Hexaborate(2-) and Dodecaborate(6-) Anions as Ligands to Zinc(II) Centres: Self-Assembly and Single-Crystal XRD Characterization of [Zn{k3O-B6O7(OH)6}(k3N-dien)].0.5H2O (dien = NH(CH2-CH2NH2)2), (NH4)2[Zn{k2O-B6O7(OH)6}2 (H2O)2].2H2O and (1,3-pnH2)3[(k1N-H3N{CH2}3NH2) Zn{k3O-B12O18(OH)6}]2.14H2O (1,3-pn = 1,3-diaminopropane)
Altahan, M.A.; Beckett, M.A.; Coles, S.J.; Horton, P.N.; Inorganics 7 (2019) 44–; doi:10.3390/inorganics7040044

data_1556686
_publ_section_title
;
 Hexaborate(2-) and Dodecaborate(6-) Anions as Ligands to Zinc(II)
 Centres: Self-Assembly and Single-Crystal XRD Characterization of
 [Zn{k3O-B6O7(OH)6}(k3N-dien)].0.5H2O (dien = NH(CH2-CH2NH2)2),
 (NH4)2[Zn{k2O-B6O7(OH)6}2 (H2O)2].2H2O and (1,3-pnH2)3[(k1N-H3N{CH2}3NH2)
 Zn{k3O-B12O18(OH)6}]2.14H2O (1,3-pn = 1,3-diaminopropane)
;
_journal_name_full               Inorganics
_journal_page_first              44
_journal_paper_doi               10.3390/inorganics7040044
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C4 H19 B6 N3 O13 Zn, 0.5(H2 O)'
_chemical_formula_sum            'C4 H20 B6 N3 O13.5 Zn'
_chemical_formula_weight         456.46
_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
_cell_angle_alpha                90
_cell_angle_beta                 99.5800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.0212(3)
_cell_length_b                   9.15620(10)
_cell_length_c                   13.6318(2)
_cell_measurement_reflns_used    15078
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2600
_cell_measurement_theta_min      2.7260
_cell_volume                     3202.55(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -98.00  19.00   1.00    2.00    --   -9.50 -57.00 -60.00  117
  2  \w    -98.00  19.00   1.00    2.00    --   -9.50 -57.00 -90.00  117
  3  \w    -33.00  79.00   1.00    2.00    --   -9.50  38.00 -90.00  112
  4  \w    -33.00  -3.00   1.00    2.00    --   -9.50  38.00  30.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0163980000
_diffrn_orient_matrix_UB_12      -0.0306357000
_diffrn_orient_matrix_UB_13      -0.0416834000
_diffrn_orient_matrix_UB_21      -0.0113781000
_diffrn_orient_matrix_UB_22      0.0695346000
_diffrn_orient_matrix_UB_23      -0.0118337000
_diffrn_orient_matrix_UB_31      0.0191250000
_diffrn_orient_matrix_UB_32      0.0150886000
_diffrn_orient_matrix_UB_33      -0.0301134000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18390
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_recrystallization_method
'The material was recrystallised from water'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3651
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+5.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3541
_reflns_number_total             3651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-44.cif
_cod_data_source_block           MAB1
_cod_original_formula_sum        'C4 H20 B6 N3 O13.50 Zn'
_cod_database_code               1556686
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.551
_shelx_res_checksum              45284
_shelx_hkl_checksum              44509