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_1556687
_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         'B12 H16 O28 Zn, 2(H4 N), 2(H2 O)'
_chemical_formula_sum            'B12 H28 N2 O30 Zn'
_chemical_formula_weight         731.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                108.065(2)
_cell_angle_beta                 95.020(2)
_cell_angle_gamma                90.118(2)
_cell_formula_units_Z            1
_cell_length_a                   7.4831(2)
_cell_length_b                   7.8551(2)
_cell_length_c                   11.0111(3)
_cell_measurement_reflns_used    12584
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5870
_cell_measurement_theta_min      2.8090
_cell_volume                     612.68(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_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    -26.00  83.00   1.00    1.00    --   -6.10  32.00 -14.00  109
  2  \w    -96.00  14.00   1.00    1.00    --   -6.10 -38.00  30.00  110
  3  \w    -26.00  83.00   1.00    1.00    --   -6.10  38.00-180.00  109
  4  \w    -96.00  23.00   1.00    1.00    --   -6.10 -72.00-120.00  119
  5  \w    -84.00  30.00   1.00    1.00    --    5.00 -57.00 -90.00  114
  6  \w    -35.00  19.00   1.00    1.00    --   -6.10  72.00   0.00   54
  7  \w    -26.00  83.00   1.00    1.00    --   -6.10  38.00  90.00  109
;
_diffrn_measurement_device       'four-circle \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      0.0940937000
_diffrn_orient_matrix_UB_12      -0.0091370000
_diffrn_orient_matrix_UB_13      -0.0018173000
_diffrn_orient_matrix_UB_21      -0.0128187000
_diffrn_orient_matrix_UB_22      -0.0940510000
_diffrn_orient_matrix_UB_23      -0.0278621000
_diffrn_orient_matrix_UB_31      -0.0066784000
_diffrn_orient_matrix_UB_32      0.0100382000
_diffrn_orient_matrix_UB_33      -0.0620578000
_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_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16475
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         2.729
_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    1.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
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    1.982
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2799
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0262P)^2^+0.3998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0559
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2774
_reflns_number_total             2799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-44.cif
_cod_data_source_block           MAB2
_cod_database_code               1556687
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 O12-H12
 0.85 with sigma of 0.01
 B1-H11
 1.945853 with sigma of 0.02
 Zn1-H11
 2.651307 with sigma of 0.02
 B2-H12
 1.919963 with sigma of 0.02
 Zn1-H12
 2.691362 with sigma of 0.02
3.a Free rotating group:
 O31(H31A,H31B)
3.b Rotating group:
 O21(H21A,H21B)
3.c Idealised tetrahedral OH refined as rotating group:
 O8(H8), O9(H9), O10(H10), O13(H13)
;
_shelx_res_checksum              42974
_shelx_hkl_checksum              63417