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_7046325
_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         'C70 H59 B1 Cl1 Cu1 F15 N2 P1'
_chemical_formula_sum            'C70 H59 B Cl Cu F15 N2 P'
_chemical_formula_weight         1354.00
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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     other
_audit_creation_date             2015-04-14
_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                90
_cell_angle_beta                 93.2699(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6076(2)
_cell_length_b                   10.15290(10)
_cell_length_c                   35.4924(3)
_cell_measurement_reflns_used    22706
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     7054.11(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.991
_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  0.102
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14627
_diffrn_reflns_theta_full        74.595
_diffrn_reflns_theta_max         76.118
_diffrn_reflns_theta_min         4.260
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.689
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.210
_platon_squeeze_details
;
;
_refine_diff_density_max         1.15
_refine_diff_density_min         -1.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0008
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         14575
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.0021585
_refine_ls_shift/su_mean         0.0000522
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.13P)^2^ + 2.22P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1742
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1742
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              44
_reflns_limit_l_min              0
_reflns_number_gt                13345
_reflns_number_total             14627
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.38
_oxford_diffrn_Wilson_scale      0.28
_oxford_refine_ls_r_factor_ref   0.0640
_oxford_refine_ls_scale          2.237(17)
_oxford_reflns_number_all        14575
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '374RMRT15 in P 21/n'
_cod_data_source_file            c8dt01661e2.cif
_cod_data_source_block           374RMRT15
_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 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C70 H59 B1 Cl1 Cu1 F15 N2 P1'
_cod_database_code               7046325
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
DELU 0.01  P(67) C(80)  C(81)  C(82)  C(83)  C(84)  C(85) 
SIMU 0.01  P(67) C(80)  C(81)  C(82)  C(83)  C(84)  C(85) 
END                                                                             
;