Accessing heavy allyl-analogous [(TerN)2E]- (E = Sb, Bi) ions and their reactivity towards ECl3
Alexander Hinz; Axel Schulz; Alexander Villinger; Chem.Commun. 51 (2015) 11437–; doi:10.1039/C5cc04355G

data_7117428
_publ_section_title
;
 Accessing heavy allyl-analogous [(TerN)2E]- (E = Sb, Bi) ions and their
 reactivity towards ECl3
;
_journal_name_full               Chem.Commun.
_journal_page_first              11437
_journal_paper_doi               10.1039/C5cc04355G
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C52 H58 Bi Cl Mg N2 O, C6 H6'
_chemical_formula_sum            'C58 H64 Bi Cl Mg N2 O'
_chemical_formula_weight         1073.85
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-04-13 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.645(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7359(12)
_cell_length_b                   16.6363(10)
_cell_length_c                   23.257(2)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.35
_cell_volume                     5091.9(7)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            106709
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         2.354
_exptl_absorpt_coefficient_mu    3.568
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.846
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         18429
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+4.7251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                13294
_reflns_number_total             18429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc04355g2.cif
_cod_data_source_block           ah066b_2
_cod_database_code               7117428
_shelx_estimated_absorpt_t_min   0.494
_shelx_estimated_absorpt_t_max   0.674
_shelxl_version_number           2013-4
_shelx_res_checksum              78931