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_7122104
_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 I N2, Cl O4'
_chemical_formula_sum            'C16 H22 Cl I N2 O4'
_chemical_formula_weight         468.72
_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             2018-06-05
_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                 126.137(8)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   27.2651(14)
_cell_length_b                   10.9468(3)
_cell_length_c                   23.2069(12)
_cell_measurement_reflns_used    17154
_cell_measurement_temperature    100
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     5593.9(7)
_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 0.996
_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  0.037
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34815
_diffrn_reflns_theta_full        76.107
_diffrn_reflns_theta_max         76.107
_diffrn_reflns_theta_min         4.004
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.007
_exptl_absorpt_correction_T_max  0.19
_exptl_absorpt_correction_T_min  0.09
_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    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.63
_refine_diff_density_min         -1.52
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9847
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5829
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.0021835
_refine_ls_shift/su_mean         0.0000506
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +42.71P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1083
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1082
_reflns_limit_h_max              27
_reflns_limit_h_min              -34
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                5507
_reflns_number_total             5833
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.13
_oxford_diffrn_Wilson_scale      0.78
_oxford_refine_ls_r_factor_ref   0.0395
_oxford_refine_ls_scale          1.184(4)
_oxford_reflns_number_all        5831
_oxford_structure_analysis_title 139lcm18-100K
_cod_data_source_file            c8cc05430d2.cif
_cod_data_source_block           IColl2ClO4-I-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_sg_symbol_H-M      'C 2/c '
_cod_database_code               7122104
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)