Synthesis of carborane-fused carbo- and heterocycles via zirconacyclopentane intermediates.
Cui, Chun-Xiao; Ren, Shikuo; Qiu, Zaozao; Xie, Zuowei; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2453–2459; doi:10.1039/c7dt04751g

data_7045305
_publ_section_title
;
 Synthesis of carborane-fused carbo- and heterocycles via
 zirconacyclopentane intermediates.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2453
_journal_page_last               2459
_journal_paper_doi               10.1039/c7dt04751g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C8 H22 B10 Te'
_chemical_formula_sum            'C8 H22 B10 Te'
_chemical_formula_weight         353.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-15 deposited with the CCDC.
2018-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.5980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8329(4)
_cell_length_b                   9.6869(3)
_cell_length_c                   23.4211(7)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      60.62
_cell_measurement_theta_min      5.446
_cell_volume                     3207.77(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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_temperature      296
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26292
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.679
_diffrn_reflns_theta_min         4.828
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.747
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.2558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1861 before and 0.0993 after correction. The Ratio of minimum to maximum transmission is 0.3402. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-Hexane'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.772
_refine_diff_density_min         -2.228
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1049P)^2^+5.6967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.1916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6091
_reflns_number_total             7309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04751g2.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 7045305--7045308.cif.'
_cod_database_code               7045305
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.388
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C3A(H3AA)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C4A(H4AA,H4AB), C5A(H5AA,
 H5AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC)
2.d Boron cage BH refined with riding coordinates:
 B3(H3A), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9), B10(H10), B11(H11),
 B12(H12), B3A(H3AB), B4A(H4AC), B5A(H5AC), B6A(H6AC), B7A(H7AC), B8A(H8AD),
 B9A(H9A), B10A(H10A), B11A(H11A), B12A(H12A)
;
_shelx_res_checksum              68937
_olex2_submission_special_instructions 'No special instructions were received'