Anionic N-heterocyclic carbenes (NHCs): a versatile route to saturated NHCs bearing pendant weakly coordinating anions.
Phillips, Nicholas; Tirfoin, Rémi; Aldridge, Simon; Dalton transactions (Cambridge, England : 2003) 43 (2014) 15279–15282; doi:10.1039/c4dt02662d

data_7032255
_publ_section_title
;
 Anionic N-heterocyclic carbenes (NHCs): a versatile route to saturated
 NHCs bearing pendant weakly coordinating anions.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15279
_journal_page_last               15282
_journal_paper_doi               10.1039/c4dt02662d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C58 H63 B1 F15 K1 N2 O6'
_chemical_formula_sum            'C58 H63 B F15 K N2 O6'
_chemical_formula_weight         1219.03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 98.9391(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5956(2)
_cell_length_b                   22.6260(3)
_cell_length_c                   24.4132(4)
_cell_measurement_reflns_used    12567
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5781.64(16)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            70863
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_min         5.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.01
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9348
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         13012
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.0205665
_refine_ls_shift/su_mean         0.0005101
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 24.9 35.3 16.8 3.87 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1453
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1453
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                9113
_reflns_number_total             13012
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.76
_oxford_diffrn_Wilson_scale      13.68
_oxford_refine_ls_r_factor_ref   0.1062
_oxford_refine_ls_scale          0.29095(19)
_oxford_reflns_number_all        13012
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c4dt02662d2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7032252--7032257.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C58 H63 B1 F15 K1 N2 O6'
_cod_database_code               7032255
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 313,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) H   ( 323,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 382,X'S) H   ( 383,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 393,X'S) H   ( 392,X'S) 
RIDE C   (  42,X'S) H   ( 422,X'S) H   ( 421,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 533,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 543,X'S) H   ( 542,X'S) 
RIDE C   (  67,X'S) H   ( 672,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) H   ( 682,X'S) 
RIDE C   (  70,X'S) H   ( 702,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 712,X'S) H   ( 711,X'S) 
RIDE C   (  73,X'S) H   ( 732,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 742,X'S) H   ( 741,X'S) 
RIDE C   (  76,X'S) H   ( 762,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 772,X'S) H   ( 771,X'S) 
RIDE C   (  79,X'S) H   ( 792,X'S) H   ( 791,X'S) 
RIDE C   (  80,X'S) H   ( 802,X'S) H   ( 801,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) H   ( 822,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) H   ( 832,X'S) 
RIDE C   ( 300,X'S) H   (3001,X'S) 
RIDE C   ( 301,X'S) H   (3013,X'S) H   (3011,X'S) H   (3012,X'S) 
RIDE C   ( 302,X'S) H   (3021,X'S) H   (3023,X'S) H   (3022,X'S) 
RIDE C   ( 310,X'S) H   (3101,X'S) 
RIDE C   ( 311,X'S) H   (3111,X'S) H   (3113,X'S) H   (3112,X'S) 
RIDE C   ( 312,X'S) H   (3122,X'S) H   (3121,X'S) H   (3123,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME C(48) C(300) C(301) C(302) AND 
CONT C(48) C(300) C(302) C(301) AND 
CONT C(48) C(310) C(311) C(312) AND 
CONT C(48) C(310) C(312) C(311) 
SIMU 0.01 C(48) C(300) C(301) C(302) AND 
CONT C(48) C(300) C(302) C(301) AND 
CONT C(48) C(310) C(311) C(312) AND 
CONT C(48) C(310) C(312) C(311) 
DELU 0.01 C(48) C(300) C(301) C(302) AND 
CONT C(48) C(300) C(302) C(301) AND 
CONT C(48) C(310) C(311) C(312) AND 
CONT C(48) C(310) C(312) C(311) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;