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_1564457
_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_absolute_configuration unk
_chemical_formula_moiety         'Cu H16 N4 O2, B4 H4 O9, 2(H2 O)'
_chemical_formula_sum            'B4 Cu H24 N4 O13'
_chemical_formula_weight         395.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 111.222(4)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   10.419(2)
_cell_length_b                   27.922(7)
_cell_length_c                   8.1060(19)
_cell_measurement_reflns_used    1947
_cell_measurement_temperature    175
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.22
_cell_volume                     2198.3(9)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_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      175
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6187
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.465
_diffrn_reflns_theta_min         1.459
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.562
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0553 before and 0.0379 after correction. The Ratio of minimum to maximum transmission is 0.8457. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_meas      .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.54(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         3833
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.4319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                3323
_reflns_number_total             3833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            I.cif
_cod_data_source_block           I
_cod_original_cell_volume        2198.2(9)
_cod_original_formula_sum        'B4 H24 Cu N4 O13'
_cod_database_code               1564457
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.835
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.46(2)
 0.54(2)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups, All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(N3) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(B3) = Uanis(B2)
4. Others
 Fixed Sof: H5(0.5) H6(0.5) H1A(0.5) H1B(0.5) H1C(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) H3A(0.5) H3B(0.5) H3C(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
5.a Everything fixed:
 H5, H6
5.b Riding coordinates:
 O4(H4), O12(H12), O13(H13), O14(H14), O15(H15), O1W(H1WA,H1WB), O2W(H2WA,
 H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C), N5(H5A,
 H5B,H5C), N6(H6A,H6B,H6C), N7(H7A,H7B,H7C), N8(H8A,H8B,H8C)
;
_shelx_res_checksum              11432
_shelx_hkl_checksum              73687
_olex2_submission_special_instructions 'No special instructions were received'