The crystal structure of catena-poly[(μ2-4,4′-dipyridine-κ2 N,N′)-bis(3,5,6-trichloropyridine-2-oxyacetato-κO)-bis(ethanol-κO)nickel(II)], C28H26Cl6N4NiO8
Li, Jun-Xia; Du, Zhong-Xiang; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 887–890; doi:10.1515/ncrs-2020-0083

data_8105320
_publ_section_title
;
 The crystal structure of catena-poly[(\m2-4,4&#x2032;-dipyridine-\k2
 N,N&#x2032;)-bis(3,5,6-trichloropyridine-2-oxyacetato-\kO)-bis(ethanol-\kO)nickel(II)],
 C28H26Cl6N4NiO8
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              887
_journal_page_last               890
_journal_paper_doi               10.1515/ncrs-2020-0083
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         '0.5(C56 H52 Cl12 N8 Ni2 O16)'
_chemical_formula_sum            'C28 H26 Cl6 N4 Ni O8'
_chemical_formula_weight         817.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 99.609(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7577(10)
_cell_length_b                   12.6174(7)
_cell_length_c                   16.7333(10)
_cell_measurement_reflns_used    1450
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      22.7420
_cell_measurement_theta_min      3.7700
_cell_volume                     3280.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      291.2(3)
_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 0.827
_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    -81.00 -38.00   1.00    2.00    --  -13.49-178.00-150.00   43
  2  \w    -11.00  25.00   1.00    2.00    --  -13.49 -99.00  90.00   36
  3  \w    -20.00  22.00   1.00    2.00    --  -13.49 -99.00 -30.00   42
  4  \w    -52.00  37.00   1.00    2.00    --   14.89 -77.00-150.00   89
;
_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      -0.0190633000
_diffrn_orient_matrix_UB_12      0.0308472000
_diffrn_orient_matrix_UB_13      -0.0336787000
_diffrn_orient_matrix_UB_21      0.0242587000
_diffrn_orient_matrix_UB_22      -0.0280712000
_diffrn_orient_matrix_UB_23      -0.0252124000
_diffrn_orient_matrix_UB_31      -0.0336676000
_diffrn_orient_matrix_UB_32      -0.0376844000
_diffrn_orient_matrix_UB_33      -0.0088015000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7139
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.437
_diffrn_reflns_theta_min         3.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3421
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0674
_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^)+(0.0505P)^2^+8.2614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2154
_reflns_number_total             3421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0083_suppl.cif
_cod_data_source_block           ljx191111-3
_cod_database_code               8105320
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.734
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 C13-H4
 1.867415 with sigma of 0.02
 Ni1-H4
 2.669545 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C13(H13A,H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C12(H12), C11(H11), C5(H5)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;