Crystal structure of tetraaqua-bis(μ2-5-aminoisophthalato-κ3N:O,O′)-bis(4,4′-dipyridylsulfide-κ1N)dizinc(II), C36H34N6O12S2Ni2
Chang, Xin-Hong; Zhai, Zhi-Min; Lu, Xiao-Min; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 73–75; doi:10.1515/ncrs-2019-0492

data_8105021
_publ_section_title
;
 Crystal structure of
 tetraaqua-bis(\m2-5-aminoisophthalato-\k3N:O,O&#x2032;)-bis(4,4&#x2032;-dipyridylsulfide-\k1N)dizinc(II),
 C36H34N6O12S2Ni2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              73
_journal_page_last               75
_journal_paper_doi               10.1515/ncrs-2019-0492
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C18 H17 N3 Ni O6 S'
_chemical_formula_sum            'C18 H17 N3 Ni O6 S'
_chemical_formula_weight         462.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 108.592(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.642(4)
_cell_length_b                   6.2241(4)
_cell_length_c                   21.667(2)
_cell_measurement_reflns_used    2212
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.5550
_cell_measurement_theta_min      3.7560
_cell_volume                     3788.8(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.877
_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    -15.00  24.00   1.00    8.00    --  -13.80 -99.00   0.00   39
  2  \w      0.00  48.00   1.00    8.00    --  -13.80  19.00 -60.00   48
  3  \w    -86.00 -61.00   1.00    8.00    --  -13.80-178.00-150.00   25
  4  \w    -20.00   5.00   1.00    8.00    --  -13.80 -99.00 120.00   25
  5  \w    -80.00   3.00   1.00    8.00    --  -13.80 -57.00  90.00   83
  6  \w      2.00  57.00   1.00    8.00    --  -13.80  19.00-120.00   55
  7  \w    -41.00  -3.00   1.00    8.00    --  -13.80  77.00-150.00   38
  8  \w     -4.00  81.00   1.00    8.00    --   14.82  38.00  30.00   85
  9  \w    -52.00 -35.00   1.00    8.00    --   14.82 -57.00-120.00   17
;
_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      -0.0123949000
_diffrn_orient_matrix_UB_12      0.0038839000
_diffrn_orient_matrix_UB_13      0.0230774000
_diffrn_orient_matrix_UB_21      -0.0216953000
_diffrn_orient_matrix_UB_22      0.0167432000
_diffrn_orient_matrix_UB_23      -0.0255142000
_diffrn_orient_matrix_UB_31      -0.0036670000
_diffrn_orient_matrix_UB_32      -0.1126591000
_diffrn_orient_matrix_UB_33      -0.0030111000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.1146
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15078
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.399
_diffrn_reflns_theta_min         3.353
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48518
_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    1.620
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0907
_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^)+(0.0438P)^2^+1.0191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2929
_reflns_number_total             4181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0492_suppl.cif
_cod_data_source_block           zm-244
_cod_original_cell_volume        3788.9(7)
_cod_database_code               8105021
_chemical_oxdiff_formula         C1H1O1N1Ni1
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.727
_reflns_odcompleteness_completeness 99.53
_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 N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
2.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18)
;