Crystal structure of catena-poly[triaqua(μ2-1,2-bis(4-pyridyl)ethane-κ2 N:N′)-(1,2-bis(4-pyridyl)ethane-κN)nickel(II)] 2-aminonicotinate nitrate – 1,2-bis(4-pyridyl)ethane – water (2/1/8), C36H44N8NiO12
Wang, Yu-Fang; Wei, Jing-Jing; Zhai, Xiao-Hui; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 383–385; doi:10.1515/ncrs-2017-0273

data_8106160
_publ_section_title
;
 Crystal structure of catena-poly[triaqua(\m2-1,2-bis(4-pyridyl)ethane-\k2
 N:N&#x2032;)-(1,2-bis(4-pyridyl)ethane-\kN)nickel(II)] 2-aminonicotinate
 nitrate -- 1,2-bis(4-pyridyl)ethane -- water (2/1/8), C36H44N8NiO12
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              383
_journal_page_last               385
_journal_paper_doi               10.1515/ncrs-2017-0273
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety
'C24 H26 N4 Ni O3, C6 H5 N2 O2, C6 H5 N, N O3, 4(H2 O)'
_chemical_formula_sum            'C36 H44 N8 Ni O12'
_chemical_formula_weight         839.50
_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                76.624(4)
_cell_angle_beta                 72.200(4)
_cell_angle_gamma                70.802(5)
_cell_formula_units_Z            2
_cell_length_a                   10.6451(5)
_cell_length_b                   12.1086(6)
_cell_length_c                   17.2600(7)
_cell_measurement_reflns_used    9611
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5850
_cell_measurement_theta_min      3.6370
_cell_volume                     1979.18(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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      293(2)
_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    -10.00  84.00   1.00   21.45    --   16.93  77.00 150.00   94
  2  \w    -20.00  56.00   1.00   21.45    --   16.93 -99.00 -60.00   76
  3  \w    -20.00  56.00   1.00   21.45    --   16.93 -99.00  60.00   76
  4  \w      0.00  84.00   1.00   21.45    --   16.93  57.00 -90.00   84
  5  \w    -52.00  86.00   1.00   21.45    --   16.93   0.00   0.00  138
  6  \w      0.00  84.00   1.00   21.45    --   16.93  57.00  30.00   84
  7  \w    -88.00 -49.00   1.00   21.45    --  -15.84-178.00  90.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0599582000
_diffrn_orient_matrix_UB_12      0.0227170000
_diffrn_orient_matrix_UB_13      0.0302664000
_diffrn_orient_matrix_UB_21      -0.0344745000
_diffrn_orient_matrix_UB_22      -0.0341411000
_diffrn_orient_matrix_UB_23      -0.0097104000
_diffrn_orient_matrix_UB_31      0.0229400000
_diffrn_orient_matrix_UB_32      -0.0474230000
_diffrn_orient_matrix_UB_33      0.0298803000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22780
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.494
_diffrn_reflns_theta_max         25.494
_diffrn_reflns_theta_min         3.292
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         7347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0510P)^2^+0.5770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5965
_reflns_number_total             7347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0273_suppl.cif
_cod_data_source_block           w009
_cod_original_cell_volume        1979.18(18)
_cod_database_code               8106160
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O1(H1A,H1B), O8(H8A,H8B), O7(H7A,H7B)
2.b Free rotating group:
 O6(H6C,H6D), O9(H9A,H9B)
2.c Rotating group:
 O2(H2A,H2B), O3(H3A,H3B), N6(H6A)
2.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11),
 C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
  C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36)
;
_olex2_date_sample_data_collection 2016-06-07
_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 1.546
_oxdiff_exptl_absorpt_empirical_full_min 0.582