Unexpected behaviour in derivatives of Barluenga's reagent, Hal(Coll)<sub>2</sub>X (Coll = 2,4,6-trimethyl pyridine, collidine; Hal = I, Br; X = PF<sub>6</sub>, ClO<sub>4</sub> & BF<sub>4</sub>).
Morgan, Lewis C. F.; Kim, Yejin; Blandy, Jack N.; Murray, Claire A.; Christensen, Kirsten E.; Thompson, Amber L.; Chemical communications (Cambridge, England) 54 (2018) 9849–9852; doi:10.1039/c8cc05430d

data_7122100
_publ_section_title
;
 Unexpected behaviour in derivatives of Barluenga's reagent,
 Hal(Coll)<sub>2</sub>X (Coll = 2,4,6-trimethyl pyridine, collidine; Hal =
 I, Br; X = PF<sub>6</sub>, ClO<sub>4</sub> &amp; BF<sub>4</sub>).
;
_journal_issue                   70
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9849
_journal_page_last               9852
_journal_paper_doi               10.1039/c8cc05430d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C16 H22 Br N2, B F4'
_chemical_formula_sum            'C16 H22 B Br F4 N2'
_chemical_formula_weight         409.07
_chemical_melting_point          ?
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2018-06-04
_audit_creation_method           CRYSTALS_ver_14.61_build_6720
_audit_update_record
;
2018-07-05 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8782(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.9753(5)
_cell_length_b                   8.47823(11)
_cell_length_c                   15.0337(3)
_cell_measurement_reflns_used    16388
_cell_measurement_temperature    100
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     3600.27(11)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29348
_diffrn_reflns_theta_full        73.110
_diffrn_reflns_theta_max         76.156
_diffrn_reflns_theta_min         3.129
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.37
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3713
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.0007224
_refine_ls_shift/su_mean         0.0000234
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +13.43P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1089
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1089
_reflns_limit_h_max              35
_reflns_limit_h_min              -36
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3582
_reflns_number_total             3728
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.62
_oxford_diffrn_Wilson_scale      0.39
_oxford_refine_ls_r_factor_ref   0.0442
_oxford_refine_ls_scale          1.773(12)
_oxford_reflns_number_all        3713
_oxford_structure_analysis_title 099KEC14-100K
_cod_data_source_file            c8cc05430d2.cif
_cod_data_source_block           BrColl2BF4-100K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7122093--7122107.cif.
;
_cod_original_cell_volume        3600.28(11)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               7122100
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)