Experimental and quantum chemical studies of anionic analogues of N-heterocyclic carbenes.
Niu, Haoyu; Mangan, Robert J.; Protchenko, Andrey V.; Phillips, Nicholas; Unkrig, Wiebke; Friedmann, Christian; Kolychev, Eugene L.; Tirfoin, Rémi; Hicks, Jamie; Aldridge, Simon; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7445–7455; doi:10.1039/c8dt01661e

data_7046326
_publ_section_title
;
 Experimental and quantum chemical studies of anionic analogues of
 N-heterocyclic carbenes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7445
_journal_page_last               7455
_journal_paper_doi               10.1039/c8dt01661e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C125 H128 B2 F30 N4'
_chemical_formula_sum            'C125 H128 B2 F30 N4'
_chemical_formula_weight         2277.98
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2014-09-19
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2018-04-19 deposited with the CCDC.
2018-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                68.934(3)
_cell_angle_beta                 72.219(3)
_cell_angle_gamma                70.185(4)
_cell_formula_units_Z            1
_cell_length_a                   12.1720(5)
_cell_length_b                   16.2564(7)
_cell_length_c                   17.7217(5)
_cell_measurement_reflns_used    14651
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      3
_cell_volume                     3010.5(2)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12520
_diffrn_reflns_theta_full        74.387
_diffrn_reflns_theta_max         76.688
_diffrn_reflns_theta_min         3.443
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1186.000
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.190
_platon_squeeze_details
;
;
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9730
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         12472
_refine_ls_number_restraints     299
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.0006973
_refine_ls_shift/su_mean         0.0000556
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 1.21P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1230
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1230
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              20
_reflns_limit_k_min              -18
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                11057
_reflns_number_total             12520
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.29
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.0502
_oxford_refine_ls_scale          4.52(5)
_oxford_reflns_number_all        12472
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '289WGRT14 in P-1'
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(5001,OCC) PART(5002,OCC) 
WEIGHT -1 PART(5002,OCC) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  10,X'S) H   ( 103,X'S) H   ( 102,X'S) H   ( 101,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) H   ( 473,X'S) 
RIDE C   (  49,X'S) H   ( 493,X'S) H   ( 492,X'S) H   ( 491,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 523,X'S) H   ( 522,X'S) H   ( 521,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) H   ( 543,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) H   ( 573,X'S) 
RIDE C   (  58,X'S) H   ( 583,X'S) H   ( 582,X'S) H   ( 581,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 743,X'S) H   ( 742,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 753,X'S) H   ( 752,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) H   ( 772,X'S) H   ( 773,X'S) 
RIDE C   (  78,X'S) H   ( 783,X'S) H   ( 782,X'S) H   ( 781,X'S) 
RIDE C   (  94,X'S) H   ( 943,X'S) H   ( 942,X'S) H   ( 941,X'S) 
RIDE C   (  95,X'S) H   ( 951,X'S) H   ( 952,X'S) H   ( 953,X'S) 
RIDE C   (  98,X'S) H   ( 981,X'S) 
RIDE C   (  99,X'S) H   ( 991,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 114,X'S) H   (1143,X'S) H   (1142,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1153,X'S) H   (1152,X'S) H   (1151,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) H   (1182,X'S) H   (1183,X'S) 
RIDE C   ( 120,X'S) H   (1203,X'S) H   (1202,X'S) H   (1201,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
REM 
REM TOLUENE DISORDER 
REM 
SAME  C(73)  C(77)  C(75)  C(69) AND 
CONT  C(73)  C(69)  C(77)  C(75) AND 
CONT  C(73)   C(75)  C(69)  C(77) AND 
CONT  C(76)  C(74)  C(78)  C(69) AND 
CONT  C(76)  C(78)  C(69)  C(74) AND 
CONT  C(76)  C(69)  C(74)  C(78) 
DELU 0.01 C(73)  C(77)  C(75)  C(69) AND 
CONT  C(73)  C(69)  C(77)  C(75) AND 
CONT  C(73)   C(75)  C(69)  C(77) AND 
CONT  C(76)  C(74)  C(78)  C(69) AND 
CONT  C(76)  C(78)  C(69)  C(74) AND 
CONT  C(76)  C(69)  C(74)  C(78) 
U(IJ)'S 0 ,0.01 = C(77) TO C(75) 
U(IJ)'S 0 ,0.01 = C(78) TO C(74) 
REM 
REM TOLUENE DISORDER 
REM 
DIST 1.50 0.01 = C(1) TO C(10) 
DIST 1.50 0.01 = C(97) TO C(94), C(96) TO C(95) 
SAME  C(97)  C(107)  C(105)  C(103)  C(100)  C(98) AND 
CONT  C(97)  C(98)  C(100)  C(103)  C(105)  C(107) AND 
CONT  C(96)  C(106)  C(104)  C(102)  C(101)  C(99) AND 
CONT  C(96)  C(99)  C(101)  C(102)  C(104)  C(106) 
SIMU 0.01 C(97)  C(107)  C(105)  C(103)  C(100)  C(98) AND 
CONT  C(97)  C(98)  C(100)  C(103)  C(105)  C(107) AND 
CONT  C(96)  C(106)  C(104)  C(102)  C(101)  C(99) AND 
CONT  C(96)  C(99)  C(101)  C(102)  C(104)  C(106) 
SIMU 0.01 C(97)  C(94) AND 
CONT  C(96)  C(95) 
DELU 0.01 C(97)  C(107)  C(105)  C(103)  C(100)  C(98) AND 
CONT  C(97)  C(98)  C(100)  C(103)  C(105)  C(107) AND 
CONT  C(96)  C(106)  C(104)  C(102)  C(101)  C(99) AND 
CONT  C(96)  C(99)  C(101)  C(102)  C(104)  C(106) 
DELU 0.01 C(97)  C(94) AND 
CONT  C(96)  C(95) 
END                                                                             
;
_cod_data_source_file            c8dt01661e2.cif
_cod_data_source_block           289WGRT14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7046314--7046326.cif.
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7046326