Linear and macrocyclic oligo(<i>p</i>-phenylene iminoboranes) with ferrocenyl side groups - observation of selective, non-templated macrocyclization.
Schneider, Johannes S.; Krummenacher, Ivo; Braunschweig, Holger; Helten, Holger; Chemical communications (Cambridge, England) 59 (2023) 8408–8411; doi:10.1039/d3cc01825c

data_7131837
_publ_section_title
;
 Linear and macrocyclic oligo(<i>p</i>-phenylene iminoboranes) with
 ferrocenyl side groups - observation of selective, non-templated
 macrocyclization.
;
_journal_issue                   54
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8408
_journal_page_last               8411
_journal_paper_doi               10.1039/d3cc01825c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C16 H14 B Br Fe'
_chemical_formula_sum            'C16 H14 B Br Fe'
_chemical_formula_weight         352.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-29 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.50(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.920(4)
_cell_length_b                   11.581(3)
_cell_length_c                   13.820(3)
_cell_measurement_reflns_used    7488
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.31
_cell_volume                     1403.7(8)
_computing_cell_refinement       'Saint+ ver. 7.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13618
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.471
_diffrn_reflns_theta_min         2.311
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.901
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.629
_exptl_crystal_size_mid          0.467
_exptl_crystal_size_min          0.338
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0390P)^2^+0.5420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2630
_reflns_number_total             2894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01825c2.cif
_cod_data_source_block           test1_a_CCDC1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7131837
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              10555
_shelx_hkl_checksum              32004