Hydrothermal synthesis and crystal structure of cylo[tetraaqua-bis(μ2-1,4-bis(1H-benzo[d]imidazol-1-yl)but-2-ene-κ2 N:N′)-bis(μ2-4-nitro-phthalate-κ2 O,O′)dinickel(II)], C26H23N5O8Ni
Wei-Dong, Yin; Gui-Lian, Li; Qian-Long, Liu; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 983–986; doi:10.1515/ncrs-2019-0202

data_8105912
_publ_section_title
;
 Hydrothermal synthesis and crystal structure of
 cylo[tetraaqua-bis(\m2-1,4-bis(1H-benzo[d]imidazol-1-yl)but-2-ene-\k2
 N:N&#x2032;)-bis(\m2-4-nitro-phthalate-\k2 O,O&#x2032;)dinickel(II)],
 C26H23N5O8Ni
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              983
_journal_page_last               986
_journal_paper_doi               10.1515/ncrs-2019-0202
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C26 H23 N5 Ni O8'
_chemical_formula_sum            'C26 H23 N5 Ni O8'
_chemical_formula_weight         592.20
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 112.097(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4152(5)
_cell_length_b                   10.8836(3)
_cell_length_c                   16.1172(5)
_cell_measurement_reflns_used    20197
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0390
_cell_measurement_theta_min      3.9540
_cell_volume                     2505.41(15)
_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      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    -41.00  54.00   1.00    4.39    --  -13.80  77.00 150.00   95
  2  \w    -41.00  54.00   1.00    4.39    --  -13.80  77.00  90.00   95
  3  \w    -41.00  54.00   1.00    4.39    --  -13.80  77.00-120.00   95
  4  \w    -12.00  82.00   1.00    4.39    --   14.82  77.00 -30.00   94
  5  \w    -12.00  82.00   1.00    4.39    --   14.82  77.00  30.00   94
  6  \w    -12.00  82.00   1.00    4.39    --   14.82  77.00 150.00   94
  7  \w    -86.00 -35.00   1.00    4.39    --  -13.80-178.00-120.00   51
  8  \w    -86.00 -35.00   1.00    4.39    --  -13.80-178.00-150.00   51
  9  \w    -20.00  54.00   1.00    4.39    --   14.82 -99.00  30.00   74
 10  \w     -3.00  65.00   1.00    4.39    --   14.82-119.00 163.00   68
 11  \w     -2.00  24.00   1.00    4.39    --   14.82  57.00-120.00   26
;
_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      -0.0032113000
_diffrn_orient_matrix_UB_12      -0.0072779000
_diffrn_orient_matrix_UB_13      0.0424555000
_diffrn_orient_matrix_UB_21      0.0493263000
_diffrn_orient_matrix_UB_22      -0.0067215000
_diffrn_orient_matrix_UB_23      0.0200888000
_diffrn_orient_matrix_UB_31      0.0047657000
_diffrn_orient_matrix_UB_32      0.0644626000
_diffrn_orient_matrix_UB_33      0.0068716000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41531
_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         25.500
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53732
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4653
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+4.0714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4270
_reflns_number_total             4653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0202_suppl.cif
_cod_data_source_block           lgl-20
_cod_original_cell_volume        2505.42(14)
_cod_database_code               8105912
_reflns_odcompleteness_completeness 99.67
_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 O(H,H) groups
2. Restrained distances
 O6-N5 \\sim O6A-N5
 with sigma of 0.02
 O5-N5 \\sim O5A-N5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O6A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O5A)=Sof(O6A)=1-FVAR(1)
 Sof(O5)=Sof(O6)=FVAR(1)
5.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C19(H19A,H19B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25)
;
_olex2_date_sample_data_collection 2018-10-26
_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 1.452
_oxdiff_exptl_absorpt_empirical_full_min 0.629