Crystal structure of the nickel(II) complex aqua-(2,6-di(pyrazin-2-yl)-4,4′-bipyridine-κ3 N,N′,N′′)-(phthalato-κ2 O,O′)nickel(II) tetrahydrate, C26H26N6O9Ni
Yu-Fang, Wang; Zhang, Shu-Qi; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 907–909; doi:10.1515/ncrs-2021-0141

data_8104620
_publ_section_title
;
 Crystal structure of the nickel(II) complex
 aqua-(2,6-di(pyrazin-2-yl)-4,4&#x2032;-bipyridine-\k3
 N,N&#x2032;,N&#x2032;&#x2032;)-(phthalato-\k2 O,O&#x2032;)nickel(II)
 tetrahydrate, C26H26N6O9Ni
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              907
_journal_page_last               909
_journal_paper_doi               10.1515/ncrs-2021-0141
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C26 H18 N6 Ni O5, 4(H2 O)'
_chemical_formula_sum            'C26 H26 N6 Ni O9'
_chemical_formula_weight         625.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                70.936(5)
_cell_angle_beta                 75.684(4)
_cell_angle_gamma                63.266(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2329(5)
_cell_length_b                   11.7535(5)
_cell_length_c                   12.1109(7)
_cell_measurement_reflns_used    11246
_cell_measurement_temperature    290
_cell_measurement_theta_max      27.1390
_cell_measurement_theta_min      3.6800
_cell_volume                     1340.14(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      290
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  25.00   1.00    2.52    --  -13.80 -99.00  60.00   45
  2  \w    -12.00  82.00   1.00    2.52    --   14.82  77.00  30.00   94
  3  \w     -2.00  82.00   1.00    2.52    --   14.82  57.00   0.00   84
  4  \w     -2.00  82.00   1.00    2.52    --   14.82  57.00-150.00   84
  5  \w     -2.00  82.00   1.00    2.52    --   14.82  57.00 -90.00   84
  6  \w     -2.00  82.00   1.00    2.52    --   14.82  57.00 150.00   84
  7  \w    -86.00 -35.00   1.00    2.52    --  -13.80-178.00  60.00   51
  8  \w    -86.00 -34.00   1.00    2.52    --  -13.80 178.00-120.00   52
  9  \w    -20.00  54.00   1.00    2.52    --   14.82 -99.00  90.00   74
 10  \w    -20.00  54.00   1.00    2.52    --   14.82 -99.00 -30.00   74
 11  \w    -20.00  54.00   1.00    2.52    --   14.82 -99.00-120.00   74
 12  \w     35.00  74.00   1.00    2.52    --   14.82 178.00  30.00   39
 13  \w    -20.00  54.00   1.00    2.52    --   14.82 -99.00 120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0004580000
_diffrn_orient_matrix_UB_12      -0.0612765000
_diffrn_orient_matrix_UB_13      0.0363306000
_diffrn_orient_matrix_UB_21      -0.0145283000
_diffrn_orient_matrix_UB_22      -0.0124998000
_diffrn_orient_matrix_UB_23      -0.0475465000
_diffrn_orient_matrix_UB_31      0.0697085000
_diffrn_orient_matrix_UB_32      -0.0309249000
_diffrn_orient_matrix_UB_33      -0.0177259000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25097
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.281
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0257P)^2^+0.8487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4479
_reflns_number_total             4994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0141_suppl.cif
_cod_data_source_block           exp_1631
_cod_original_cell_volume        1340.13(13)
_cod_database_code               8104620
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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.a Riding coordinates:
 O5(H5A,H5B), O7(H7A,H7B), O8(H8A,H8B), O6(H6A,H6B), O9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C12(H12),
 C18(H18), C17(H17), C16(H16), C15(H15), C21(H21), C22(H22), C23(H23), C24(H24)
;
_olex2_date_sample_data_collection 2018-11-02
_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 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.796