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_1564458
_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         'C25 H17 Cu N4 O2, B5 H4 O10, C3 H7 N O'
_chemical_formula_sum            'C28 H28 B5 Cu N5 O13'
_chemical_formula_weight         760.14
_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   geom
_cell_angle_alpha                102.982(2)
_cell_angle_beta                 95.930(2)
_cell_angle_gamma                110.838(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3336(13)
_cell_length_b                   11.0661(14)
_cell_length_c                   16.462(2)
_cell_measurement_reflns_used    4833
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      26.772
_cell_measurement_theta_min      2.279
_cell_volume                     1679.3(4)
_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      175.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.0349
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15711
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.979
_diffrn_reflns_theta_min         2.052
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0538 before and 0.0377 after correction. The Ratio of minimum to maximum transmission is 0.8118. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      .
_exptl_crystal_description       plate
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7248
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0902P)^2^+2.1044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1903
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4714
_reflns_number_total             7248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            II.cif
_cod_data_source_block           II
_cod_database_code               1564458
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.761
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-O13 = C29-O14 = C32-O15
 1.2 with sigma of 0.005
 C26-N5 = C29-N6 = C32-N7
 1.3 with sigma of 0.005
 N5-C27 = N5-C28 = N6-C30 = N6-C31 = N7-C33 = N7-C34
 1.45 with sigma of 0.002
 C26-C27 = C26-C28 = C27-C28 = C29-C30 = C29-C31 = C30-C31
 2.4 with sigma of 0.005
 C32-C33 = C32-C34 = C33-C34
 2.4 with sigma of 0.005
 O13-N5 = O14-N6 = O15-N7
 2 with sigma of 0.005
3. Restrained planarity
 O13, C26, N5, C27, C28
 with sigma of 0.01
 O14, C29, N6, C30, C31
 with sigma of 0.01
 O15, C32, N7, C33, C34
 with sigma of 0.01
4. Others
 Fixed Sof: O13(0.2) N5(0.2) C26(0.2) H26(0.2) C27(0.2) H27A(0.2) H27B(0.2)
 H27C(0.2) C28(0.2) H28A(0.2) H28B(0.2) H28C(0.2) O14(0.5) N6(0.5) C29(0.5)
 H29(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 H31C(0.5) O15(0.3) N7(0.3) C32(0.3) H32(0.3) C33(0.3) H33A(0.3) H33B(0.3)
 H33C(0.3) C34(0.3) H34A(0.3) H34B(0.3) H34C(0.3)
 Fixed Uiso: O13(0.1) N5(0.1) C26(0.1) C27(0.1) C28(0.1) O14(0.1) N6(0.1)
 C29(0.1) C30(0.1) C31(0.1) O15(0.1) N7(0.1) C32(0.1) C33(0.1) C34(0.1)
5.a Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C29(H29), C32(H32)
5.c Idealised tetrahedral OH refined as rotating group:
 O7(H7), O8(H8A), O9(H9A), O10(H10A)
;
_shelx_res_checksum              12110
_shelx_hkl_checksum              83206
_olex2_submission_special_instructions 'No special instructions were received'