Formation of oxidopolyborates in destruction of the [B11H14]‒ anion promoted by transition metals
Avdeeva, Varvara V.; Malinina, Elena A.; Vologzhanina, Anna V.; Sivaev, Igor B.; Kuznetsov, Nikolay T.; Inorganica Chimica Acta 509 (2020) 119693–; doi:10.1016/j.ica.2020.119693

data_1564459
_publ_section_title
;
 Formation of oxidopolyborates in destruction of the [B11H14]-- anion
 promoted by transition metals
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119693
_journal_paper_doi               10.1016/j.ica.2020.119693
_journal_volume                  509
_journal_year                    2020
_chemical_formula_moiety
'C30 H24 N6 Ni, B5 H4 O10, C5 H4 N, Cl, 5(H2 O)'
_chemical_formula_sum            'C35 H42 B5 Cl N7 Ni O15'
_chemical_formula_weight         948.96
_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                 101.7200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.8907(12)
_cell_length_b                   12.7373(7)
_cell_length_c                   29.9242(15)
_cell_measurement_reflns_used    792
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.30
_cell_measurement_theta_min      1.57
_cell_volume                     8543.0(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            66640
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.835
_diffrn_reflns_theta_min         1.390
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.3016
_exptl_absorpt_correction_T_min  0.2254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1095 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.7473.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         15809
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+11.1599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11795
_reflns_number_total             15809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            III.cif
_cod_data_source_block           III
_cod_database_code               1564459
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.760
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H16A-H16B
 1.4 with sigma of 0.02
 O16-H16B = O16-H16A
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Fixed Sof: O17(0.5) H17A(0.5) H17B(0.5)
5.a Riding coordinates:
 O11(H11A,H11B), O13(H13A,H13B), O16(H16A,H16B), O14(H14A)
5.b Free rotating group:
 O15(H15A,H15B), O17(H17A,H17B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35)
5.d Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O5(H5), O7(H7A), O10(H10A)
;
_shelx_res_checksum              24594
_shelx_hkl_checksum              42259
_olex2_submission_special_instructions 'No special instructions were received'