Crystal structure of catena-poly[triaqua-(μ2-1,4-di(pyridin-4-yl)benzene-κ2 N:N′)-(3′,5-dicarboxy-[1,1′-biphenyl]-3,4′-dicarboxylato-κO)nickel(II)], C32H26N2O11Ni
Chen, Shi-Jun; Li, Shi-Hui; Zhao, Yan; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1119–1121; doi:10.1515/ncrs-2020-0196

data_8105395
_publ_section_title
;
 Crystal structure of
 catena-poly[triaqua-(\m2-1,4-di(pyridin-4-yl)benzene-\k2
 N:N&#x2032;)-(3&#x2032;,5-dicarboxy-[1,1&#x2032;-biphenyl]-3,4&#x2032;-dicarboxylato-\kO)nickel(II)],
 C32H26N2O11Ni
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1119
_journal_page_last               1121
_journal_paper_doi               10.1515/ncrs-2020-0196
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C32 H26 N2 Ni O11'
_chemical_formula_sum            'C32 H26 N2 Ni O11'
_chemical_formula_weight         673.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.207(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6085(5)
_cell_length_b                   23.5084(14)
_cell_length_c                   15.8052(9)
_cell_measurement_reflns_used    3781
_cell_measurement_temperature    290.11(10)
_cell_measurement_theta_max      25.5490
_cell_measurement_theta_min      3.5200
_cell_volume                     2819.4(3)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.11(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  26.00   1.00    8.00    --  -12.53 -99.00-180.00   46
  2  \w     35.00  86.00   1.00    8.00    --   13.55 178.00 -30.00   51
  3  \w    -54.00  30.00   1.00    8.00    --   13.55 -57.00   0.00   84
  4  \w     -3.00  81.00   1.00    8.00    --   13.55  57.00 -30.00   84
;
_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      0.0162365000
_diffrn_orient_matrix_UB_12      0.0209211000
_diffrn_orient_matrix_UB_13      0.0319474000
_diffrn_orient_matrix_UB_21      0.0051885000
_diffrn_orient_matrix_UB_22      -0.0215859000
_diffrn_orient_matrix_UB_23      0.0314356000
_diffrn_orient_matrix_UB_31      0.0919203000
_diffrn_orient_matrix_UB_32      -0.0025041000
_diffrn_orient_matrix_UB_33      -0.0040678000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14931
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65034
_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            green
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         5148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+1.8577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                3922
_reflns_number_total             5148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2020-0196_suppl.cif
_cod_data_source_block           511
_cod_database_code               8105395
_chemical_oxdiff_formula         'c h n o ni'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5A), C7(H7), C8(H8A), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C20(H20), C22(H22), C24(H24),
  C25(H25), C28(H28)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_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 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.615