5) 0.733(3) 0.034(8) Uiso 1 1 d . . . . .
H7 H 0.822(3) 0.024(5) 0.697(3) 0.043(9) Uiso 1 1 d . . . . .
 
 
_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
Mg O6 2.0260(13) . ?
Mg O6 2.0260(13) 3_766 ?
Mg O4 2.0874(12) 3_766 ?
Mg O4 2.0874(12) . ?
Mg O5 2.1118(12) 3_766 ?
Mg O5 2.1119(13) . ?
O4 H4B 0.9500 . ?
O4 H4A 0.9500 . ?
O6 H6B 0.9500 . ?
O6 H6A 0.9500 . ?
O5 H5B 0.9500 . ?
O5 H5A 0.9500 . ?
O3 C1 1.314(2) . ?
O1 N1 1.243(2) . ?
O2 N1 1.238(2) . ?
N1 C4 1.433(2) . ?
C4 C3 1.393(3) . ?
C4 C5 1.397(3) . ?
C1 C2 1.418(3) . ?
C1 C6 1.420(3) . ?
C2 C3 1.373(3) . ?
C2 H2A 0.9500 . ?
C5 C6 1.377(3) . ?
C5 H5 0.9500 . ?
C3 H3 0.9500 . ?
C6 H6 0.9500 . ?
O7 H8 0.85(3) . ?
O7 H7 0.84(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
 _geom_angle_publ_flag
O6 Mg O6 180.0 . 3_766 ?
O6 Mg O4 86.99(5) . 3_766 ?
O6 Mg O4 93.01(5) 3_766 3_766 ?
O6 Mg O4 93.01(5) . . ?
O6 Mg O4 86.99(5) 3_766 . ?
O4 Mg O4 180.0 3_766 . ?
O6 Mg O5 89.06(5) . 3_766 ?
O6 Mg O5 90.94(5) 3_766 3_766 ?
O4 Mg O5 90.60(5) 3_766 3_766 ?
O4 Mg O5 89.40(5) . 3_766 ?
O6 Mg O5 90.94(5) . . ?
O6 Mg O5 89.06(5) 3_766 . ?
O4 Mg O5 89.40(5) 3_766 . ?
O4 Mg O5 90.60(5) . . ?
O5 Mg O5 180.0 3_766 . ?
Mg O4 H4B 120.0 . . ?
Mg O4 H4A 120.0 . . ?
H4B O4 H4A 120.0 . . ?
Mg O6 H6B 120.0 . . ?
Mg O6 H6A 120.0 . . ?
H6B O6 H6A 120.0 . . ?
Mg O5 H5B 120.0 . . ?
Mg O5 H5A 120.0 . . ?
H5B O5 H5A 120.0 . . ?
O2 N1 O1 122.20(16) . . ?
O2 N1 C4 118.49(17) . . ?
O1 N1 C4 119.30(17) . . ?
C3 C4 C5 121.21(18) . . ?
C3 C4 N1 119.93(18) . . ?
C5 C4 N1 118.84(18) . . ?
O3 C1 C2 121.29(17) . . ?
O3 C1 C6 120.96(17) . . ?
C2 C1 C6 117.75(17) . . ?
C3 C2 C1 121.20(18) . . ?
C3 C2 H2A 119.4 . . ?
C1 C2 H2A 119.4 . . ?
C6 C5 C4 119.29(18) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C2 C3 C4 119.43(18) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C6 C1 121.05(18) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
H8 O7 H7 104(3) . . ?
 
_refine_diff_density_max    0.595
_refine_diff_density_min   -0.867
_refine_diff_density_rms    0.067



