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_1556688
_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
'C3 H17 B12 N2 O24 Zn, 7(H2 O), 1.5(C3 H12 N2)'
_chemical_formula_sum            'C7.5 H49 B12 N5 O31 Zn'
_chemical_formula_weight         900.60
_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                82.954(2)
_cell_angle_beta                 76.156(2)
_cell_angle_gamma                68.655(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3681(2)
_cell_length_b                   10.6910(2)
_cell_length_c                   19.2746(4)
_cell_measurement_reflns_used    24816
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0180
_cell_measurement_theta_min      2.8160
_cell_volume                     1744.44(7)
_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 0.998
_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    -39.00  77.00   1.00    1.00    --  -11.90  38.00 120.00  116
  2  \w   -101.00  22.00   1.00    1.00    --  -11.90 -72.00-180.00  123
  3  \w   -101.00  19.00   1.00    1.00    --  -11.90 -57.00 -60.00  120
  4  \w   -101.00  19.00   1.00    1.00    --  -11.90 -57.00   0.00  120
  5  \w   -101.00  15.00   1.00    1.00    --  -11.90 -38.00 150.00  116
  6  \w    -46.00  22.00   1.00    1.00    --  -11.90  72.00   0.00   68
  7  \w    -43.00  77.00   1.00    1.00    --  -11.90  57.00 -90.00  120
;
_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      0.0226431000
_diffrn_orient_matrix_UB_12      -0.0460093000
_diffrn_orient_matrix_UB_13      0.0285423000
_diffrn_orient_matrix_UB_21      -0.0475267000
_diffrn_orient_matrix_UB_22      0.0501438000
_diffrn_orient_matrix_UB_23      0.0249025000
_diffrn_orient_matrix_UB_31      -0.0643677000
_diffrn_orient_matrix_UB_32      -0.0212274000
_diffrn_orient_matrix_UB_33      0.0019706000
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38867
_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         27.484
_diffrn_reflns_theta_min         2.532
_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    0.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90992
_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    1.715
_exptl_crystal_description       prism
_exptl_crystal_F_000             934
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         7958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0139P)^2^+5.3794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7654
_reflns_number_total             7958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-44.cif
_cod_data_source_block           MAB3
_cod_original_formula_sum        'C7.50 H49 B12 N5 O31 Zn'
_cod_database_code               1556688
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.873
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Sof(O51)=Sof(H51A)=Sof(H51B)=1-FVAR(1)
 Sof(O52)=Sof(H52A)=Sof(H52B)=FVAR(1)
 Sof(O41)=Sof(H41A)=Sof(H41B)=1-FVAR(2)
 Sof(O42)=Sof(H42A)=Sof(H42B)=FVAR(2)
 Fixed Sof: N21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) N22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C21(0.5) H21D(0.5) H21E(0.5) C22(0.5) H22D(0.5) H22E(0.5)
 C23(0.5) H23A(0.5) H23B(0.5)
3.a Free rotating group:
 O31(H31A,H31B), O32(H32A,H32B), O33(H33A,H33B), O34(H34A,H34B), O35(H35A,
 H35B), O42(H42A,H42B), O52(H52A,H52B), O41(H41A,H41B), O51(H51A,H51B)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2D,H2E), C3(H3A,H3B), C11(H11D,H11E), C12(H12D,
 H12E), C13(H13A,H13B), C21(H21D,H21E), C22(H22D,H22E), C23(H23A,H23B)
3.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N11(H11A,H11B,H11C), N12(H12A,H12B,H12C), N21(H21A,H21B,
 H21C), N22(H22A,H22B,H22C)
3.d Idealised tetrahedral OH refined as rotating group:
 O19(H19), O20(H20), O21(H21), O22(H22), O23(H23), O24(H24)
;
_shelx_res_checksum              49543
_shelx_hkl_checksum              82903