The crystal structure of [bis(2,2′-bipyridine-6-carboxylato-κ 3 N,N,O)magnesium(II)]dihydrate, C22H18N4O6Mg
Xi-Shi, Tai; Hong-Chang, Li; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 887–889; doi:10.1515/ncrs-2023-0257

data_8107592
_publ_section_title
;
 The crystal structure of [bis(2,2&#x2032;-bipyridine-6-carboxylato-\k 3
 N,N,O)magnesium(II)]dihydrate, C22H18N4O6Mg
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              887
_journal_page_last               889
_journal_paper_doi               10.1515/ncrs-2023-0257
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C22 H14 Mg N4 O4, 2(H2 O)'
_chemical_formula_sum            'C22 H18 Mg N4 O6'
_chemical_formula_weight         458.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3055(2)
_cell_length_b                   15.1214(2)
_cell_length_c                   18.1048(2)
_cell_measurement_reflns_used    11847
_cell_measurement_temperature    296.72(10)
_cell_measurement_theta_max      77.2390
_cell_measurement_theta_min      2.9580
_cell_volume                     4190.19(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.72(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     36.00  61.00   0.50    0.55    --  108.37 -57.00  90.00   50
  2  \w     41.00  66.00   0.50    0.55    --  108.37 -57.00   0.00   50
  3  \w     37.00  64.00   0.50    0.55    --  108.37 -57.00-180.00   54
  4  \w     37.00  63.00   0.50    0.55    --  108.37 -57.00-150.00   52
  5  \w     98.00 166.00   0.50    0.55    --  108.37  34.00 -31.00  136
  6  \w    101.00 177.00   0.50    0.55    --  108.37 125.00-180.00  152
  7  \w     38.00  92.00   0.50    0.55    --  108.37-117.00 -46.00  108
  8  \w    -70.00 -26.00   0.50    0.55    --  -91.75  90.00 148.00   88
  9  \w    -29.00  23.00   0.50    0.15    --  -48.32  34.00 -31.00  104
 10  \w     44.00  95.00   0.50    0.55    --  108.37 -99.00   0.00  102
 11  \w    -27.00  13.00   0.50    0.15    --  -48.32  19.00 120.00   80
 12  \w    -94.00 -36.00   0.50    0.15    --  -48.32 -34.00 170.00  116
 13  \w   -132.00 -86.00   0.50    0.55    --  -91.75 -99.00 120.00   92
 14  \w   -120.00 -95.00   0.50    0.15    --  -48.32-125.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0995441000
_diffrn_orient_matrix_UB_12      -0.0152784000
_diffrn_orient_matrix_UB_13      0.0008068000
_diffrn_orient_matrix_UB_21      0.0053403000
_diffrn_orient_matrix_UB_22      -0.0416481000
_diffrn_orient_matrix_UB_23      -0.0775464000
_diffrn_orient_matrix_UB_31      0.0142202000
_diffrn_orient_matrix_UB_32      -0.0917266000
_diffrn_orient_matrix_UB_33      0.0349111000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16694
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.450
_diffrn_reflns_theta_min         4.782
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.00092(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4272
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0376
_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/[\s^2^(Fo^2^)+(0.0585P)^2^+1.0126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3742
_reflns_number_total             4272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0257_suppl_001.cif
_cod_data_source_block           2
_cod_database_code               8107592
_chemical_oxdiff_formula         'C H N O Mg'
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O6-H6A = O6-H6B
 0.85 with sigma of 0.02
 O5-H5A = O5-H5B
 0.85 with sigma of 0.02
 H6A-H6B
 1.34 with sigma of 0.04
 H5A-H5B
 1.34 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              92876
_shelx_hkl_checksum              62353
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.433
_oxdiff_exptl_absorpt_empirical_full_min 0.657